Method for preparing organometallic composite material
11306200 · 2022-04-19
Assignee
Inventors
- Qun Chen (Changzhou, CN)
- Haiqun Chen (Changzhou, CN)
- Jian Lu (Changzhou, CN)
- Chunping Fang (Changzhou, CN)
- Wen Yi (Changzhou, CN)
- Feng LI (Changzhou, CN)
- Shuhua Wang (Changzhou, CN)
- Zhongjing Chen (Changzhou, CN)
- Lina Zhang (Changzhou, CN)
- Mingyang He (Changzhou, CN)
Cpc classification
C08L2205/03
CHEMISTRY; METALLURGY
C08K2201/005
CHEMISTRY; METALLURGY
B29C48/13
PERFORMING OPERATIONS; TRANSPORTING
B29C48/022
PERFORMING OPERATIONS; TRANSPORTING
C08L27/06
CHEMISTRY; METALLURGY
C08L97/02
CHEMISTRY; METALLURGY
C08L97/02
CHEMISTRY; METALLURGY
C08L27/06
CHEMISTRY; METALLURGY
B29C48/40
PERFORMING OPERATIONS; TRANSPORTING
B29C48/92
PERFORMING OPERATIONS; TRANSPORTING
B29C48/16
PERFORMING OPERATIONS; TRANSPORTING
International classification
C08L27/06
CHEMISTRY; METALLURGY
C08K3/30
CHEMISTRY; METALLURGY
B29C48/88
PERFORMING OPERATIONS; TRANSPORTING
B29C48/00
PERFORMING OPERATIONS; TRANSPORTING
Abstract
The present invention provides a method for preparing organometallic composite material, comprising: providing PVC resin, activated calcium carbonate, plant fiber, calcium stearate, barium sulfate, paraffin, sodium bicarbonate, zinc laurate, nanometre titanium dioxide, organometallic salt, shell powder, carbon nanotube, talcum powder and stabilizer; mixing and heating; subject to first cooling after extrusion and second cooling under vacuum; towing to obtain the organometallic composite material, wherein the organometallic salt is a benzoic acid metal salt mixture. The present method can significantly reduce the processing temperature of PVC composite by 20 to 50° C., and also increase the toughness and strength of the material so as to alleviate the exudation of the composite material as in the conventional technologies and extend the lifespan of the composite material.
Claims
1. A method for preparing a composite material, comprising: providing a PVC resin, an activated calcium carbonate, a plant fiber, calcium stearate, barium sulfate, paraffin wax, sodium bicarbonate, zinc laurate, nanometer-sized titanium dioxide, an organometallic salt, shell powder, carbon nanotubes, talcum powder, and a stabilizer to create a first mixture; mixing and heating the first mixture to obtain a second mixture; extruding the second mixture to obtain a molded article; subjecting the molded article to a first cooling to obtain a cooled molded article; subjecting the cooled molded article to a second cooling under vacuum to obtain the composite material.
2. The method of claim 1, wherein the organometallic salt is a benzoic acid metal salt represented by the following formula: ##STR00015## wherein n=1, 2 or 3; M is selected from copper, iron, zinc, magnesium, calcium, or combinations thereof.
3. The method of claim 1, wherein the PVC resin is from 50 to 70 parts by mass; the activated calcium carbonate is from 16 to 30 parts by mass; the plant fiber is from 2 to 6 parts by mass; the calcium stearate is from 4 to 14 parts by mass; the barium sulfate is from 2 to 8 parts by mass; the paraffin wax is from 12 to 18 parts by mass; the sodium bicarbonate is from 1 to 3 parts by mass; the zinc laurate is from 2 to 6 parts by mass; the nanometer-sized titanium dioxide is from 4 to 8 parts by mass; the organometallic salt is from 10 to 50 parts by mass; the shell powder is from 4 to 8 parts by mass; the carbon nanotubes are from 2 to 4 parts by mass; the talcum powder is from 3 to 5 parts by mass; and the stabilizer is from 2 to 4 parts by mass.
4. The method of claim 2, wherein the PVC resin is from 50 to 70 parts by mass; the activated calcium carbonate is from 16 to 30 parts by mass; the plant fiber is from 2 to 6 parts by mass, the calcium stearate is from 4 to 14 parts by mass; the barium sulfate is from 2 to 8 parts by mass; the paraffin wax is from 12 to 18 parts by mass; the sodium bicarbonate is from 1 to 3 parts by mass; the zinc laurate is from 2 to 6 parts by mass; the nanometer-sized titanium dioxide is from 4 to 8 parts by mass; the organometallic salt is from 10 to 50 parts by mass; the shell powder is from 4 to 8 parts by mass; the carbon nanotubes are from 2 to 4 parts by mass; the talcum powder is from 3 to 5 parts by mass; and the stabilizer is from 2 to 4 parts by mass.
5. The method of claim 1, wherein the mixing and heating comprises mixing at a first speed from 400 to 500 r/min for 1 to 2 hours at a first temperature from 100 to 120° C., followed by mixing at a second speed from 80 to 120 r/min for 30 to 50 minutes at a second temperature from 30 to 40° C., and wherein said extruding is performed at different temperatures according to different zones: 110 to 120° C. in zone 1; 125 to 135° C. in zone 2; 140 to 150° C. in zone 3; 165 to 175° C. in zone 4; and 105 to 110° C. in a confluence core, and wherein said first cooling is water cooling, and wherein said second cooling under vacuum has a temperature from −10 to −15° C.
6. The method of claim 1, wherein the mixing and heating comprises mixing at a speed of 450 r/min for 1.1 hours at a temperature of 101° C., followed by mixing at a speed of 80 r/min for 40 minutes at a temperature of 31° C.
7. A composite material prepared by the method according to claim 1, wherein the PVC resin is from 50 to 70 parts by mass; the activated calcium carbonate is from 16 to 30 parts by mass; the plant fiber is from 2 to 6 parts by mass; the calcium stearate is from 4 to 14 parts by mass; the barium sulfate is from 2 to 8 parts by mass; the paraffin wax is from 12 to 18 parts by mass; the sodium bicarbonate is from 1 to 3 parts by mass; the zinc laurate is from 2 to 6 parts by mass; the nanometer-sized titanium dioxide is from 4 to 8 parts by mass; the organometallic salt is from 10 to 50 parts by mass; the shell powder is from 4 to 8 parts by mass; the carbon nanotube is from 2 to 4 parts by mass; the talcum powder is from 3 to 5 parts by mass; and the stabilizer is from 2 to 4 parts by mass.
8. The composite material according to claim 7, wherein the organometallic salt is a benzoic acid metal salt represented by the following formula: ##STR00016## wherein n=1, 2 or 3; M is selected from copper, iron, zinc, magnesium, calcium, or combinations thereof.
9. The composite material according to claim 7, wherein the material has an exudation rate from 0.3% to 15%.
10. The composite material according to claim 8, wherein the material has an exudation rate from 0.3% to 15%.
Description
DETAILED DESCRIPTION
Example 1
(1) 60 parts of PVC resin (polymerization degree is 800 to 1300, the density is 1.38 g/cm.sup.3), 23 parts of activated calcium carbonate, 2 parts of plant fiber (mixture of bagasse, cotton and crop straw), 9 parts of calcium stearate, 2 parts of barium sulfate, 12 parts of paraffin, 1 part of sodium bicarbonate, 2 parts of zinc laurate, 4 parts of nanometre titanium dioxide (particle size 60 to 80 nm), 30 parts of organometallic salts, 4 parts of shell powder, 2 parts of carbon nanotubes (density: 2.1 g/cm.sup.3 at 20° C.), 3 parts of talcum powder and 2 parts of stabilizer (Barium-Zinc stabilizer, liquid) are provided, wherein the organometallic salts are benzoic acid metal salt mixture (purchased from Adamant Technological Environmental, forming agent, catalogue no.: WY-68) which has the following formula:
(2) ##STR00002##
(3) wherein n=1, 2 or 3; and M is selected from cations including copper, iron, zinc, magnesium, calcium, etc.; wherein the benzoic acid metal salt mixture includes one or more of benzoic acid metal salt, dibenzoic acid metal salt, tribenzoic acid metal salt or any combination thereof; according to the mass percentage, the amount of benzoic acid metal salt in organometallic salt is in a range from 70% to 80% by weight, and the dibenzoic acid metal salt is from 60% to 70% by weight of the remaining benzoic acid metal salt mixture other than the benzoic acid metal salt.
(4) The above-mentioned materials are added into a high-speed mixer, where the temperature is increased to 101° C., the mixing speed is 450 r/min, and mixing time is for 1.1 hours; after the dispersion, the temperature is reduced to 31° C., the mixing speed is adjusted to 80 r/min, and the mixing time is 40 minutes to obtain the mixture.
(5) The obtained mixture is extruded and shaped by twin-screw extruder, and the profile is obtained after water cooling. The settings of twin-screw extruder are: 110 to 120° C. (zone 1), 125 to 135° C. (zone 2), 140 to 150° C. (zone 3), 165 to 175° C. (zone 4), and 105 to 110° C. (confluence core); the profile is sent to −11° C., cooled in vacuum, towed, to obtain the final product.
Example 2
(6) 50 parts of PVC resin (polymerization degree is 1300, the density is 1.38 g/cm.sup.3), 16 parts of activated calcium carbonate, 2 parts of plant fiber (mixture of bagasse, cotton and crop straw), 6 parts of calcium stearate, 2 parts of barium sulfate, 12 parts of paraffin, 1 part of sodium bicarbonate, 2 parts of zinc laurate, 4 parts of nanometre titanium dioxide (particle size 60 to 80 nm), 10 parts of organometallic salts, 4 parts of shell powder, 2 parts of carbon nanotubes (density: 2.1 g/cm.sup.3 at 20° C.), 3 parts of talcum powder and 2 parts of stabilizer (Barium-Zinc stabilizer, liquid) are provided, wherein the organometallic salts is benzoic acid metal salt mixture (purchased from Adamant Technological Environmental, forming agent, catalogue no.: WY-68) which has the following formula:
(7) ##STR00003##
(8) wherein n=1, 2 or 3; M is selected from cations including copper, iron, zinc, magnesium, calcium, etc.; wherein the benzoic acid metal salt mixture includes one or more of benzoic acid metal salt, dibenzoic acid metal salt, tribenzoic acid metal salt or any combination thereof; according to the mass percentage, the amount of benzoic acid metal salt in organometallic salt is in a range from 70% to 80% by weight, and the dibenzoic acid metal salt is from 60% to 70% by weight of the remaining benzoic acid metal salt mixture other than the benzoic acid metal salt.
(9) The above-mentioned materials are added into a high-speed mixer, where the temperature is increased to 110° C., the mixing speed is 400 r/min, and mixing time is 1.5 hours; after the dispersion, the temperature is reduced to 35° C., the speed is adjusted to 105 r/min, and mixed for 40 minutes to obtain the mixture.
(10) The obtained mixture is extruded and shaped by twin-screw extruder, and the profile is obtained after water cooling. The settings of twin-screw extruder are: 110 to 120° C. (zone 1), 125 to 135° C. (zone 2), 140 to 150° C. (zone 3), 165 to 175° C. (zone 4), and 105 to 110° C. (confluence core); the profile is sent to −10° C., cooled in vacuum, towed, to obtain the final product.
Example 3
(11) 65 parts of PVC resin (polymerization degree is 1100, the density is 1.38 g/cm.sup.3), 24 parts of activated calcium carbonate, 3 parts of plant fiber (mixture of bagasse, cotton and crop straw), 10 parts of calcium stearate, 3 parts of barium sulfate, 14 parts of paraffin, 2 parts of sodium bicarbonate, 3 parts of zinc laurate, 6 parts of nanometre titanium dioxide (particle size 60 to 80 nm), 40 parts of organometallic salts, 5 parts of shell powder, 3 parts of carbon nanotubes (density: 2.1 g/cm.sup.3 at 20° C.), 3.5 parts of talcum powder and 2.5 parts of stabilizer (Barium-Zinc stabilizer, liquid) are provided, wherein the organometallic salts is benzoic acid metal salt mixture (purchased from Adamant Technological Environmental, forming agent, catalogue no.: WY-68) which has the following formula:
(12) ##STR00004##
(13) wherein n=1, 2 or 3; M is selected from cations including copper, iron, zinc, magnesium, calcium, etc.; wherein the benzoic acid metal salt mixture includes one or more of benzoic acid metal salt, dibenzoic acid metal salt, tribenzoic acid metal salt or any combination thereof; according to the mass percentage, the amount of benzoic acid metal salt in organometallic salt is in a range from 70% to 80% by weight, and the dibenzoic acid metal salt is from 60% to 70% by weight of the remaining benzoic acid metal salt mixture other than the benzoic acid metal salt.
(14) The above-mentioned materials are added into a high-speed mixer, where the temperature is increased to 120° C., the mixing speed is 500 r/min, and mixing time is 2 hours; after the dispersion, the temperature is reduced to 40° C., the mixing speed is adjusted to 120 r/min, and mixed for 50 minutes to obtain the mixture.
(15) The obtained mixture is extruded and shaped by twin-screw extruder, and the profile is obtained after water cooling. The settings of twin-screw extruder are: 110 to 120° C. (zone 1), 125 to 135° C. (zone 2), 140 to 150° C. (zone 3), 165 to 175° C. (zone 4), and 105 to 110° C. (confluence core); the profile is sent to −15° C., cooled in vacuum, towed, to obtain the final product.
Example 4
(16) 70 parts of PVC resin (polymerization degree is 1200, the density is 1.38 g/cm.sup.3), 30 parts of activated calcium carbonate, 6 parts of plant fiber (mixture of bagasse, cotton and crop straw), 12 parts of calcium stearate, 8 parts of barium sulfate, 18 parts of paraffin, 3 parts of sodium bicarbonate, 6 parts of zinc laurate, 8 parts of nanometre titanium dioxide (particle size 60 to 80 nm), 50 parts of organometallic salts, 8 parts of shell powder, 4 parts of carbon nanotubes (density: 2.1 g/cm.sup.3 at 20° C.), 5 parts of talcum powder and 4 parts of stabilizer (Barium-Zinc stabilizer, liquid) are provided, wherein the organometallic salts is benzoic acid metal salt mixture (purchased from Adamant Technological Environmental, forming agent, catalogue no.: WY-68) and its formula is as follows:
(17) ##STR00005##
(18) wherein n=1, 2 or 3; M is selected from cations including copper, iron, zinc, magnesium, calcium, etc.; wherein the benzoic acid metal salt mixture includes one or more of benzoic acid metal salt, dibenzoic acid metal salt, tribenzoic acid metal salt or any combination thereof; according to the mass percentage, the amount of benzoic acid metal salt in organometallic salt is in a range from 70% to 80% by weight, and the dibenzoic acid metal salt is from 60% to 70% by weight of the remaining benzoic acid metal salt mixture other than the benzoic acid metal salt.
(19) The above-mentioned materials are added into the high-speed mixer, where the temperature is increased to 90° C., the mixing speed to 450 r/min, and mixing time is 2 hours; after the dispersion, the temperature is reduced to 35° C., the mixing speed is adjusted to 120 r/min, and mixing time is 35 minutes to obtain the mixture.
(20) The obtained mixture is extruded and shaped by twin-screw extruder, and the profile is obtained after water cooling. The settings of twin-screw extruder are: 110 to 120° C. (zone 1), 125 to 135° C. (zone 2), 140 to 150° C. (zone 3), 165 to 175° C. (zone 4), and 105 to 110° C. (confluence core); the profile is sent to −13° C., cooled in vacuum, towed, to obtain the final product.
Example 5
(21) 60 parts of PVC resin (polymerization degree is 1300, the density is 1.38 g/cm.sup.3), 23 parts of activated calcium carbonate, 2 parts of plant fiber (mixture of bagasse, cotton and crop straw), 9 parts of calcium stearate, 2 parts of barium sulfate, 12 parts of paraffin, 1 part of sodium bicarbonate, 2 parts of zinc laurate, 4 parts of nanometre titanium dioxide (particle size 60 to 80 nm), 30 parts of organometallic salts, 4 parts of shell powder, 2 parts of carbon nanotubes (density: 2.1 g/cm.sup.3 at 20° C.), 3 parts of talcum powder and 2 parts of stabilizer (Barium-Zinc stabilizer, liquid) are provided, wherein the organometallic salts is benzoic acid metal salt mixture (purchased from Adamant Technological Environmental, forming agent, catalogue no.: WY-68) which has the following formula:
(22) ##STR00006##
(23) wherein n=1, 2 or 3; M is selected from cations including copper, iron, zinc, magnesium, calcium, etc.; wherein the benzoic acid metal salt mixture includes one or more of benzoic acid metal salt, dibenzoic acid metal salt, tribenzoic acid metal salt or any combination thereof; according to the mass percentage, the amount of benzoic acid metal salt in organometallic salt is in a range from 70% to 80% by weight, and the dibenzoic acid metal salt is from 60% to 70% by weight of the remaining benzoic acid metal salt mixture other than the benzoic acid metal salt.
(24) The above-mentioned materials are added into the high-speed mixer, where the temperature is increased to 110° C., the mixing speed is 400 r/min, and mixing time is 1.5 hours; after the dispersion, the temperature is reduced to 35° C., the mixing speed is adjusted to 105 r/min, and mixing time is 40 minutes to obtain the mixture.
(25) The obtained mixture is extruded and shaped by twin-screw extruder, and the profile is obtained after water cooling. The settings of twin-screw extruder are: 110 to 120° C. (zone 1), 125 to 135° C. (zone 2), 140 to 150° C. (zone 3), 165 to 175° C. (zone 4), and 105 to 110° C. (confluence core); the profile is sent to −10° C., cooled in vacuum, towed, and obtain the final product.
Example 6
(26) 65 parts of PVC resin (polymerization degree is 1100, the density is 1.38 g/cm.sup.3), 24 parts of activated calcium carbonate, 3 parts of plant fiber (mixture of bagasse, cotton and crop straw), 10 parts of calcium stearate, 3 parts of barium sulfate, 14 parts of paraffin, 2 parts of sodium bicarbonate, 3 parts of zinc laurate, 6 parts of nanometre titanium dioxide (particle size 60 to 80 nm), 40 parts of organometallic salts, 5 parts of shell powder, 3 parts of carbon nanotubes (density: 2.1 g/cm.sup.3 at 20° C.), 3.5 parts of talcum powder and 2.5 parts of stabilizer (Barium-Zinc stabilizer, liquid) are provided, wherein the organometallic salts is benzoic acid metal salt mixture (purchased from Adamant Technological Environmental, forming agent, catalogue no.: WY-68) which has the following formula:
(27) ##STR00007##
(28) wherein n=1, 2 or 3; M is selected from cations including copper, iron, zinc, magnesium, calcium, etc.; wherein the benzoic acid metal salt mixture includes one or more of benzoic acid metal salt, dibenzoic acid metal salt, tribenzoic acid metal salt or any combination thereof; according to the mass percentage, the amount of benzoic acid metal salt in organometallic salt is in a range from 70% to 80% by weight, and the dibenzoic acid metal salt is from 60% to 70% by weight of the remaining benzoic acid metal salt mixture other than the benzoic acid metal salt.
(29) The above-mentioned materials are added into the high-speed mixer, the temperature is increased to 120° C., the mixing speed is 500 r/min, and mixing time is 2 hours; after the dispersion, the temperature is reduced to 40° C., the mixing speed is adjusted to 120 r/min, and mixing time is 50 minutes to obtain the mixture.
(30) The obtained mixture is extruded and shaped by twin-screw extruder, and the profile is obtained after water cooling. The settings of twin-screw extruder are: 110 to 120° C. (zone 1), 125 to 135° C. (zone 2), 140 to 150° C. (zone 3), 165 to 175° C. (zone 4), and 105 to 110° C. (confluence core); the profile is sent to −15° C., cooled in vacuum, towed, to obtain the final product.
Example 7
(31) 70 parts of PVC resin (polymerization degree is 1300, the density is 1.38 g/cm.sup.3), 30 parts of activated calcium carbonate, 6 parts of plant fiber (mixture of bagasse, cotton and crop straw), 12 parts of calcium stearate, 8 parts of barium sulfate, 18 parts of paraffin, 3 parts of sodium bicarbonate, 6 parts of zinc laurate, 8 parts of nanometre titanium dioxide (particle size 60 to 80 nm), 50 parts of organometallic salts, 8 parts of shell powder, 4 parts of carbon nanotubes (density: 2.1 g/cm.sup.3 at 20° C.), 5 parts of talcum powder and 4 parts of stabilizer (Barium-Zinc stabilizer, liquid) are provided, wherein the organometallic salts is benzoic acid metal salt mixture (purchased from Adamant Technological Environmental, forming agent, catalogue no.: WY-68) which has the following formula:
(32) ##STR00008##
(33) wherein n=1, 2 or 3; M is selected from cations including copper, iron, zinc, magnesium, calcium, etc.; wherein the benzoic acid metal salt mixture includes one or more of benzoic acid metal salt, dibenzoic acid metal salt, tribenzoic acid metal salt or any combination thereof; according to the mass percentage, the amount of benzoic acid metal salt in organometallic salt is in a range from 70% to 80% by weight, and the dibenzoic acid metal salt is from 60% to 70% by weight of the remaining benzoic acid metal salt mixture other than the benzoic acid metal salt.
(34) The above-mentioned materials are into the high-speed mixer, the temperature is increased to 90° C., the mixing speed is 450 r/min, and mixing time is 2 hours; after the dispersion, the mixing temperature is reduced to 35° C., the mixing speed is adjusted to 120 r/min, and the mixing time is 35 minutes to obtain the mixture.
(35) The obtained mixture is extruded and shaped by twin-screw extruder, and the profile is obtained after water cooling. The settings of twin-screw extruder are: 110 to 120° C. (zone 1), 125 to 135° C. (zone 2), 140 to 150° C. (zone 3), 165 to 175° C. (zone 4), and 105 to 110° C. (confluence core); the profile is sent to −13° C., cooled in vacuum, towed, to obtain the final product.
Example 8
(36) 60 parts of PVC resin (polymerization degree is 1000, the density is 1.38 g/cm.sup.3), 23 parts of calcium carbonate, 2 parts of plant fiber (mixture of bagasse, cotton and crop straw), 9 parts of calcium stearate, 2 parts of barium sulfate, 12 parts of paraffin, 1 part of sodium bicarbonate, 2 parts of zinc laurate, 4 parts of nanometre titanium dioxide (particle size 60 to 80 nm), 30 parts of organometallic salts, 4 parts of shell powder, 2 parts of carbon nanotubes (density: 2.1 g/cm.sup.3 at 20° C.), 3 parts of talcum powder and 2 parts of stabilizer (Barium-Zinc stabilizer, liquid) are provided, wherein the organometallic salts is benzoic acid metal salt mixture (purchased from Adamant Technological Environmental, forming agent, catalogue no.: WY-68) which has the following formula:
(37) ##STR00009##
(38) wherein n=1, 2 or 3; M is selected from cations including copper, iron, zinc, magnesium, calcium, etc.; wherein the benzoic acid metal salt mixture includes one or more of benzoic acid metal salt, dibenzoic acid metal salt, tribenzoic acid metal salt or any combination thereof; according to the mass percentage, the amount of benzoic acid metal salt in organometallic salt is in a range from 70% to 80% by weight, and the dibenzoic acid metal salt is from 60% to 70% by weight of the remaining benzoic acid metal salt mixture other than the benzoic acid metal salt.
(39) The above-mentioned materials are added into the high-speed mixer, where the temperature is increased to 101° C., the mixing speed is 450 r/min, and mixing time is 1.1 hours; after the dispersion, the temperature is reduced to 31° C., the mixing speed is adjusted to 80 r/min, and mixing time is 40 minutes to obtain the mixture.
(40) The obtained mixture is extruded and shaped by twin-screw extruder, and the profile is obtained after water cooling. The settings of twin-screw extruder are: 110 to 120° C. (zone 1), 125 to 135° C. (zone 2), 140 to 150° C. (zone 3), 165 to 175° C. (zone 4), and 105 to 110° C. (confluence core); the profile is sent to −11° C., cooled in vacuum, towed, and obtain the final product.
Example 9
(41) 60 parts of PVC resin (polymerization degree is 1000, the density is 1.38 g/cm.sup.3), 23 parts of activated calcium carbonate, 2 parts of plant fiber (mixture of bagasse, cotton and crop straw), 9 parts of calcium stearate, 2 parts of barium sulfate, 12 parts of paraffin, 1 part of sodium bicarbonate, 2 parts of zinc laurate, 4 parts of nanometre titanium dioxide (particle size 60 to 80 nm), 30 parts of organometallic salts, 4 parts of shell powder, 2 parts of carbon nanotubes (density: 2.1 g/cm.sup.3 at 20° C.), 3 parts of talcum powder and 2 parts of stabilizer (Barium-Zinc stabilizer, liquid) are provided, wherein the organometallic salts is benzoic acid metal salt mixture (purchased from Adamant Technological Environmental, forming agent, catalogue no.: WY-68) which has the following formula:
(42) ##STR00010##
(43) wherein n=1, 2 or 3; M is selected from cations including copper, iron, zinc, magnesium, calcium, etc.; wherein the benzoic acid metal salt mixture includes one or more of benzoic acid metal salt, dibenzoic acid metal salt, tribenzoic acid metal salt or any combination thereof; according to the mass percentage, the amount of benzoic acid metal salt in organometallic salt is in a range from 70% to 80% by weight, and the dibenzoic acid metal salt is from 60% to 70% by weight of the remaining benzoic acid metal salt mixture other than the benzoic acid metal salt.
(44) The above-mentioned materials are added into the high-speed mixer, raise the temperature to 101° C., the mixing speed is 450 r/min, and mixing time is 1.1 hours; after the dispersion, the temperature is reduced to 31° C., the mixing speed is adjusted to 80 r/min, and the mixing time is 40 minutes to obtain the mixture.
(45) The obtained mixture is extruded and shaped by twin-screw extruder, and the profile is obtained after water cooling. The settings of twin-screw extruder are: 110 to 120° C. (zone 1), 125 to 135° C. (zone 2), 140 to 150° C. (zone 3), 165 to 175° C. (zone 4), and 105 to 110° C. (confluence core); the profile is sent to −11° C., cooled in vacuum, towed, to obtain the final product.
Example 10
(46) 60 parts of PVC resin (polymerization degree is 900, the density is 1.38 g/cm.sup.3), 23 parts of activated calcium carbonate, 2 parts of plant fiber (mixture of bagasse, cotton and crop straw), 9 parts of calcium stearate, 2 parts of barium sulfate, 12 parts of paraffin, 1 part of sodium bicarbonate, 2 parts of zinc laurate, 4 parts of nanometre titanium dioxide (particle size 60 to 80 nm), 30 parts of organometallic salts, 4 parts of shell powder, 2 parts of carbon nanotubes (density: 2.1 g/cm.sup.3 at 20° C.), 3 parts of talcum powder and 2 parts of stabilizer (Barium-Zinc stabilizer, liquid) are provided, wherein the organometallic salts is benzoic acid metal salt mixture (purchased from Adamant Technological Environmental, forming agent, catalogue no.: WY-68) which has the following formula:
(47) ##STR00011##
(48) wherein n=1, 2 or 3; M is selected from cations including copper, iron, zinc, magnesium, calcium, etc.; wherein the benzoic acid metal salt mixture includes one or more of benzoic acid metal salt, dibenzoic acid metal salt, tribenzoic acid metal salt or any combination thereof; according to the mass percentage, the amount of benzoic acid metal salt in organometallic salt is in a range from 70% to 80% by weight, and the dibenzoic acid metal salt is from 60% to 70% by weight of the remaining benzoic acid metal salt mixture other than the benzoic acid metal salt.
(49) The above-mentioned materials are added into the high-speed mixer, where the temperature is increased to 101° C., the mixing speed is 450 r/min, and mixing time is 1.1 hours; after the dispersion, the temperature is reduced to 31° C., the mixing speed is adjusted to 80 r/min, and mixing time is 40 minutes to obtain the mixture.
(50) The obtained mixture is extruded and shaped by twin-screw extruder, and the profile is obtained after water cooling. The settings of twin-screw extruder are: 110 to 120° C. (zone 1), 125 to 135° C. (zone 2), 140 to 150° C. (zone 3), 165 to 175° C. (zone 4), and 105 to 110° C. (confluence core); the profile is sent to −11° C., cooled in vacuum, towed, to obtain the final product.
Example 11
(51) 60 parts of PVC resin (polymerization degree is 800, the density is 1.38 g/cm.sup.3), 20 parts of activated calcium carbonate, 2 parts of plant fiber (mixture of bagasse, cotton and crop straw), 9 parts of calcium stearate, 2 parts of barium sulfate, 12 parts of paraffin, 1 part of sodium bicarbonate, 2 parts of zinc laurate, 4 parts of nanometre titanium dioxide (particle size 60 to 80 nm), 30 parts of organometallic salts, 4 parts of shell powder, 2 parts of carbon nanotubes (density: 2.1 g/cm.sup.3 at 20° C.), 3 parts of talcum powder and 2 parts of stabilizer (Barium-Zinc stabilizer, liquid) are provided, wherein the organometallic salts is benzoic acid metal salt mixture (purchased from Adamant Technological Environmental, forming agent, catalogue no.: WY-68) which has the following formula:
(52) ##STR00012##
(53) wherein n=1, 2 or 3; M is selected from cations including copper, iron, zinc, magnesium, calcium, etc.; wherein the benzoic acid metal salt mixture includes one or more of benzoic acid metal salt, dibenzoic acid metal salt, tribenzoic acid metal salt or any combination thereof; according to the mass percentage, the amount of benzoic acid metal salt in organometallic salt is in a range from 70% to 80% by weight, and the dibenzoic acid metal salt is from 60% to 70% by weight of the remaining benzoic acid metal salt mixture other than the benzoic acid metal salt.
(54) The above-mentioned materials are added into the high-speed mixer, the temperature is increased to 90° C., the mixing speed is 450 r/min, and mixing time is 2 hours; after the dispersion, the temperature is reduced to 35° C., the mixing speed is adjusted to 120 r/min, and mixing time is 35 minutes to obtain the mixture.
(55) The obtained mixture is extruded and shaped by twin-screw extruder, and the profile is obtained after water cooling. The settings of twin-screw extruder are: 110 to 120° C. (zone 1), 125 to 135° C. (zone 2), 140 to 150° C. (zone 3), 165 to 175° C. (zone 4), and 105 to 110° C. (confluence core); the profile is sent to −13° C., cooled in vacuum, towed, to obtain the final product.
Example 12
(56) 60 parts of PVC resin (polymerization degree is 1200, the density is 1.38 g/cm.sup.3), 25 parts of activated calcium carbonate, 3.5 parts of plant fiber (mixture of bagasse, cotton and crop straw), 10 parts of calcium stearate, 2 parts of barium sulfate, 14 parts of paraffin, 2 parts of sodium bicarbonate, 3 parts of zinc laurate, 3 parts of nanometre titanium dioxide (particle size 60 to 80 nm), 30 parts of organometallic salts, 3 parts of shell powder, 3 parts of carbon nanotubes (density: 2.1 g/cm.sup.3 at 20° C.), 3 parts of talcum powder and 3 parts of stabilizer (Barium-Zinc stabilizer, liquid) are provided, wherein the organometallic salts is benzoic acid metal salt mixture (purchased from Adamant Technological Environmental, forming agent, catalogue no.: WY-68) which has the following formula:
(57) ##STR00013##
(58) wherein n=1, 2 or 3; M is selected from cations including copper, iron, zinc, magnesium, calcium, etc.; wherein the benzoic acid metal salt mixture includes one or more of benzoic acid metal salt, dibenzoic acid metal salt, tribenzoic acid metal salt or any combination thereof; according to the mass percentage, the amount of benzoic acid metal salt in organometallic salt is in a range from 70% to 80% by weight, and the dibenzoic acid metal salt is from 60% to 70% by weight of the remaining benzoic acid metal salt mixture other than the benzoic acid metal salt.
(59) The above-mentioned materials are added into the high-speed mixer, where the temperature is increased to 101° C., the mixing speed to 450 r/min, and mixing time is 1.1 hours; after the dispersion, the temperature is reduced to 31° C., the mixing speed is adjusted to 80 r/min, and mixing time is 40 minutes to obtain the mixture.
(60) The obtained mixture is extruded and shaped by twin-screw extruder, and the profile is obtained after water cooling. The settings of twin-screw extruder are: 110 to 120° C. (zone 1), 125 to 135° C. (zone 2), 140 to 150° C. (zone 3), 165 to 175° C. (zone 4), and 105 to 110° C. (confluence core); the profile is sent to −11° C., cooled in vacuum, towed, to obtain the final product.
Example 13
(61) 60 parts of PVC resin (polymerization degree is 1200, the density is 1.38 g/cm.sup.3), 23 parts of activated calcium carbonate, 4 parts of plant fiber (mixture of bagasse, cotton and crop straw), 9 parts of calcium stearate, 5 parts of barium sulfate, 15 parts of paraffin, 1.5 parts of sodium bicarbonate, 4 parts of zinc laurate, 6 parts of nanometre titanium dioxide (particle size 60 to 80 nm), 30 parts of organometallic salts, 6 parts of shell powder, 3 parts of carbon nanotubes (density: 2.1 g/cm.sup.3 at 20° C.), 4 parts of talcum powder and 3 parts of stabilizer (Barium-Zinc stabilizer, liquid) are provided, wherein the organometallic salts is benzoic acid metal salt mixture (purchased from Adamant Technological Environmental, forming agent, catalogue no.: WY-68) which has the following formula:
(62) ##STR00014##
(63) wherein n=1, 2 or 3; M is selected from cations including copper, iron, zinc, magnesium, calcium, etc.; wherein the benzoic acid metal salt mixture includes one or more of benzoic acid metal salt, dibenzoic acid metal salt, tribenzoic acid metal salt or any combination thereof; and according to the mass percentage, the amount of benzoic acid metal salt in organometallic salt is in a range from 70% to 80% by weight, and the dibenzoic acid metal salt is from 60% to 70% by weight of the remaining benzoic acid metal salt mixture other than the benzoic acid metal salt.
(64) The above-mentioned materials are added into the high-speed mixer, where the temperature is increased to 101° C., the mixing speed is 450 r/min, and mixing time is 1.1 hours; after the dispersion, the temperature is reduced to 31° C., the mixing speed is adjusted to 80 r/min, and mixing time is 40 minutes to obtain the mixture.
(65) The obtained mixture is extruded and shaped by twin-screw extruder, and the profile is obtained after water cooling. The settings of twin-screw extruder are: 110 to 120° C. (zone 1), 125 to 135° C. (zone 2), 140 to 150° C. (zone 3), 165 to 175° C. (zone 4), and 105 to 110° C. (confluence core); the profile is sent to −11° C., cooled in vacuum, towed, to obtain the final product.
Comparative Example 1
(66) 58 parts of PVC resin (polymerization degree is 1400, the density is 1.38 g/cm.sup.3), 17 parts of activated calcium carbonate, 3 parts of plant fiber (mixture of bagasse, cotton and crop straw), 6 parts of calcium stearate, 3 parts of barium sulfate, 13 parts of paraffin, 1.5 parts of sodium bicarbonate, 2.5 parts of zinc laurate, 3 parts of nanometre titanium dioxide (particle size 60 to 80 nm), 5 parts of shell powder, 2 parts of carbon nanotubes (density: 2.1 g/cm.sup.3 at 20° C.), 3 parts of talcum powder and 2 parts of stabilizer (Barium-Zinc stabilizer, liquid) are provided.
(67) The above-mentioned materials are added into the high-speed mixer, where the temperature is increased to 101° C., the mixing speed is 450 r/min, and mixing time is 1.1 hours; after the dispersion, the temperature is reduced to 31° C., the mixing speed is 80 r/min, and mixing time is 40 minutes to obtain the mixture.
(68) The obtained mixture is extruded and shaped by twin-screw extruder, and the profile is obtained after water cooling. The settings of twin-screw extruder are: 110 to 120° C. (zone 1), 125 to 135° C. (zone 2), 140 to 150° C. (zone 3), 165 to 175° C. (zone 4), and 105 to 110° C. (confluence core); the profile is sent to −11° C., cooled in vacuum, towed, to obtain the final product.
Comparative Example 2
(69) 74 parts of PVC resin (polymerization degree is 1100, the density is 1.38 g/cm.sup.3), 32 parts of activated calcium carbonate, 6.5 parts of plant fiber (mixture of bagasse, cotton and crop straw), 14 parts of calcium stearate, 8 parts of barium sulfate, 18 parts of paraffin, 2 parts of sodium bicarbonate, 4 parts of zinc laurate, 6 parts of nanometre titanium dioxide (particle size 60 to 80 nm), 12 parts of plasticizers, 6 parts of shell powder, 6 parts of carbon nanotubes (density: 2.1 g/cm.sup.3 at 20° C.), 5 parts of talcum powder and 4 parts of stabilizer (Barium-Zinc stabilizer, liquid) are provided.
(70) The above-mentioned materials are added into the high-speed mixer, the temperature is increased to 110° C., the mixing speed is 400 r/min, and mixing time is 1.5 hours; after the dispersion, the temperature is reduced to 35° C., the mixing speed is adjusted to 105 r/min, and mixing time is 40 minutes to obtain the mixture.
(71) The obtained mixture is extruded and shaped by twin-screw extruder, and the profile is obtained after water cooling. The settings of twin-screw extruder are: 110 to 120° C. (zone 1), 125 to 135° C. (zone 2), 140 to 150° C. (zone 3), 165 to 175° C. (zone 4), and 105 to 110° C. (confluence core); the profile is sent to −15° C., cooled in vacuum, towed, to obtain the final product.
(72) The performance tests were carried out on the PVC final products prepared in the comparison 1 to 2 and the embodiments 1 to 13, and the results are shown in table-1.
(73) TABLE-US-00001 TABLE 1 Performance tests of Comparative Examples 1 to 2 and Examples 1 to 13 tensile elongation Processing impact Exudation strength at break temperature strength rate (MPa) (%) (° C.) (KJ/m.sup.2) (%) Example 1 55.6 283.6 150 39.2 2 Example 2 53.8 235.9 170 33.1 8 Example 3 53.9 256.1 160 36.3 7 Example 4 52.6 223.6 180 32.7 9 Example 5 52.3 221.5 175 34.5 10 Example 6 53.2 227.8 170 32.1 12 Example 7 50.6 217.1 185 31.9 13 Example 8 48.7 190.5 175 31.1 16 Example 9 46.3 185.3 180 29.7 18 Example 10 44.5 180.2 185 27.8 21 Example 11 42.6 160.4 190 26.3 23 Example 12 65 335.7 150 51.3 0.3 Example 13 54.8 274.9 160 37.8 1.5 Comparative 34.3 130.6 180 24.9 25 Example 1 Comparative 36.7 140.8 185 25.7 27 Example 2 *Test conditions for the exudation rate: the exudation mass to the original total mass of the composite material is measured under the dry condition and the temperature from 50 to 60° C. after 2 weeks; the processing temperature is the temperature of the barrel during the injection process.
(74) According to the above data, with the addition of the organometallic salt, the improvement of the coordination relationship between each substance in the material might be due to the change of the reaction site with PVC. Compared with the comparative examples, the organometallic composite material possesses with higher tensile strength, elongation at break and significantly lower exudation rate. Therefore, the composite material has not only lower processing temperature, but also better toughness and is not easy to break.