Advanced lead-free radiation protection materials utilizing modified brine sludge composition and the process thereof

Abstract

The novel process enables designing of raw materials and processing parameters, enabling synergistic and simultaneous chemical reactions among the various reactants of the design mix of chemical precursor of brine sludge which includes barium sulphate, magnesium hydroxide, calcium carbonate, sodium chloride, silica, aluminum containing compounds necessary for developing highly efficient shielding phases leading to homogenous matrix of shielding materials.

Claims

1. A process for making an advanced lead-free radiation protection material utilizing modified brine sludge composition, the process comprising: a. drying of 200 g-800 g of brine sludge in an air oven at 100° C.-110° C. for a period of 1-2 hours to produce a heat-treated brine sludge, followed by simultaneous solid state reaction processing and dry grinding with 20-90 g of tungsten powder and 10 g-60 g metakaolin for a period of 2-4 hours; b. after step a, adding and grinding 2 g-8 g potassium hydroxide for a period of 1-2 hrs and further adding and grinding 1 g-4 g potassium silicate for a period of 1-2 hrs to obtain fine homogeneous radiation protection powder of modified brine sludge composition; c. after step b, adding and thoroughly blending with 4 ml-16 ml of water and compacting in a steel mold by providing hydraulic pressure in the range of 100-300 kg/cm.sup.2 to obtain tiles; and d. after step c, heating the tiles in a furnace in the temperature range of 900° C.-1100° C. for a period of 1-2 hours to obtain the advanced lead-free radiation protection material.

2. The process as claimed in claim 1, wherein in step a drying of 200 g-800 g of brine sludge is carried out in an air oven at 100° C. for a period of 1-2 hours.

3. The process as claimed in claim 1, wherein the solid state reaction processing is carried out by mechano-chemical stimulation of the heat-treated brine sludge.

4. The process as claimed in claim 1, wherein compacting is carried out in a steel mold by providing hydraulic pressure in the range of 100-300 kg/cm.sup.2 to obtain tiles of dimensions 10 cm×10 cm×6-10 mm.

Description

DETAILED DESCRIPTION OF THE INVENTION

(1) The invention will now be described in detail in connection with certain preferred and optional embodiments, so that various aspects thereof may be more fully understood and appreciated.

Definitions

(2) For convenience, before further description of the present disclosure, certain terms employed in the specification, and examples are delineated here. These definitions should be read in the light of the remainder of the disclosure and understood as by a person of skill in the art. The terms used herein have the meanings recognized and known to those of skill in the art, however, for convenience and completeness, particular terms and their meanings are set forth below.

(3) The articles “a”, “an” and “the” are used to refer to one or to more than one (i.e., to at least one) of the grammatical object of the article.

(4) The terms “comprise” and “comprising” are used in the inclusive, open sense, meaning that additional elements may be included. It is not intended to be construed as “consists of only”.

(5) Throughout this specification, unless the context requires otherwise the word “comprise”, and variations such as “comprises” and “comprising”, will be understood to imply the inclusion of a stated element or step or group of element or steps but not the exclusion of any other element or step or group of element or steps.

(6) Ratios, concentrations, amounts, and other numerical data may be presented herein in a range format. It is to be understood that such range format is used merely for convenience and brevity and should be interpreted flexibly to include not only the numerical values explicitly recited as the limits of the range, but also to include all the individual numerical values or sub-ranges encompassed within that range as if each numerical value and sub-range is explicitly recited. For example, a temperature in the range of 100° C. to 110° C. should be interpreted to include not only the explicitly recited limits of 100° C. to 110° C. but also to include sub-ranges, such as 101° C. to 109° C., and so forth, as well as individual amounts, within the specified ranges, such as 100.0° C., 107.3° C. and 110° C.

(7) The present disclosure is not to be limited in scope by the specific embodiments described herein, which are intended for the purposes of exemplification only. Functionally-equivalent products, compositions, and methods are clearly within the scope of the disclosure, as described herein.

(8) The present invention provides an advanced lead-free radiation protection materials utilizing modified brine sludge composition and the process thereof. The process enables designing of raw materials and processing parameters, enabling synergistic and simultaneous chemical reactions among the various reactants of the design mix of chemical precursor of brine sludge which includes barium sulphate, magnesium hydroxide, calcium carbonate, sodium chloride, silica, aluminum containing compounds necessary for developing highly efficient shielding phases leading to homogenous matrix of shielding materials. The present invention involves processes like drying, powdering and mechano-chemical dry grinding of brine sludge with tungsten metal powder, metakaolin, potassium hydroxide, potassium silicate to obtain the modified brine sludge composition and further followed by sintering, for developing homogeneous advanced radiation protection material.

(9) The present invention also provides radiation protection phases by chemical designing and mineralogically formulating compositions based on various precursors of chemicals present in brine sludge along with other chemical precursors. The present invention provides a simultaneous synthesis of desired multi elemental, multi phased, shielding phases lead to the formation of fine homogeneous radiation protection matrix.

(10) Further the developed process also enables conversion of toxic elements like chromium, zinc, copper and vanadium, present in brine sludge in obtaining additional lead-free shielding phases and thus enables converting a toxic waste material in to a highly value-added advanced radiation protection material possess homogeneous radiation shielding matrix. The process involves the modified shielding powder so obtained and is having multi shielding phases and multi crystal phases due to presence of multi elements like Ba, W, Ca, Si, Al, Na, K etc. The process provides desired novel shielding phases by chemical designing and mineralogically formulating compositions based on various precursors of chemicals present in brine sludge along with other chemical precursors. Additionally, the present invention provides desired mineralogical phases necessary for obtaining uniform and homogenous advanced radiation protection materials. The process provides designing of raw materials and processing parameters, enabling synergistic and simultaneous chemical reactions among the various reactants of the design mix of raw materials.

(11) The process enables conversion of toxic elements like chromium, zinc, copper and vanadium, present in brine sludge into non-toxic form and leading to development of lead-free shielding phases. And further convert a toxic brine sludge waste material in to a highly value-added advanced radiation shielding materials possess homogeneous radiation protection matrix. Also, the process provides a complete usage of toxic chloral-alkali industry waste namely brine sludge. The process of the present disclosure utilizes and saves the cost of chemicals inherently present in brine sludge otherwise required for making advanced lead-free radiation protection materials. And further solves the disposal problem of toxic brine sludge waste by utilizing it for the development of advanced material useful in strategic sector and to save the environment all over the world.

(12) To overcome the drawbacks of the hitherto to known processes, the present process simultaneous and synergistic chemical reactions of various mineralogical and chemical compounds which includes barium sulphate, magnesium hydroxide, calcium carbonate, sodium chloride, silica, aluminum containing compounds of brine sludge along with complementary chemical compound namely tungsten powder, metakaolin, potassium hydroxide and potassium silicate to obtain the fine homogeneous powder of modified brine sludge composition for developing homogeneous advanced radiation protection materials. The process involves developing of desired shielding phases possessing uniform and homogenous protection matrix in the developed advanced radiation protection material. Further the process involves designing of raw materials compositions and processing parameters, enabling synergistic and simultaneous chemical reactions among the various reactants of the design mix of raw materials. The modified shielding powder so obtained has multi shielding phases and multi crystal phases due to presence of multi elements like Ba, W, Ca, Si, Al, Na, K etc.

(13) The process provides desired novel shielding phases by chemical designing and mineralogically formulating compositions based on various precursors of chemicals present in brine sludge along with other chemical precursors. The process enables developing of desired mineralogical phases necessary for obtaining uniform and homogenous advanced radiation protection materials. Therefore, the process of the present invention enables for making “advanced lead-free radiation protection materials utilizing modified brine sludge composition and the process thereof” by mechano-chemical activation of heat-treated brine sludge useful for obtaining modified brine sludge composition for developing homogeneous advanced radiation protection materials. Further the use of developed “advanced lead-free radiation protection materials utilizing modified brine sludge composition” lies in the areas of radiation shielding applications e.g. diagnostic radiation installations such as diagnostic X-ray and CT scanner room, to other strategic radiation shielding installation.

(14) Accordingly the present invention provides a process for making advanced lead-free radiation protection material utilizing modified brine sludge composition the process comprising drying of 200 g-800 g of brine sludge in an air oven at 100° C.-110° C. for a period of 1-2 hours, followed by solid state reaction processing via mechano-chemical stimulation of above heat treated brine sludge by dry grinding along with 20-90 g of tungsten powder and 10 g-60 g metakaolin in a mill for a period of 2-4 hours, followed by adding and grinding 2 g-8 g potassium hydroxide for a period of 1-2 hrs and further adding and grinding 1 g-4 g potassium silicate for a period of 1-2 hrs to obtained fine homogeneous radiation protection powder of modified brine sludge composition, followed by adding and thoroughly blending 4 ml-16 ml of water in it and so obtained material was further compacted in a steel mold, using hydraulic pressure in the range of 100-300 kg/cm.sup.2 in the form of tiles of dimensions 10 cm×10 cm×6-10 mm and further heated in a furnace in the temperature range of 900° C.-1100° C. for a period of 1-2 hours to make advanced lead-free radiation protection materials.

(15) In an embodiment of the present invention there is provided a process of making advanced lead-free radiation protection material utilizing modified brine sludge composition, the process comprising: a) drying of 200 g-800 g of brine sludge in an air oven at 100° C.-110° C. for a period of 1-2 hours, followed by solid state reaction processing and dry grinding along with 20-90 g of tungsten powder and 10 g-60 g metakaolin for a period of 2-4 hours; b) step a followed by adding and grinding 2 g-8 g potassium hydroxide for a period of 1-2 hrs and further adding and grinding 1 g-4 g potassium silicate for a period of 1-2 hrs to obtain fine homogeneous radiation protection powder of modified brine sludge composition; c) step b followed by adding and thoroughly blending with 4 ml-16 ml of water and compacting in a steel mold, using hydraulic pressure in the range of 100-300 kg/cm.sup.2 in the form of tiles; and d) step c followed by heating the tiles in a furnace in the temperature range of 900° C.-1100° C. for a period of 1-2 hours to obtain advanced lead-free radiation protection materials.

(16) In an embodiment of the present invention there is provided a process of making advanced lead-free radiation protection material utilizing modified brine sludge composition as disclosed herein, wherein drying of 200 g-800 g of brine sludge is carried out in an air oven at 100° C.-110° C. for a period of 1-2 hours.

(17) In another embodiment of the present invention there is provided a process of making advanced lead-free radiation protection material utilizing modified brine sludge composition as disclosed herein, wherein the process comprises solid-state reaction processing via mechano-chemical stimulation of heat-treated brine sludge by dry grinding along with 20-90 g of tungsten powder and 10 g-60 g metakaolin in a mill etc. for a period of 2-4 hours.

(18) In yet another embodiment of the present invention there is provided a process of making advanced lead-free radiation protection material utilizing modified brine sludge composition as disclosed herein, wherein adding and grinding of 2 g-8 g potassium hydroxide is carried out for a period of 1-2 hrs to the above powder from step a.

(19) In yet another embodiment of the present invention there is provided a process of making advanced lead-free radiation protection material utilizing modified brine sludge composition as disclosed herein, wherein adding and grinding of 1 g-4 g potassium silicate is carried out for a period of 1-2 hrs to obtain fine homogeneous radiation protection powder of modified brine sludge composition.

(20) In still another embodiment of the present invention there is provided a process of making advanced lead-free radiation protection material utilizing modified brine sludge composition as disclosed herein, wherein the 4 ml-16 ml of water was added and thoroughly blended in so obtained modified brine sludge composition.

(21) In still another embodiment of the present invention there is provided a process of making advanced lead-free radiation protection material utilizing modified brine sludge composition as disclosed herein, wherein the obtained above material was further compacted in a steel mold, using hydraulic pressure in the range of 100-300 kg/cm.sup.2 in the form of tiles of dimensions 10 cm×10 cm×6-10 mm.

(22) In still another embodiment of the present invention there is provided a process of making advanced lead-free radiation protection material utilizing modified brine sludge composition as disclosed herein, wherein the compacted material was further heated in a furnace in the temperature range of 900° C.-1100° C. for a period of 1-2 hours to make advanced lead-free radiation protection materials.

(23) In another embodiment of the present invention there is provided a process of making advanced lead-free radiation protection material utilizing modified brine sludge composition as disclosed herein, wherein the process involves simultaneous and synergistic chemical reactions of various mineralogical and chemical compounds which includes barium sulphate, magnesium hydroxide, calcium carbonate, sodium chloride, silica, aluminum containing compounds of brine sludge along with complementary chemical compound namely tungsten powder, metakaolin, potassium hydroxide and potassium silicate to obtain the fine homogeneous powder of modified brine sludge composition.

(24) In yet another embodiment of the present invention there is provided a process of creaking advanced lead-free radiation protection material is utilizing modified brine sludge composition as disclosed herein, wherein the process provides a desired shielding phase possessing uniform and homogenous protection matrix in the developed advanced radiation protection material.

(25) In still another embodiment of the present invention there is provided a process of making advanced lead-free radiation protection material utilizing modified brine sludge composition as disclosed herein, wherein the process provides designing of raw materials compositions and processing parameters, enabling synergistic and simultaneous chemical reactions among the various reactants of the design mix of raw materials. The present invention also provides the modified shielding powder so obtained and is having multi shielding phases and multi crystal phases due to presence of multi elements like Ba, W, Ca, Si, Al, Na, K etc.

(26) In one another embodiment of the present invention there is provided a process of creaking advanced lead-free radiation protection material utilizing modified brine sludge composition as disclosed herein, wherein the modified radiation protection powder so obtained possesses particle ranging from micron to nano size.

(27) In still another embodiment of the present invention there is provided a process of making advanced lead-free radiation protection material utilizing modified brine sludge composition as disclosed herein, wherein the process provides advanced functional radiation shielding materials which are devoid of conventionally used toxic lead, pure barium compound and hematite ore.

(28) In still another embodiment of the present invention there is provided a process of making advanced lead-free radiation protection material utilizing modified brine sludge composition as disclosed herein, wherein the process provides a desired homogeneous shielding matrix by chemically designed and mineralogical formulated compositions using various complementary precursors present in brine sludge and various constituents.

(29) In still another embodiment of the present invention there is provided a process of making advanced lead-free radiation protection material utilizing modified brine sludge composition as disclosed herein, wherein the process provides the process enabling conversion of toxic elements, present in brine sludge, in to non-toxic shielding phases in the developed advanced lead-free radiation is protection materials.

(30) In still another embodiment of the present invention there is provided a process of making advanced lead-free radiation protection material utilizing modified brine sludge composition as disclosed herein, wherein the process provides a simple, energy efficient, environmentally friendly and the cost-effective process enabling wide spread utilization of developed material for broad application spectrum ranging from diagnostic radiation installations such as diagnostic X-ray room to CT scanner room to other strategic radiation shielding installation etc.

EXAMPLES

(31) The following examples are given by way of illustration of the working of the invention in actual practice and therefore should not be construed to limit the scope of the present invention in any way.

Example 1

(32) For making advanced lead-free radiation protection material utilizing modified brine sludge composition, 200 g of brine sludge was dried in an air oven at 100° C. for a period of 1 hour, followed by solid state reaction processing via mechano-chemical stimulation of above heat-treated brine sludge by dry grinding it along with 20 g of tungsten powder and 10 g meta kaolin in a mill for 2 hours. Further, 2 g of potassium hydroxide was added and grinded for 1 hr. Again, 1 g potassium silicate was added and grinded for 1 hr to obtain fine homogeneous radiation protection powder of modified brine sludge composition. Additionally, 4 ml of water was added and thoroughly blended with the above powder. The material so obtained was then compacted in a steel mold, using hydraulic pressure of 100 kg/cm.sup.2 in the form of tiles of dimensions 10 cm×10 cm×6 mm. The tiles were then heated in a furnace at 900° C. temperature for 1 hour to obtain advanced lead-free radiation protection materials.

(33) The radiation protection material of thickness value of 6 mm prepared above was evaluated for its X-ray attenuation test with standard filter at respective kV using narrow beam X-ray qualities at 250 kV and the attenuation for kVp i.e. at 90 and 100 kVp were found to be 81 and 78% respectively. The impact strength of the sample was found to be 0.021 kgfm.Math.cm.sup.−1 and water absorption was found to be 17.0%.

Example 2

(34) For making advanced lead-free radiation protection material utilizing modified brine sludge composition, 300 g of brine sludge was dried in an air oven at 100° C. for a period of 1 hour, followed by solid state reaction processing via mechano-chemical stimulation of above heat-treated brine sludge by dry grinding it along with 30 g of tungsten powder and 25 g meta kaolin in a mill for two and half hours. Further, 3 g of potassium hydroxide was added and grinded for 1 hr. Again, 1.5 g potassium silicate was added and grinded for 1 hr to obtain fine homogeneous radiation protection powder of modified brine sludge composition. Further, 6 ml of water was added and thoroughly blended with the above powder. The material obtained was then compacted in a steel mold, using hydraulic pressure of 200 kg/cm.sup.2 in the form of tiles of dimensions 10 cm×10 cm×7 mm. The tiles were then heated in a furnace at 950° C. temperature for 1.5 hours to obtain advanced lead-free radiation protection materials.

(35) The radiation protection material of thickness value of 7 mm prepared above was evaluated for its X-ray attenuation test with standard filter at respective kV using narrow beam X-ray qualities at 250 kV and the attenuation for kVp i.e. at 90 and 100 kVp were found to be 83 and 80% respectively. The impact strength of the sample was found to be 0.023 kgfm.Math.cm.sup.−1 and water absorption was found to be 14.0%.

Example 3

(36) For making advanced lead-free radiation protection material utilizing modified brine sludge composition, 400 g of brine sludge was dried in an air oven at 100° C. for a period of one and half hour, followed by solid state reaction processing via mechano-chemical stimulation of above heat-treated brine sludge by dry grinding it along with 40 g of tungsten powder and 45 g meta kaolin in a mill for 3 and half hours. Further, 4 g of potassium hydroxide was added and grinded for one and half hr. Again. 2 g potassium silicate was added and grinded for one and half hr. to obtain fine homogeneous radiation protection powder of modified brine sludge composition. Further, 8 ml of water was added and thoroughly blended with the above powder. The material obtained was then compacted in a steel mold, using hydraulic pressure of 250 kg/cm.sup.2 in the form of tiles of dimensions 10 cm×10 cm×8 mm. The tiles were then heated in a furnace at 1000° C. temperature for 1.5 hours to obtain advanced lead-free radiation protection materials.

(37) The radiation protection material of thickness value of 8 mm prepared above was evaluated for its X-ray attenuation test with standard filter at respective kV using narrow beam X-ray qualities at 250 kV and the attenuation for kVp i.e. at 90 and 100 kVp were found to be 86 and 84% respectively. The impact strength of the sample was found to be 0.025 kgfm.Math.cm.sup.−1 and water absorption was found to be 12.0%.

Example 4

(38) For making advanced lead-free radiation protection material utilizing modified brine sludge composition, 650 g of brine sludge was dried in an air oven at 110° C. for a period of 2 hours, followed by solid state reaction processing via mechano-chemical stimulation of above heat-treated brine sludge by dry grinding it along with 60 g of tungsten powder and 50 g meta kaolin in a mill for three and half hours. Further, 5 g of potassium hydroxide was added and grinded for two and half hrs. Again, 2 g potassium silicate was added and grinded for 2 hr. to obtain fine homogeneous radiation protection powder of modified brine sludge composition. Further, 10 ml of water was added and thoroughly blended with the above powder. The material so obtained was further compacted in a steel mold, using hydraulic pressure of 275 kg/cm.sup.2 in the form of tiles of dimensions 10 cm×10 cm×9 mm. The tiles were then heated in a furnace at 1000° C. temperature for 1 hour to obtain advanced lead-free radiation protection materials.

(39) The radiation protection material of thickness value of 9 mm prepared above was evaluated for its X-ray attenuation test with standard filter at respective kV using narrow beam X-ray qualities at 250 kV and the attenuation for kVp i.e. at 90 and 100 kVp were found to be 88 and 86% respectively. The impact strength of the sample was found to be 0.030 kgfm.Math.cm.sup.−1 and water absorption was found to be 10.0%.

Example 5

(40) For making advanced lead-free radiation protection material utilizing modified brine sludge composition, 800 g of brine sludge was dried in an air oven at 110° C. for a period of 2 hours, followed by solid state reaction processing via mechano-chemical stimulation of above heat-treated brine sludge by dry grinding it along with 90 g of tungsten powder and 60 g meta kaolin in a mill for 4 hours. Further, 8 g of potassium hydroxide was added and grinded for 2 hr. Again. 4 g potassium silicate was added and grinded for 2 hr to obtain fine is homogeneous radiation protection powder of modified brine sludge composition. Further, 16 ml of water was added and thoroughly blended with the above powder. The material obtained was then compacted in a steel mold, using hydraulic pressure of 300 kg/cm.sup.2 in the form of tiles of dimensions 10 cm×10 cm×10 mm. The tiles were then heated in a furnace at 1100° C. temperature for 1 hour to obtain advanced lead-free radiation protection materials.

(41) The radiation protection material of thickness value of 9 mm prepared above was evaluated for its X-ray attenuation test with standard filter at respective kV using narrow beam X-ray qualities at 250 kV and the attenuation for kVp i.e. at 90 and 100 kVp were found to be 90 and 88% respectively. The impact strength of the sample was found to be 0.032 kgfm.Math.cm.sup.−1 and water absorption was found to be 8.0%.

Advantages of the Present Invention

(42) The process of the present invention involves drying, powdering and grinding for mechano-chemical activation of heat-treated brine sludge for obtaining fine homogeneous powder for developing homogeneous advanced radiation protection materials.

(43) The process of the present invention provides radiation protection phases by chemical designing and mineralogically formulating compositions based on various precursors of chemicals present in brine sludge along with other raw materials.

(44) The process of the present invention provides a desired mineralogical phase necessary for obtaining uniform and homogenous advanced radiation protection materials.

(45) The process involves designing of raw materials and processing parameters, enabling synergistic and simultaneous chemical reactions among the various reactants of the design mix of raw materials.

(46) The process provides a conversion of toxic elements like chromium, zinc, copper and vanadium, present in brine sludge into non-toxic form and leading to development of non-toxic shielding phases.

(47) Other advantage of the process of the present invention is conversion of a toxic brine sludge waste material in to a highly value added advanced non-toxic radiation shielding materials possessing homogeneous is radiation shielding matrix. And the process ensures complete utilization of toxic brine sludge.

(48) The process utilizes and avoids use of costly chemicals which are inherently present in the brine sludge otherwise required for making advanced lead-free radiation protection materials.

(49) The process solves the disposal problem of toxic brine sludge waste and saves the environment.

(50) The process is economically fruitful by providing value added advanced non-toxic radiation protection materials and ensuring total utilization of toxic brine sludge, otherwise incurred on maintenance of brine sludge ponds globally.