Quartz sand/graphite composite molten salt heat transfer and heat storage medium and preparation method thereof
10865335 ยท 2020-12-15
Assignee
Inventors
Cpc classification
C09K5/12
CHEMISTRY; METALLURGY
C09K3/18
CHEMISTRY; METALLURGY
C09K5/00
CHEMISTRY; METALLURGY
C09K5/02
CHEMISTRY; METALLURGY
International classification
C09K5/00
CHEMISTRY; METALLURGY
C09K3/18
CHEMISTRY; METALLURGY
C09K5/12
CHEMISTRY; METALLURGY
Abstract
The present invention relates to the solar photo-thermal power generation technology. Provided is a quartz sand/graphite composite molten salt heat transfer and heat storage medium and a preparation method thereof. The medium is characterized in that it is prepared by adding quartz sand into an existing common heat transfer and heat storage molten salt system for compounding. Hot stability of the obtained heat transfer and heat storage medium is generally improved, an application temperature range is expanded, causticity is reduced, and a service life of a device is greatly prolonged. In addition, a material cost is low.
Claims
1. A heat transfer and storage medium comprising silica sand compounded with a heat transfer and storage molten salt system, wherein a weight proportion of said silica sand in said heat transfer and storage medium is 10% to 50%, said heat transfer and storage molten salt system selected from a group consisting of a binary nitrate molten salt system and a ternary nitrate molten salt system, wherein: the binary nitrate molten salt system is a KNO.sub.3NaNO.sub.2 system comprising, in relative parts by weight, 30-40 parts potassium nitrate, and 60-70 parts sodium nitrite; and the ternary nitrate molten salt system is a KNO.sub.3NaNO.sub.3NaNO.sub.2 system selected from a group consisting of following formulas, in relative part by weight: 40 parts potassium nitrate, 15 parts sodium nitrate and 30 parts sodium nitrite; 80 parts potassium nitrate, 5 parts sodium nitrate and 10 parts sodium nitrite; and 60 parts potassium nitrate, 15 parts sodium nitrate and 50 parts sodium nitrite.
2. The heat transfer and storage medium according to claim 1, wherein: the weight proportion of said silica sand in said heat transfer and storage medium is 10% to 40%.
3. The heat transfer and storage medium according to claim 1, wherein: the weight proportion of said silica sand in said heat transfer and storage medium is 20% to 45%.
4. The heat transfer and storage medium according to claim 1, wherein: the weight proportion of said silica sand in said heat transfer and storage medium is 30% to 40%.
Description
DESCRIPTION OF DRAWINGS
(1)
(2) 1: High temperature storage tank 2: Molten salt tank, 3: Gas flow dryer 4: Heat exchanger 5-1: Granulating device 5-2: Cooling device 6: Storage bin 7Packaging device 8Storage device 9Solar collector system 10Portable electric tracing 11Stirring device 12Feed inlet 13Interlayer cavity 14High-temperature molten salt pump 15Blowers 16,17,18 Heat carrier pump, 18Cryogenic storage tank 20-1,20-2,20-3Heat carrier pipe.
EMBODIMENTS
(3) Describe the invention in details by combining detailed embodiment as follows:
(4) Experimental Data
(5) Ordinary silica sand (silica content is larger than 75%), 100 sieve number is purchased from Shandong Hongtai Silica Sand factory.
(6) Graphite: commercially purchase available
(7) Potassium nitrate, sodium nitrate, sodium nitrite, cesium nitrate, calcium nitrate, and lithium nitrate: Industrial pure, all of them can be purchased from general chemical products company.
(8) Potassium carbonate, sodium carbonate, sodium chloride and lithium chloride, commercially pure grade, all of them can be purchased from general chemical products company.
(9) The preparation process of the silica sand/graphite composite heat transfer and heat storage medium of the present invention has two options:
(10) 1. Small-scale production can be used for laboratory studies by the following steps:
(11) Step 1. Constitute molten salt system in proportion. Put it into vacuum furnace to heat to dewater and degas to make it to be molten status. When it is heated, the temperature is 50-100 C. above the temperature of phase change of molten salt.
(12) Step 2, Take the silica sand/graphite in proportion, then add them into the molten molten salt system of the step (1). Stir the molten salt mixture magnetically for 0.5-1 h and insulate and ultrasound for 0.5-2 h, then naturally cool to obtain a uniform and stable silica sand/graphite composite molten salt.
(13) 2. It will preferably select the molten salt technology and related matching molten salt devices in the following for large-scale production: molten salt preparation equipment: the mentioned device includes the heat source unit, molten salt tank with a interlayer cavity (13) (2) air crushing dryer (3) granulating device (5-1), cooling device (5-2) and the output device;
(14) During the operation, add the constituted materials of molten salt system in proportion into molten salt tank (2) with jacketing. Start heat source device and heat it to molten sate and add silica sand/graphite in proportion and heat continuously to uniform molten salt system.
(15) The uniform heated composite molten salt is pumped to a gas flow crushing dryer (3) to crush and dry gas flow to obtain the silica sand/graphite composite molten salt heat transfer and thermal storage medium, and then output by output device after being granulated and cooled.
(16) The mentioned heat source unit includes a heat carrier bearing chamber, which is connected through the heat carrier pipe (20-1) between the carrying chamber of heat carrier and the interlayer cavity (13);
(17) The mentioned molten salt tank (2) gas flow crushing dryer (3) the granulating device (5-1) cooling device (5-2) and the output device are connected through the molten salt pipe. The mentioned molten salt pipe extending from the lower end of molten salt tank (2) connects with the upper end of gas flow crushing dryer (3) The lower end of gas flow crushing dryer (3) is connected with the heat exchanger (4.) The Uniform molten salt system of the molten salt tank is pumped above into gas flow crushing dryer. Meanwhile the heat air is blown into dryer from the bottom of the gas flow crushing dryer. Two are contrary. Purpose: Form the liquid-phase molten salt system into dry and even powder form through gas flow crushing dryer. It is convenient to pack to sell on the one side. The performance can be uniform and stable when it is used on the other side.
(18) The mentioned heat source devices are the solar collector system (9), mobile electric tracing (10) or independently controlled and parallel solar collector system (9) and mobile electric tracing (10). The heat source device of this device can be a single or separate solar collector system (9) and a single mobile electric tracing. It can also be controlled independently and in parallel solar collector system (9) and mobile electric tracing (10).
(19) There are independently controlled two carrier pipes between the solar collector system (9) and the molten salt tank (20-1). One of them is provided with a high temperature storage tank (1). There is a valve between the solar collector 9 and the high temperature storage tank which is used for controlling the heat carrier flow to the high temperature storage tank 1. When the valve is closed, you can use the solar collector system 9 or a mobile electric tracing 10 directly heating the heat carrier by heating the molten salt tank 2, which is for the preparation of high temperature molten salt. When the energy is sufficient or the molten salt tank does not need to be heated, the valve between the solar collector system and the high-temperature storage tank 1 can be open. After a solar heating system heating the heat carrier, the heat carrier can be stored in the high-temperature storage tank through piping to high temperature storage tanks, when heating is required, the high-temperature molten salt preparation can be achieved by the heat carrier pump (19) pumped into the interlayer cavity (13) and further heating molten salt tank (2).
(20) Preferably selecting the molten salt and the molten salt tank pipe between the gas flow crushing dryer (3) provided the high-temperature molten salt pump (14), which is used to draw the heated molten salt to the jet mill dryer.
(21) Preferably selecting the interlayer cavity (13) bottom of the molten salt tank (2) and the heat exchanger (4) is connected by a period of heat carrier pipe (20-2) in communication. The pipe section of the heat carrier (20-2) for the interlayer cavity (13) of the heat carrier guided to the heat exchanger (4) for heating the required hot air from device, enabling the rest heat from heat carrier (13) of the interlayer cavity to be re-used, energy-saving and environmental protection.
(22) Preferably selecting the heat exchanger (4) and the heat source device, connecting through a period of heat carrier pipe (20-3) in communication, provided cryogenic storage tank (18) on the heat carrier pipe (20-3), the cryogenic storage tank (18) is provided with a heat carrier pump (16) (17) at both ends of the heat carrier pipe (20-3). The heat carrier is cooling after being exhausted in the heat exchanger, which is pumping back the cryogenic storage tank through the heat carrier pipe (20-3) (16) to a, through the heat carrier pump (17) is sent back the source device and recycling use.
(23) Preferably, the molten salt tank (2) also includes stirring device (11) and inlet (12)
(24) Preferably mentioned output device sequentially includes build bin (6), packaging device (7) and/or storage device (8).
(25) Each section of the mentioned heat carrier pipe is at least provided with a heat carrier pump.
(26) Each section pipe of the above described device all is provided with sufficient valve for controlling the flow and flow direction of material in pipe. Valves on the heat carrier pipe, which is between the heat source device and molten salt tank interlayer cavity, controls the heating temperature by controlling the transmission throughput and speed of the heat carrier. the molten salt tank itself is with a pressure control device.
Embodiment 1-3. Add Silica Sand into Binary Nitrate System KNO.SUB.3.NaNO.SUB.3 .to Prepare Heat Transfer and Heat Storage Medium
(27) Step 1. Prepare and compose the materials of binary nitrate molten salt system according to the formula listed in table 1 and put them into reaction kettle to heat and stir to melt solid completely and insulate for 0.5-1 h. The heating temperature is 80-120 C. over phase-transition temperature of molten salt.
Step 2. Under the condition of stirring, disperse silica sand into binary nitrate molten sand system and stir for 1-2 h continuously until the mixed substances become gel.
(28) TABLE-US-00001 TABLE 1 The formula of binary nitrate molten salt in each embodiment Example Binary nitrate Formula of No. molten salt system binary nitrate system (part by weight) 1 KNO.sub.3NaNO.sub.3 Potassium nitrate: 10 parts. Sodium nitrate: 90 parts. 2 Potassium nitrate: 30 parts. Sodium nitrate: 45 parts. 3 Potassium nitrate: 45 parts. Sodium nitrate: 30 parts.
Added silica sand (specification is 100 meshes) is carried out according to the following gradient. The first group: Silica sand occupies 1% of binary nitrate molten sand heat transfer and heat storage medium with three kinds of silica sands compounded. Obtain the first one to the third products. The second group: Silica sand occupies 10% of binary nitrate molten sand heat transfer and heat storage medium with three kinds of silica sands compounded. Obtain the fourth to the sixth products. The third group: Silica sand occupies 20% of binary nitrate molten sand heat transfer and heat storage medium with three kinds of silica sands compounded. Obtain the seventh to the ninth products.
The fourth group: Silica sand occupies 30% of binary nitrate molten sand heat transfer and heat storage medium with three kinds of silica sands compounded. Obtain the tenth to the twelfth products.
The fifth group: Silica sand occupies 40% of binary nitrate molten sand heat transfer and heat storage medium with three kinds of silica sands compounded. Obtain the thirteenth to the fifteenth products.
The sixth group: Silica sand occupies 50% of binary nitrate molten sand heat transfer and heat storage medium with three kinds of silica sands compounded. Obtain the sixteenth to the eighteenth products.
(29) The contrast of each product is the corresponding binary nitrate molten salt of the product.
(30) Step 3 Latent Heat of Phase Change Test and Melting Point Test:
(31) Adopt universal differential scanning calorimeter (scan under atmospheric pressure).
(32) Test results show that latent heat of phase change is increased obviously compared with contrast.
(33) The weight percentage ratio of silica sand composite binary nitrate molten no. KNO.sub.3NaNO.sub.3 molten salt system (it is the contrast at the same time).
(34) TABLE-US-00002 TABLE 2 Test Results of Melting Point The Number of silica sand composite binary nitrate molten salt Melting point C. Contrast: potassium nitrate 10%. Sodium 270 nitrate 90% 1 250 4 254 7 256 10 270 13 274 16 278 Contrast: potassium nitrate 40%. Sodium 220 nitrate 60% 2 205 5 207 8 203 11 219 14 228 17 231 Contrast: potassium nitrate 60%. Sodium 210 nitrate 40% 3 198 6 199 9 193 12 210 15 213 18 212
(35) The melting point of products of the first group to the third group is reduced a little bit. The melting point of products of the fifth group to the sixth group is increased slightly.
(36) Step 4. Heat Stability Test
(37) The heat stability test is carried out on prepared 18 heat transfer and heat storage mediums and 3 binary molten nitrate salts in the control group.
(38) The test is carried out with a gravimetric analysis: put 18 molten salts obtained in embodiments 1-3 into a nickel crucible respectively put the same into a temperature-controlled furnace for heating. Carry out experiment from a room temperature. Take out an experimental crucible at set intervals and weigh with an analytical balance. If the weight of a sample is not yet decreased in a certain temperature section, the temperature of the temperature control furnace should be improved. Then, the experimental crucible is taken out at set intervals and weighed, and heating is continued after reaching at another steady state.
(39) The equilibrium temperature limit of four binary nitrate systems in the control group is 550 C. By heating for 100 h at 550 C. the loss rate can reach 10%; and by heating for 30 h, the loss rate reaches 5%. By heating for 100 h at 710 C. the loss rate can reach 25%; and by heating for 30 h, the loss rate reaches 13%.
(40) The heat stability test is carried out on three groups of 18 heat transfer heat storage mediums obtained in embodiments 1-3.
(41) TABLE-US-00003 TABLE 3 Statistical results of loss rate at 550 C. Product Time (hour) group No. 30 100 The first <5% <10% group The second <3.8% <7% group The third <3.5% <6.5% group The fourth <3.2% <6.1% group The fifth <2.9% <5.5% group The sixth <3% <5% group
(42) It can be seen that the heat stability of the products of each group can be significantly improved by adding silica sand at 550 C. relative to the contrast.
(43) TABLE-US-00004 TABLE 4 Statistical results of loss rate at 710 C. Product Time (hour) group No. 30 100 The first <10.2% <22% group The second <7.6% <16.2% group The third <6.5% <14.5% group The fourth <5.5% <13.0% group The fifth <5.1% <12% group The sixth <5.1% <11% group
(44) It can be seen that the heat stability of the products of each group can be significantly improved by adding very little silica sand at 710 C. relative to contrast.
Embodiments 4-7. Prepare Heat Transfer and Heat Storage Medium by Adding Silica Sand in Binary Nitrate System KNO.SUB.3.NaNO.SUB.2
(45) Step 1. Prepare the material constituting the binary nitrate system according to the formula listed in Table 5. Put the same into a reaction kettle, heat and mix to fuse solid completely, and then insulate for 0.5-1 h. The heating temperature is 80-120 C. above the phase change temperature of the molten salt.
Step 2. Disperse the silica sand into the molten binary nitrate system under the condition of stirring and stir continuously for 1-2 h. The mixture is colloidal.
(46) TABLE-US-00005 TABLE 5 Formula of binary nitrate system in each embodiment Embodiment Binary nitrate Formula of binary nitrate system (part No. system by weight) 4 KNO3NaNO2 Potassium nitrate: 30 parts; sodium nitrite: 70 parts 5 Potassium nitrate: 40 parts; sodium nitrite: 60 parts 6 Potassium nitrate: 45 parts; sodium nitrite: 55 parts 7 Potassium nitrate: 55 parts; sodium nitrite: 45 parts
The added silica sand (the specification is 100 meshes) is conducted according to the following proportional gradient:
The first group: silica sand accounts for 1% in four quartz sand composite binary molten nitrate salt based heat transfer heat storage mediums, and the 1.sup.st-4.sup.th products are obtained.
The second group: quartz sand accounts for 10% in four quartz sand composite binary molten nitrate salt based heat transfer heat storage mediums, and 5th-8th products are obtained.
The third group: quartz sand accounts for 20% in four quartz sand composite binary molten nitrate salt based heat transfer heat storage mediums, and 9th-12th products are obtained.
The fourth group: quartz sand accounts for 30% in four quartz sand composite binary molten nitrate salt based heat transfer heat storage mediums, and 13th-16th products are obtained.
The fifth group: quartz sand accounts for 40% in four quartz sand composite binary molten nitrate salt based heat transfer heat storage mediums, and the 17th-20th products are obtained.
The sixth group: quartz sand accounts for 50% in four quartz sand composite binary molten nitrate salt based heat transfer heat storage mediums, and 21st-24th products are obtained.
(47) The contrast of each product is the corresponding binary nitrate salt of the product.
(48) Step 3. Latent Heat of Phase Change Test and Melting Point Test:
(49) The general differential scanning calorimeter DSC is used (scan at an ordinary pressure).
(50) The test results show that, the latent heat of phase change is obviously increased by comparing with the contrast.
(51) TABLE-US-00006 TABLE 6 Test results of melting point Quartz sand composite binary molten nitrate Melting salt No. point ( C.) Contrast: potassium nitrate: 30 parts; sodium 207 nitrite: 70 parts 1 197 5 195 9 193 13 199 17 213 21 220 Contrast: potassium nitrate: 40 parts; sodium 133 nitrite: 60 parts 2 125 6 118 10 115 14 123 18 140 22 142 Contrast: potassium nitrate: 45 parts; sodium 132 nitrite: 55 parts 3 122 7 121 11 119 15 126 19 138 23 141 Contrast: potassium nitrate: 55 parts; sodium 133 nitrite: 45 parts 4 126 8 120 12 117 16 125 20 139 24 145
(52) The melting points of the products in the 1st-4th group are decreased somewhat; and the melting points of the products in the fifth group and sixth group re increased somewhat.
(53) Step 4. Heat Stability Test
(54) The heat stability test is carried out on prepared 24 heat transfer heat storage mediums and contrasted 4 binary molten nitrate salts.
(55) The test is carried out with the weighting method: put 24 molten salts obtained in embodiments 5-8 into the nickel crucible respectively put the same into the temperature-controlled furnace for heating. Carry out experiment from the room temperature and take out an experimental crucible at set intervals and weigh with the analytical balance. If the weight of the sample is not yet decreased in a temperature section, the temperature of the temperature-controlled furnace is improved. Then, the experimental crucible is taken out at set intervals and weighed, and heating is continued after arriving at another steady state.
(56) The equilibrium temperature limit of four binary nitrate systems in the contrast is 500 C. By heating for 100 h at 500 C., the loss rate can reach 12%; and by heating for 30 h, the loss rate reaches 5%. By heating for 100 h at 600 C. the loss rate can reach 22%; and by heating for 30 h, the loss rate reaches 12%.
(57) The heat stability test is carried out on six groups of 24 heat transfer heat storage mediums obtained in embodiments 4-7.
(58) TABLE-US-00007 TABLE 7 Statistical results of loss rate at 500 C. Product Time (hour) group No. 30 100 The first <5% <10% group The second <3.6% <7.5% group The third <3.7% <7.0% group The fourth <3.2% <6.1% group The fifth <2.9% <5.5% group The sixth <3% <5% group
(59) It can be seen that, the heat stability of groups of products can be significantly improved by adding quartz sand at 500 C. relative to the contrast.
(60) TABLE-US-00008 TABLE 8 Statistical results of loss rate at 800 C. Product Time (hour) group No. 30 100 The first <9% <20% group The second <7.6% <17% group The third <6.5% <12% group The fourth <5.8% <10% group The fifth <5.6% <8.4% group The sixth <5.3% <7.9% group
(61) It can be seen that, the heat stability of groups of products can be significantly improved by adding very little quartz sand at 600 C. relative to the contrast.
Embodiment 8-11 Add Silica Sand in Ternary Nitrate System KNO.SUB.3.NaNO.SUB.3.NaNO.SUB.2 .to Prepare Heat Transfer and Heat Storage Medium
(62) Step 1 Prepare materials forming ternary nitrate molten salt system according to the formula listed in the table 9. Put them in the reactor, heat and stir to melt solid completely, and then insulate for 0.5-1 h. The heating temperature is 50-100 C. over the temperature of phase change of molten salt.
(63) TABLE-US-00009 TABLE 9 Materials of Ternary Nitrate Molten Salt Number of Formula of ternary nitrate embodiment Ternary nitrate system molten salt (part by weight) 8 KNO.sub.3NaNO.sub.3NaNO.sub.2 Potassium nitrate: 40 parts. Sodium nitrate: 15 parts. Sodium nitrite: 30 parts. 9 Potassium nitrate: 80 parts. Sodium nitrate: 5 parts. Sodium nitrite: 10 parts. 10 Potassium nitrate: 60 parts. Sodium nitrate: 15 parts. Sodium nitrite: 50 parts. 11 Potassium nitrate: 53 parts. Sodium nitrate: 7 parts. Sodium nitrite: 40 parts.
Step 2: Under condition of stirring, disperse silica sand into molten ternary nitrate molten salt system and stir 1-2 h continuously until the mixture is gelatinous.
(64) The added silica sand (specification is 100 meshes) is carried out according to the following
(65) The first group: Silica sand occupies 1% of four types of silica sands composite ternary nitrate heat transfer and heat storage medium. Obtain the first to the fourth products.
(66) The second group: Silica sand occupies 10% of four types of silica sands composite ternary nitrate heat transfer and heat storage medium. Obtain the fifth to the eighth products.
(67) The third group: Silica sand occupies 25% of four types of silica sands composite ternary nitrate heat transfer and heat storage medium. Obtain the ninth to the twelfth products.
(68) The fourth group: Silica sand occupies 40% of four types of silica sands composite ternary nitrate heat transfer and heat storage medium. Obtain the thirteenth to the sixteenth products.
(69) The fifth group: Silica sand occupies 50% of four types of silica sands composite ternary nitrate heat transfer and heat storage medium. Obtain the seventeenth to the twentieth products.
(70) Step 3. Latent Heat of Phase Change Test and Melting Point Test
(71) Adopt universal differential scanning calorimeter to scan (at atmospheric pressure)
(72) Test results show that the intent heat of phase change is increased obviously compared with contrast. The melting point of the first group of the products to the third group of products keep unchanged. The melting points of the fourth group and the fifth group of products are improved slightly.
(73) Step 4 Heat Stability Test
(74) Contrasting ternary nitrate molten salt, carry out thermal stability test for the 20 kinds of heat transfer and heat storage mediums obtained from preparation.
(75) Test is carried out by adopting gravimetric analysis: Put 20 kinds of molten salts obtained from embodiment 8-11 into nickel crucible and heat it in temperature-controlled furnace. Carry out experiment starting from normal temperature. Take out crucible of experiment at intervals to weigh it by analytical balance. If the sample weight is not reduced any more at certain temperature range, the temperature of temperature-controlled furnace should be increased and then take out crucible of experiment at intervals to weigh and raise temperature again continuously after reaching another steady state.
(76) Contrast the stable temperature limit 500 C. of ternary nitrate system, the loss rate can reach 25% when it is heated for 100 hours at 500 C. The loss rate can reach 10% when it is heated for 30 hours at 500 C. The loss rate can reach 30% when it heated for 100 hours at 600 C. The loss rate can reach 15% when it is heated for 30 hours at 500 C. The loss rate can reach 35% when it is heated for 100 hours at 700 C. The loss rate can reach 24% when it is heated for 30 hours at 700 C.
(77) Carry out thermal stability test for five groups of twenty kinds of heat transfer and heat storage mediums obtained from embodiment 8-11.
(78) TABLE-US-00010 TABLE 10 Statistical Results of Loss Rate at 600 C. Product Time (hour) group no. 30 100 The first 8~10% 22~26% group The second 7~9% 18~20% group The third 4~6% 15~20% group The fourth 2~3% 12~16% group The fifth 2~4% 12~16% group
(79) TABLE-US-00011 TABLE 11 The Statistical Results of Loss Rate at 700 C. Product Time (hour) group no. 30 100 The first 15~20% 25~30% group The second 12~15% 20~23% group The third 10~13% 18~20% group The fourth 8~12% 15~18% group The fifth 9~12% 15~18% group
(80) It can be seen that the heat stability of the products of each group is increased obviously at 600 C. and 700 C. after adding silica sand relative to contrast.
Embodiment 12-14 Prepare Heat Transfer and Heat Storage Medium by Adding Silica Sand in Ternary Nitrate System KNO.SUB.3.NaNO.SUB.3.Ca(NO.SUB.3.)
(81) Step 1, 2 Prepare silica sand composite ternary nitrate according to the formula listed in table 12. The method is the same as the methods of step 1, 2 of embodiments 8-11.
(82) TABLE-US-00012 TABLE 12 The Materials of Ternary Nitrate Molten Salt Ebodiment Ternary Nitrate System Number Ternary Nitrate System Formula (Part by Weight) 12 KNO.sub.3NaNO.sub.3Ca (NO.sub.3).sub.2 Potassium nitrate: 45 parts. Sodium nitrate: 7 parts. Calcium nitrate: 48 parts. 13 Potassium nitrate: 29.97 parts. Sodium nitrate: 20.53 parts. Calcium nitrate: 49.5 parts. 14 Potassium nitrate: 22.97 parts. Sodium nitrate: 11.89 parts. Calcium nitrate: 65.32 parts.
(83) The adding of silica sand is carried out according to gradient.
(84) The first group: silica sand occupies 1% of three kinds of silica sand composite ternary nitrate molten salt heat transfer and heat storage medium. The 1st-3rd products are obtained.
(85) The second group: silica sand occupies 30% of four kinds of silica sand composite ternary nitrate molten salt heat transfer and heat storage. The 4th-6th products are obtained.
(86) The third group: silica sand occupies 50% of four kinds of silica sand composite ternary nitrate molten salt heat transfer and heat storage. The 7th-9th products are obtained.
(87) Step 3 Latent Heat of Phase Change Test and Melting Test
(88) Adopt universal differential scanning calorimeter DSC (scan at normal pressure)
(89) Test result shows that the latent heat of phase change is increased obviously. Compared with the contrast, the melting points of the first group and the second group keep unchanged basically. The melting point of the third group is improved obviously.
(90) Step 4 Heat Stability Test
(91) Carry out heat stability test on prepared nine kinds of heat transfer and heat storage mediums by contrasting ternary nitrate molten salt.
(92) Test is carried out by adopting weighting method: Put nine kinds of molten salt obtained from embodiment 12-14 into silver crucible and heat them in the temperature-controlled furnace. Carry out experiment starting from normal temperature and take out experimental crucible at intervals and weigh by using analytic balance. If the weight of sample is not reduced any more at certain temperature section, the temperature of temperature-controlled furnace should be improved and then take out experimental crucible at intervals to weigh and rise temperature continuously again after reaching another stable status.
(93) The limit is 550 C. by contrasting the stable temperature of ternary nitrate system. At 550 C. heat for 30 hours, and then the loss rate is around 3%. Heat for 50 hours, and then loss rate is around 6%. At 650 C. heat for 30 hours, the loss rate is around 5%. Heat for 50 hours, and then the loss rate is around 10%. At 750 C. heat for 30 hours, the loss rate is around 7%. The loss rate is around 15% when it is heated for 50 hours. The loss rate is around 7% when it is heated for 30 hours. The loss rate is around 12% when it is heated for 50 hours.
(94) Carry out heat stability test on three groups of nine kinds of heat transfer and heat storage mediums obtained from embodiments 12-14.
(95) TABLE-US-00013 TABLE 13 Statistical Results of Loss Rate at 650 C. Product Time (hour) group no. 30 50 The first <4% <8% group The second <3% <6% group The third <2.5% <4% group
(96) TABLE-US-00014 TABLE 14 The Statistical Result of Loss Rate at 750 C. Product Time (hour) group no. 30 50 The first <5% <12% group The second <4% <9% group The third <3% <6.5% group
(97) It can be seen that the loss rate of the invented products at 750 C. is close to that of contrast at 550 C. It means that the invented product possesses better heat stability and can be operated for long time stably at 750 C.
Embodiments 15-17 Prepare Heat Transfer and Heat Storage Medium by Adding Silica Sand in Polybasic Nitrate System KNO.SUB.3.NaNO.SUB.3.NaNO.SUB.2.CsNO.SUB.3
(98) Step 1. Preparation of Silica Sand Composite Polybasic Nitrate Molten Salt Products 1-3
(99) Prepare the materials constituting polybasic nitrate molten salt system according to the formula 1517 listed in table 15. Add silica sand after heating and stirring evenly and heat and stir continuously to degas and dewater. The heating temperature is 80-120 C. above the temperature of phase change of molten salt.
(100) Disperse silica sand (100 meshes) into molten polybasic nitrate molten salt system. Stir the molten mixture for 1-2 h and obtain the silica sand composite polybasic nitrate molten salt heat transfer and heat storage medium. Silica sand occupies 1%, 20%, 50% in the products 1-3 respectively.
(101) TABLE-US-00015 TABLE 15 Poly-basic Nitrate System Formula in Each Embodiment Embodiment Number Polybasic nitrate system Polybasic nitrate system formula 15 KNO.sub.3NaNO.sub.3NaNO.sub.2CsNO.sub.3 Potassium nitrate 80 parts. Sodium system nitrate 5 parts. Sodium nitrite 20 parts. Cesium nitrate 1 part. 16 Potassium nitrate 40 parts. Sodium nitrate 15 parts. Sodium nitrite 50 parts. Cesium nitrate 10 part. 17 Potassium nitrate 60 parts. Sodium nitrate 10 parts. Sodium nitrite 30 parts. Cesium nitrate 5 parts. 18 KNO.sub.3NaNO.sub.3NaNO.sub.2Ca(NO3).sub.2 Potassium nitrate 40 parts. Sodium system nitrate 15 parts. Sodium nitrite 50 parts. Cesium nitrate 10 parts. 19 Potassium nitrate 80 parts. Sodium nitrate 5 parts. Sodium nitrite 20 parts. Cesium nitrate 1 part. 20 Potassium nitrate 60 parts. Sodium nitrate 10 parts. Sodium nitrite 30 parts. Cesium nitrate 5 parts. 21 KNO.sub.3NaNO.sub.3NaNO.sub.2LiNO.sub.3 Potassium nitrate 80 parts. Sodium system nitrate 5 parts. Sodium nitrite 20 parts. Cesium nitrate 1 part. 22 Potassium nitrate 40 parts. Sodium nitrate 15 parts. Sodium nitrite 50 parts. Cesium nitrate 10 parts. 23 Potassium nitrate 60 parts. Sodium nitrate 10 parts. Sodium nitrite 40 parts. Cesium nitrate 8 parts. 24 KNO.sub.3NaNO.sub.3CsNO.sub.3Ca(NO.sub.3).sub.2 Potassium nitrate 80 parts. Sodium system nitrate 5 parts. Sodium nitrite 20 parts. Cesium nitrate 5 parts. 25 Potassium nitrate 60 parts. Sodium nitrate 10 parts. Sodium nitrite 40 parts. Cesium nitrate 10 parts. 26 Potassium nitrate 40 parts. Sodium nitrate 15 parts. Sodium nitrite 50 parts. Cesium nitrate 1 part. 27 KNO.sub.3NaNO.sub.3LiNO.sub.3CsNO.sub.3 Potassium nitrate 60 parts. Sodium system nitrate 8 parts. Sodium nitrite 20 parts. Cesium nitrate 10 parts. 28 Potassium nitrate 80 parts. Sodium nitrate 5 parts. Sodium nitrite 30 parts. Cesium nitrate 10 parts. 29 Potassium nitrate 40 parts. Sodium nitrate 15 parts. Sodium nitrite 50 parts. Cesium nitrate 6 parts. 30 KNO.sub.3NaNO.sub.3NaNO.sub.2CsNO.sub.3Ca(NO.sub.3).sub.2 Potassium nitrate 70 parts. Sodium system nitrate 5 parts. Sodium nitrite 30 parts. Cesium nitrate 10 parts. Calcium nitrate 20 parts. 31 Potassium nitrate 40 parts. Sodium nitrate 15 parts. Sodium nitrite 50 parts. Cesium nitrate 20 parts. Calcium nitrate 30 parts. 32 Potassium nitrate 80 parts. Sodium nitrate 10 parts. Sodium nitrite 10 parts. Cesium nitrate 30 parts. Calcium nitrate 10 parts.
Step 2. The Heat Stability Test of Silica Sand Composite Polybasic Nitrate Molten Salt Product 1-3
(102) Carry out heat stability test on prepared heat transfer and heat storage medium by contrasting polybasic nitrate molten salt.
(103) Test is carried out by adopting weighting method: put 3 kinds of molten salts into nickel crucible respectively obtained in embodiment 15-17. Put them into temperature-controlled furnace to heat. Carry out experiment starting from normal temperature. Take out experimental crucible at intervals to weigh by using analytic balance. If the weight of sample is not reduced any more at certain temperature section, the temperature of temperature-controlled furnace should be increased, and then take out experimental crucible to weigh at intervals and increase temperature continuously after reaching another stable state.
(104) Results show:
(105) Insulate the molten salts of silica sand composite polybasic nitrate products 1-3 for 120 hours. The loss rate is less than 1%.
(106) Insulate them for 30 hours at 700 C. The loss rates of three products are 20%, 3% and 1% respectively.
(107) Contrasting three kinds of polybasic nitrate molten salts without silica sand (the corresponding system of no. 1-3 of embodiments 15-17 in table 15), the loss rate is around 8% for operating 30 hours at 600 C. It has obvious loss at 700 C. The loss rate reaches 25% when it operates to 30 hours.
(108) It means that the stability of nitrate molten salt system at the high temperature can be improved and the operating upper limit temperature can be improved after adding silica sand.
(109) Step 3. The Latent Heat of Phase Change Test and Melting Point Test of Silica Sand Composite Polybasic Nitrate Molten Salt Products 1-3
(110) Adopt universal differential scanning calorimeter DSC (scan at normal pressure).
(111) Test results show that the latent heat of phase change in increased obviously comparing with contrast. The melting points of product 1 and product 2 keep unchanged basically. The melting point of product 3 is increased slightly.
Embodiments 18-20 Prepare Heat Transfer and Heat Storage Medium by Adding Silica Sand in Polybasic Nitrate System KNO.SUB.3.NaNO.SUB.3.NaNO.SUB.2.Ca(NO.SUB.3.).SUB.2
(112) Prepare materials constituting polybasic nitrate molten salt system according to the formula listed in table 15.
(113) The preparation method of products 4-6 are the same with embodiments 15-17 exactly. Silica sand (100 meshes) occupies 10%, 25% and 40% respectively. Contrasting molten salt without silica sand, it is the system corresponding with that in embodiments 15-17 in table 15.
(114) The heat stability test result is close to embodiments 15-17. The loss rates of the prepared three products of this invention are 10%, 3% and 1% respectively after insulating for 30 hours at 700 C. It is 28% higher that the highest of the contrast obviously.
(115) Adopt universal differential scanning calorimeter DSC (scan at normal pressure). The test results show that the latent heat of phase change is increased obviously comparing with contrast and the melting point keeps unchanged basically.
Embodiments 21-23 Prepare Heat Transfer and Heat Storage Medium by Adding Silica Sand in Polybasic Nitrate System KNO.SUB.3.NaNO.SUB.3.NaNO.SUB.2.LiNO.SUB.3
(116) Prepare the materials constituting polybasic nitrate molten salt according to the formula listed in table 15.
(117) Preparation method and test method are exactly same as the embodiments 15-17.
(118) The added silica sand (100 meshes) of product 7-9 occupies 15%, 30% and 45%.
(119) The test result of heat stability is close to embodiments 15-17. The highest loss rates of the prepared three kinds of products of the invention are 12%, 4% and 2% which is 30% lower than the contrast obviously.
(120) Adopt universal differential scanning calorimeter DSC (scan at normal pressure). The test result shows that the melting points of product 7-9 keep unchanged basically and the latent heat of phase change in increased.
Embodiments 24-26 Prepare Heat Transfer and Heat Storage Medium by Adding Silica Sand in Polybasic Nitrate System KNO.SUB.3.NaNO.SUB.3.CsNO.SUB.3.Ca(NO.SUB.3.).SUB.2
(121) The preparation method and test method of products 10-12 are the exactly same as embodiments 15-17.
(122) Silica sand (100 meshes) occupies 10%, 25% and 45% respectively. Contrasting molten sand without silica sand, it is the system corresponding with embodiments 25-27 in table 15.
(123) The test result of heat stability is close to embodiments 15-17. The highest loss of rate of three kinds of products prepared by the invention are 12%, 3% and 2% which is 30% lower than the contrast obviously.
(124) Adopt universal differential scanning calorimeter DSC (scan at normal pressure). The test result shows that the latent heat of phase change is increased comparing with the contrast, the melting points of product 10-11 keep unchanged basically and the melting point of product 12 is improved slightly.
Embodiment 27-32 Prepare Heat Transfer and Heat Storage Medium by Adding Silica Sand in Other Polybasic Nitrate System
(125) The preparation method and test method of product 13-18 is exactly same as the embodiments 16-18. The proportion of silica sand (100 meshes) of three formulas of each polybasic nitrate molten salt system are: 15%, 25% and 40%. Comparing with the molten salt without silica sand, it is the system corresponding with embodiments 27-32 in table 15.
(126) The heat stability test result shows that the highest loss rates of six kinds of products prepared by the invention are 11%, 2.5% and 1% which is 30% lower that the contrast obviously at 700 C. after insulating for 30 hours.
(127) Adopt universal differential scanning calorimeter DSC (scan at normal pressure). The test results show that the melting point of products 13-18 keeps unchanged and the latent heat of phase change is increased comparing with the contrast.
(128) The above experiment results show that the heat transfer and heat storage medium prepared by adding the silica sand in polybasic nitrate molten salt has slight corrosion on heat transfer and heat storage system. It has the following advances:
(129) It has the performance of heat transfer of nitrate molten salt and the upper limit operating temperature of polybasic nitrate is increased too. The operating temperature range is more wide and the heat stability is good.
(130) Large latent heat of phase change and high energy storage density lower the requirements on the size of heat storage system and energy. The utilization rate of energy is high and the energy-saving effect is good.
(131) The performance of conductivity for heat of the molten salt heat transfer and heat storage prepared by the invention is increased greatly. The shortcomings of poor performance of conductivity of nitrate molten salt and local overheating are overcame. It can be used widely in solar thermal power generation technical field.
Embodiment 33-36. Silica Sand Binary Carbonate Composite System
(132) The formula of binary carbonate system is shown as table 16.
(133) TABLE-US-00016 TABLE 16 The formula of binary carbonate molten salt in each embodiment Embodiment Binary carbonate Binary carbonate system formula no. system (part by weight)-comparison 33 K.sub.2CO.sub.3Na.sub.2CO.sub.3 Potassium carbonate: 30 parts. Sodium carbonate: 45 parts. 34 Potassium carbonate: 45 parts. Sodium carbonate: 30 parts. 35 Potassium carbonate: 60 parts. Sodium carbonate: 30 parts. 36 Potassium carbonate: 30 parts. Sodium carbonate: 60 parts.
Step 1. Prepare the materials constituting binary carbonate molten salt system according to the formula listed in table 16. Put them in the reactor, heat and stir to melt solid completely and then insulate for 0.5-1 h. The heating temperature is 80-120 C. over the temperature of phase change of molten salt.
Step 2. Disperse silica sand according to the proportion designed by the following experiments into molten binary carbonate salt and stir 1-2 h continuously to get silica sand composite carbonate molten salt which is colloidal.
(134) The silica sand (specification is 100 meshes) is added for the experimental design of the invention according to the following proportion gradient:
(135) The first group: silica sand occupies 1% of four kinds of silica sand composite binary carbonate molten salt heat transfer and heat storage medium. Obtain the first to the fourth products.
(136) The second group: silica sand occupies 10% of four kinds of silica sand composite binary carbonate molten salt heat transfer and heat storage medium. Obtain the fifth to the eighth products.
(137) The third group: silica sand occupies 20% of four kinds of silica sand composite binary carbonate molten salt heat transfer and heat storage medium. Obtain the ninth to the twelfth products.
(138) The fourth group: silica sand occupies 30% of four kinds of silica sand composite binary carbonate molten salt heat transfer and heat storage medium. Obtain the 13th to the sixth products.
(139) The fifth group: silica sand occupies 40% of four kinds of silica sand composite binary carbonate molten salt heat transfer and heat storage medium. Obtain the 17.sup.th to the 20th products.
(140) The sixth group: silica sand occupies 50% of four kinds of silica sand composite binary carbonate molten salt heat transfer and heat storage medium. Obtain the 21st to the 24.sup.th products.
(141) The contrast of each one product is the system of the corresponding original binary carbonate molten salt system of the product.
(142) Step 3. Latent Heat of Phase Change Test and Melting Point Test:
(143) Adopt universal differential scanning calorimeter DSC (scan at normal pressure).
(144) Test results show that the latent heat of phase change is increased obviously comparing with the contrast.
(145) The melting points of the products of the first group to the fourth group is reduced. The melting points are between 530560 C. The melting points of the products of the fifth group to that of the sixth group are improved slightly. It is around 600 C.
(146) Step 4. Heat Stability Test
(147) Carry out heat stability test for the obtained 24 kinds of heat transfer and heat storage mediums and four kinds of contrast binary carbonate molten salt
(148) The test is carried out by adopting weighting method: put 24 kinds of molten salts obtained in the embodiments 33-36 into nickel crucible and heat it in the temperature-controlled furnace. Carry out experiment starting from normal temperature. Take out experimental crucible at intervals and weigh by using analytical balance. If the weight of the sample is not reduced any more at certain temperature section, the temperature of the temperature-controlled furnace should be increased, and then take out experimental crucible at intervals to weigh and increase temperature after reaching another stable status.
(149) The result show that the heat stability of four kinds of the contrasts binary carbonate system is shown as follows:
(150) Heat for 100 hours at 800 C. The loss rate is 8%.
(151) Heat for 30 hours at 850 C. The loss rate is 8%.
(152) Heat for 30 hours at 900 C. The loss rate is 12%.
(153) Carry out heat stability test on 6 groups of 24 kinds of heat transfer and heat storage mediums obtained in embodiments 33-36. The results are shown on the table 17.
(154) TABLE-US-00017 TABLE 17 The statistical results of loss rate at each temperature Time (hour) 800 C. 850 C. 900 C. Product (100 (30 (30 group no. hours) hours) hours) The first <8% <8% <12% group The second <7% <7% <10.5% group The third <6% <6% <8.5% group The fourth <5% <5% <7% group The fifth <4.5% <4.5% <6% group The sixth <4% <4% <5.5% group
(155) It can be seen that the heat stability of the products of each group is increased relative to contrast after adding silica sand.
Embodiments 37-40 Silica Sand-Molten Salt Composite System Containing Lithium Carbonate
(156) See table 18 for the molten salt system containing lithium carbonate.
(157) TABLE-US-00018 TABLE 18 the formula of molten salt containing lithium carbonate Number of Molten salt containing Formula of molten salt containing lithium embodiment lithium carbonate carbonate(part by weight)-contrast 37 K.sub.2CO.sub.3Na.sub.2CO.sub.3NaClLi.sub.2CO.sub.3 Potassium carbonate: 20 parts. Sodium carbonate: 40 parts. Sodium chloride: 20 parts. Lithium carbonate: 10 parts. 38 Potassium carbonate: 25 parts. Sodium carbonate: 35 parts. Sodium chloride: 10 parts. Lithium carbonate: 8 parts. 49 Potassium carbonate: 45 parts. Sodium carbonate: 25 parts. Sodium chloride: 20 parts. Lithium carbonate: 5 parts. 40 Potassium carbonate: 60 parts. Sodium carbonate: 20 parts. Sodium chloride: 10 parts. Lithium carbonate: 10 parts.
Step 1. Prepare materials constituting molten salt system containing lithium carbonate according to the formula listed in table 18. Heat it in the reaction kettle and stir to melt solid completely and then insulate for 0.5-1 h. The heating temperature is 80-120 C. over the temperature of phase change of molten salt.
Step 2. Disperse silica sand into molten molten salt containing lithium carbonate according to the proportion designed by experiment and stir continuously for 1-2 h to obtain silica sand composite carbonate molten salt which is colloidal.
(158) The silica sand (specification 100 meshes) is added according to the following proportional gradient and design of the experiment.
(159) The first group: Silica sand occupies 1% of four kinds of silica sand composite carbonate molten salt heat transfer and heat storage mediums. Obtain the 25.sup.th to 28.sup.th products.
(160) The second group: Silica sand occupies 10% of four kinds of silica sand composite carbonate molten salt heat transfer and heat storage mediums. Obtain the 29.sup.th to 32.sup.nd products.
(161) The third group: Silica sand occupies 20% of four kinds of silica sand composite carbonate molten salt heat transfer and heat storage mediums. Obtain the 33rd to 36.sup.th products.
(162) The fourth group: Silica sand occupies 30% of four kinds of silica sand composite carbonate molten salt heat transfer and heat storage mediums. Obtain the 37.sup.th to 40.sup.th products.
(163) The fifth group: Silica sand occupies 40% of four kinds of silica sand composite carbonate molten salt heat transfer and heat storage mediums. Obtain the 41.sup.st to 44.sup.th products.
(164) The sixth group: Silica sand occupies 50% of four kinds of silica sand composite carbonate molten salt heat transfer and heat storage mediums. Obtain the 45.sup.th to 48.sup.th products.
(165) The contrast of each product is the corresponding molten salt system containing lithium carbonate of the product.
(166) Step 3 Latent Heat of Phase Change Test and Melting Test
(167) Adopt universal differential scanning calorimeter DSC (scan at normal pressure).
(168) Test results show that the latent heat of phase change is increased obviously comparing with the contrast.
(169) As far as the contrast is concerned,
(170) The melting points of the products of the first group to the fourth group are reduced. The melting point is between 320380 degrees Celsius
(171) The melting points of the fifth group and the sixth group are improved slightly which is around 400410 C.
(172) Step 4 Thermal Stability Test
(173) Carry out heat stability test on prepared and obtained 24 kinds of heat transfer and heat storage mediums and four kinds of contrasts of molten salt containing lithium carbonate.
(174) The test is carried out by adopting weighting method: put 24 kinds of molten salts obtained in embodiments 37-40 into nickel crucible respectively and heat it in the temperature-controlled furnace. Experiment starting from room temperature and take out experimental crucible at intervals and weigh by using analytical balance. If the weight of the sample is not reduced any more at certain temperature section, the temperature of temperature-controlled furnace should be increased, and then take out experiment crucible to weigh at intervals and increase temperature continuously after reaching another stable status.
(175) Results show that the thermal stability of four contrasts containing lithium carbonate system is shown as follows:
(176) Heat for 100 hours at 850 C. The loss rate is around 5%.
(177) Heat for 30 hours at 900 C. The loss rate is around 6%.
(178) Heat for 30 hours at 950 C. The loss rate is around 10%.
(179) Carry out heat stability test on six groups of 24 kinds of heat transfer and heat storage mediums obtained in embodiments 37-40. The result is shown on the table 19.
(180) TABLE-US-00019 TABLE 19 Statistical Result of Loss Rate at Each Temperature Time (hour) Product 850 C. 900 C. 950 C. group no. (100 hours) (30 hours) (30 hours) The first <4.9% <5.6% <9% group The second <4.2% <4.8% <8% group The third <3.8% <4.3% <7.1% group The fourth <3.3% <3.7% <5.8% group The fifth <3% <3.2% <5.5% group The sixth <2.5% <3% <5.1% group
(181) It can be seen that the heat stability of the products of each group is increased obviously after adding silica sand relative to contrasts.
Embodiments 41-43. Add Graphite in Ternary Nitrate System KNO.SUB.3.NaNO.SUB.3.Ca(NO.SUB.3.) to Prepare Heat Transfer and Heat Storage Medium
(182) Adopt the ternary nitrate molten salt system of embodiment 12-14. The method is the same as the method of step 1 of embodiments 8-11.
(183) Add graphite according to gradient.
(184) Embodiment 41 is the first group: Graphite occupies 1% of three kinds of silica sand composite ternary nitrate molten salt heat transfer and heat storage medium. Obtain the first one to the third products.
(185) Embodiment 42 is the second group: Graphite occupies 30% of three kinds of silica sand composite ternary nitrate molten salt heat transfer and heat storage medium. Obtain the fourth to the sixth products.
(186) Embodiment 43 is the third group: Graphite occupies 50% of three kinds of silica sand composite ternary nitrate molten salt heat transfer and heat storage medium. Obtain the seventh to the ninth products.
(187) Step 3. Latent Heat of Phase Change Test and Melting Point Test
(188) Adopt universal differential scanning calorimeter to scan (at normal pressure)
(189) Test results show that the latent heat of phase change is increased obviously. Compared with contrast, the melting points of the first group and the second group keep unchanged basically. The melting point of the third group is improved.
(190) Step 4 Thermal Stability Test
(191) Carry out heat stability test on prepared and obtained nine kinds of heat transfer and heat storage mediums by comparing ternary nitrate molten salt.
(192) Test is carried out by adopting weighting method: put nine kinds of molten salts into nickel crucible respectively and heat it in temperature-controlled furnace. Experiment starting from room temperature. Take out experiment crucible at intervals to weigh by using analytical balance. If the weight of the sample is not reduced any more, the temperature of temperature-controlled furnace should be increased, and then take out experiment crucible at intervals to weigh and increase temperature after reaching another stable status.
(193) Contrasting the stable temperature limit 550 C. of ternary nitrate system, when it is heated for 30 hours at 550 C. the loss rate is around 3%. The loss rate is around 8% when it is heated for 50 hours at 550 C. When it is heated for 30 hours at 650 C. the loss rate is around 5.5%. When it is heated for 50 hours, the loss rate is around 12%. When it is heated for 30 hours at 750 C. the loss rate is around 9%. When it is heated for 50 hours, the loss rate is around 17% at 750 C.
(194) Carry out thermal stability test for nine kinds of heat transfer and heat storage mediums obtained from embodiments 41-43.
(195) TABLE-US-00020 TABLE 19 Statistical Results of Loss Rate at 650 C. Product Time (hour) group no. 30 50 The first <4% <8% group The second <3.5% <6.8% group The third <2.9% <5.8% group
(196) TABLE-US-00021 TABLE 20 The statistical results of loss rate at 750 C. Product Time (hour) group no. 30 50 The first <6% <14% group The second <5% <12% group The third <4.5% <11.2% group
(197) It can be seen that the loss rate of the invented product at 750 C. is close to that of contrast at 550 C. The result is close to that with silica sand added. It can be operated stably for long time at 750 C.