CN115583659A - Method for extracting ammonium sulfate from coking desulfurization waste liquid - Google Patents
Method for extracting ammonium sulfate from coking desulfurization waste liquid Download PDFInfo
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- CN115583659A CN115583659A CN202211337970.1A CN202211337970A CN115583659A CN 115583659 A CN115583659 A CN 115583659A CN 202211337970 A CN202211337970 A CN 202211337970A CN 115583659 A CN115583659 A CN 115583659A
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C1/00—Ammonia; Compounds thereof
- C01C1/24—Sulfates of ammonium
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- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B17/00—Sulfur; Compounds thereof
- C01B17/02—Preparation of sulfur; Purification
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- C01P2006/00—Physical properties of inorganic compounds
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Abstract
The invention discloses a method for extracting ammonium sulfate from coking desulfurization waste liquid, which relates to the technical field of coking desulfurization waste liquid recovery and comprises the following steps: decoloring the coking desulfurization waste liquid; distilling and concentrating the decolored coking desulfurization waste liquid, cooling after the distillation is finished, and filtering to obtain a filter cake and a coarse filtrate; feeding the filter cake into a dissolving tank to be dissolved by water, feeding the obtained solution into an oxidation tank to be oxidized, and then filtering to obtain sulfur and ammonium sulfate solution; distilling and concentrating the ammonium sulfate solution, sending the ammonium sulfate solution into a transfer kettle for cooling after the distillation is finished, centrifugally separating after the cooling is finished, sending the separated solid into an ammonium sulfate dissolving tank for dissolving again, and sending the centrifugal liquid into an ammonium sulfate mother liquor storage tank; and after the solution in the dissolving tank reaches a certain concentration, carrying out secondary centrifugation to obtain a solid, namely an ammonium sulfate finished product, and sending the centrifugate into an ammonium sulfate mother liquor storage tank. The method has the advantages of less loss, high yield and high purity, does not additionally generate other wastes in the extraction process, and is clean and environment-friendly.
Description
Technical Field
The invention relates to the technical field of recovery of coking desulfurization waste liquid, in particular to a method for extracting ammonium sulfate from coking desulfurization waste liquid.
Background
The desulfurization and decyanation process for coke oven gas includes arsenic gangue process, ADA process, hydroquinone process, naphthoquinone process, ethanolamine process, picric acid process, HPF process, etc. Among the above processes, the HPF method is favored because it uses ammonia in the coke oven gas as an alkali source, does not require an additional remover, and has a low running cost. In the process, ammonia and pollutants such as hydrogen sulfide, hydrogen cyanide and the like undergo complex chemical reactions to generate wastewater containing ammonium thiocyanate, ammonium thiosulfate and ammonium sulfate. Taking a coking company which produces 220 million tons of coke annually as an example, the HPF method is adopted to remove hydrogen sulfide and hydrogen cyanide in coke oven gas, about 22000 tons of desulfuration and decyanation waste liquid is produced annually, the concentrations of ammonium thiocyanate, ammonium thiosulfate and ammonium sulfate contained in the waste liquid are respectively 140-150 g/L, 40-50 g/L and 5-10 g/L, and the waste water is directly discharged, thereby not only polluting the environment, but also causing the waste of the chemicals.
The mode of treating the desulfurization waste liquid by a part of coking enterprises is to add the desulfurization waste liquid into the blending coal, but the moisture and the sulfur content of the blending coal are increased, the sulfur content of the produced coke is increased, the grade of the coke is influenced, the sulfur in the desulfurization waste liquid enters the coal gas in the coking process, the sulfur content of the coal gas is increased, and finally the load of a desulfurization system is increased.
Disclosure of Invention
The invention aims to: the method for extracting the ammonium sulfate from the coking desulfurization waste liquid can extract the ammonium sulfate from the coking desulfurization waste liquid so as to solve the problem of recycling the coking desulfurization waste liquid.
The technical scheme adopted by the invention is as follows:
a method for extracting ammonium sulfate from coking desulfurization waste liquid comprises the following steps:
s1: pouring the coking desulfurization waste liquid into a decoloring kettle for decoloring;
s2: pouring the decolored coking desulfurization waste liquid into a concentration kettle for distillation and concentration, cooling after the distillation is finished, and filtering to obtain a filter cake and coarse filtrate;
s3: feeding the filter cake into a dissolving tank to be dissolved by water, feeding the obtained solution into an oxidation tank to be oxidized, and then filtering to obtain sulfur and ammonium sulfate solution;
s4: feeding the ammonium sulfate solution into a concentration kettle for distillation and concentration, feeding the ammonium sulfate solution into a transfer kettle for cooling after the distillation is finished, carrying out centrifugal separation after the cooling is finished, feeding the separated solid into an ammonium sulfate dissolving tank, and feeding the centrifugal liquid into an ammonium sulfate mother liquor storage tank;
s5: and (4) after the solution in the dissolving tank reaches a certain concentration, carrying out secondary centrifugation to obtain a solid ammonium sulfate finished product, and sending the centrifugate into an ammonium sulfate mother liquor storage tank.
Preferably, in the step S1, the decoloring temperature is 75-80 ℃ and the decoloring time is 4 hours.
Preferably, in step S2, the distillation concentration temperature is 85-95 ℃, and the concentration time is 5h.
Preferably, in step S2, the temperature reduction rate is 0.1 to 2.0 ℃/min, and the filtration is started after the temperature is reduced to 65 to 70 ℃.
Preferably, in step S3, the dissolution temperature is 50 to 55 ℃.
Preferably, in step S3, hydrogen peroxide is used as the oxidizing agent, and the mass ratio of the cake to the oxidizing agent is 50.
Preferably, in step S4, the distillation temperature is 90-95 ℃, and the distillation is finished when a large amount of solid particles appear in the solution.
Preferably, in step S5, the secondary centrifugation is performed after the ammonium sulfate concentration in the solution reaches 80%.
In summary, due to the adoption of the technical scheme, the invention has the beneficial effects that: the method can fully extract the ammonium sulfate in the coking desulfurization waste liquid, has the advantages of less loss, high yield and high purity, does not additionally generate other wastes in the extraction process, can recycle intermediate products, and is clean and environment-friendly.
Drawings
FIG. 1 is a flow chart of the present invention.
Detailed Description
For the purpose of making the objects, technical solutions and advantages of the present invention more apparent, the present invention will be further described in detail with reference to the accompanying drawings and embodiments, it being understood that the specific embodiments described herein are only for the purpose of explaining the present invention and are not intended to limit the present invention.
The invention provides a method for extracting ammonium sulfate from coking desulfurization waste liquid, which utilizes the coking desulfurization waste liquid to produce ammonium sulfate and sulfur so as to realize resource utilization of the coking desulfurization waste liquid, and byproducts can be used for producing ammonium thiocyanate.
The method mainly comprises the following steps:
s1: pouring the coking desulfurization waste liquid into a decoloring kettle, and decoloring at the temperature of 75-80 ℃ for 3.5-4.h;
s2: pouring the decolored coking desulfurization waste liquid into a concentration kettle for distillation concentration, wherein the distillation concentration temperature is 85-95 ℃, the distillation time is 4-6 h, cooling is carried out after the distillation is finished, the cooling rate is 0.1-2.0 ℃/min, the filtration is started after the cooling is carried out to 65-70 ℃, so as to obtain a filter cake and a rough filtrate, the main components of the filter cake are ammonium thiosulfate and ammonium sulfate, and the main component of the rough filtrate is ammonium thiocyanate;
s3: feeding the filter cake into a dissolving tank, dissolving the filter cake with water at 50-55 ℃, feeding the obtained solution into an oxidation tank, adding 25% hydrogen peroxide to oxidize, wherein the mass ratio of the filter cake to the hydrogen peroxide is 50-10;
s4: feeding the ammonium sulfate solution into a concentration kettle, distilling and concentrating at the temperature of 90-95 ℃, observing crystallization conditions through a sight glass of the distillation kettle, finishing distillation when a large number of solid particles appear in the solution, feeding the solution into a transfer kettle for cooling after the distillation is finished, performing centrifugal separation after the cooling is finished, feeding the separated solid into an ammonium sulfate dissolving tank for dissolving again, and feeding the centrifugal liquid into an ammonium sulfate mother liquor storage tank;
s5: and (4) after the solution in the dissolving tank reaches 80%, carrying out secondary centrifugation to obtain a solid, namely an ammonium sulfate finished product, and sending the centrifugate into an ammonium sulfate mother liquor storage tank.
The coarse filtrate obtained in step S2 can be used for producing ammonium thiocyanate, and the centrifugate obtained in steps S4 and S5 and the ammonium sulfate solution obtained in step S3 are sent into a concentration kettle for concentration.
The technical solution of the present invention is further illustrated by the following examples.
Example 1
Pouring the coking desulfurization waste liquid into a decoloring kettle, and decoloring at the temperature of 75 ℃ for 4 hours; pouring the decolored coking desulfurization waste liquid into a concentration kettle for distillation concentration, wherein the distillation concentration temperature is 90 +/-3 ℃, the distillation time is 5 hours, the temperature is reduced after the distillation is finished, the temperature reduction rate is 0.5 ℃/min, the temperature is reduced to 70 ℃, and then the filtering is carried out to obtain a filter cake and a coarse filtrate; feeding the filter cake into a dissolving tank, completely dissolving the filter cake with water at 50 +/-3 ℃, feeding the obtained solution into an oxidation tank, adding hydrogen peroxide for oxidation, wherein the ratio of the filter cake to the hydrogen peroxide is 100, and then filtering to obtain a sulfur and ammonium sulfate solution; feeding the ammonium sulfate solution into a concentration kettle, distilling and concentrating at the temperature of 90 +/-4 ℃, observing crystallization conditions through a sight glass of the distillation kettle, finishing distillation when a large number of solid particles appear in the solution, feeding the solution into a transfer kettle for cooling after the distillation is finished, performing centrifugal separation after the cooling is finished, feeding the separated solid into an ammonium sulfate dissolving tank for dissolving again, and feeding the centrifugal liquid into an ammonium sulfate mother liquor storage tank; and after the solution in the dissolving tank reaches 80%, carrying out secondary centrifugation to obtain a solid, namely an ammonium sulfate finished product, sending the centrifugate into an ammonium sulfate mother solution storage tank for later use, and mixing the solution in the ammonium sulfate mother solution storage tank with the ammonium sulfate solution obtained by oxidation filtration.
Through material accounting, 93kg of ammonium sulfate and 22kg of sulfur are produced per 1000kg of coking desulfurization waste liquid on average, and the purity of the obtained ammonium sulfate finished product is 99.7 percent, and the nitrogen content is 21.1 percent.
Example 2
Pouring the coking desulfurization waste liquid into a decoloring kettle, and decoloring at the temperature of 75 ℃ for 3.5 hours; pouring the decolored coking desulfurization waste liquid into a concentration kettle for distillation concentration, wherein the distillation concentration temperature is 86 +/-3 ℃, the distillation time is 6 hours, the temperature is reduced after the distillation is finished, the temperature reduction rate is 1.5 ℃/min, the temperature is reduced to 67 ℃, and then the filtering is carried out to obtain a filter cake and a coarse filtrate; feeding the filter cake into a dissolving tank, completely dissolving the filter cake with water at 55 +/-2 ℃, feeding the obtained solution into an oxidation tank, adding hydrogen peroxide for oxidation, wherein the ratio of the filter cake to the hydrogen peroxide is 10; feeding the ammonium sulfate solution into a concentration kettle, distilling and concentrating at the temperature of 95 +/-3 ℃, observing crystallization conditions through a sight glass of the distillation kettle, finishing distillation when a large number of solid particles appear in the solution, cooling the solution in a transfer kettle after the distillation is finished, performing centrifugal separation after the cooling is finished, feeding the separated solid into an ammonium sulfate dissolving tank for dissolving again, and feeding the centrifugal liquid into an ammonium sulfate mother liquor storage tank; and after the solution in the dissolving tank reaches 80%, carrying out secondary centrifugation to obtain a solid, namely an ammonium sulfate finished product, sending the centrifugate into an ammonium sulfate mother solution storage tank for later use, and mixing the solution in the ammonium sulfate mother solution storage tank with the ammonium sulfate solution obtained by oxidation filtration.
Through material accounting, 102kg of ammonium sulfate and 26kg of sulfur are produced per 1000kg of coking desulfurization waste liquid on average, and the purity of the obtained ammonium sulfate finished product is 99.5 percent, and the nitrogen content is 21.0 percent.
Example 3
Pouring the coking desulfurization waste liquid into a decoloring kettle, and decoloring at the temperature of 75 ℃ for 4.5 hours; pouring the decolored coking desulfurization waste liquid into a concentration kettle for distillation concentration, wherein the distillation concentration temperature is 93 +/-3 ℃, the distillation time is 4 hours, the temperature is reduced after the distillation is finished, the temperature reduction rate is 0.2 ℃/min, and the filtrate is filtered after the temperature is reduced to 65 ℃ to obtain a filter cake and a rough filtrate; feeding the filter cake into a dissolving tank, completely dissolving the filter cake with water at 50 +/-2 ℃, feeding the obtained solution into an oxidation tank, adding hydrogen peroxide for oxidation, wherein the ratio of the filter cake to the hydrogen peroxide is 50; feeding the ammonium sulfate solution into a concentration kettle, distilling and concentrating at the temperature of 95 +/-3 ℃, observing crystallization conditions through a sight glass of the distillation kettle, finishing distillation when a large number of solid particles appear in the solution, feeding the solution into a transfer kettle for cooling after the distillation is finished, performing centrifugal separation after the cooling is finished, feeding the separated solid into an ammonium sulfate dissolving tank for dissolving again, and feeding the centrifugal liquid into an ammonium sulfate mother liquor storage tank; and (3) after the solution in the dissolving tank reaches 80%, carrying out secondary centrifugation to obtain a solid, namely an ammonium sulfate finished product, sending the centrifugate into an ammonium sulfate mother liquor storage tank for later use, and mixing the solution in the ammonium sulfate mother liquor storage tank with the ammonium sulfate solution obtained by oxidation filtration.
Through material accounting, 95kg of ammonium sulfate and 23kg of sulfur are produced per 1000kg of coking desulfurization waste liquid on average, and the purity of the obtained ammonium sulfate finished product is 99.6 percent, and the nitrogen content is 21.0 percent.
Comparative example 1
Pouring the coking desulfurization waste liquid into a decoloring kettle, and decoloring at the temperature of 75 ℃ for 4 hours; pouring the decolored coking desulfurization waste liquid into a concentration kettle for distillation concentration, wherein the distillation concentration temperature is 90 +/-3 ℃, the distillation time is 5 hours, the temperature is reduced after the distillation is finished, the temperature reduction rate is 0.5 ℃/min, the temperature is reduced to 70 ℃, and then the filtering is carried out to obtain a filter cake and a coarse filtrate; feeding the filter cake into a dissolving tank, completely dissolving the filter cake with water at 50 +/-3 ℃, feeding the obtained solution into an oxidation tank, adding hydrogen peroxide for oxidation, wherein the ratio of the filter cake to the hydrogen peroxide is 20; feeding the ammonium sulfate solution into a concentration kettle, distilling and concentrating at the temperature of 90 +/-4 ℃, observing crystallization conditions through a sight glass of the distillation kettle, finishing distillation when a large number of solid particles appear in the solution, feeding the solution into a transfer kettle for cooling after the distillation is finished, performing centrifugal separation after the cooling is finished, feeding the separated solid into an ammonium sulfate dissolving tank for dissolving again, and feeding the centrifugal liquid into an ammonium sulfate mother liquor storage tank; and (3) after the solution in the dissolving tank reaches 80%, carrying out secondary centrifugation to obtain a solid, namely an ammonium sulfate finished product, sending the centrifugate into an ammonium sulfate mother liquor storage tank for later use, and mixing the solution in the ammonium sulfate mother liquor storage tank with the ammonium sulfate solution obtained by oxidation filtration.
Through material accounting, 85kg of ammonium sulfate and 17kg of sulfur are produced per 1000kg of coking desulfurization waste liquid on average, and the purity of the obtained ammonium sulfate finished product is 94.3 percent, and the nitrogen content is 20.6 percent.
Comparing example 1 with comparative example 1, it can be seen that the yield of ammonium sulfate is obviously reduced and the purity of the product is reduced after the dosage of the oxidant is reduced, which indicates that the dosage of the oxidant is insufficient, and meanwhile, the dosage of the oxidant is not less than 6% of the mass of the filter cake as can be seen from comparative example 3.
Comparative example 2
Pouring the coking desulfurization waste liquid into a decoloring kettle, and decoloring at the temperature of 75 ℃ for 4 hours; pouring the decolored coking desulfurization waste liquid into a concentration kettle for distillation concentration, wherein the distillation concentration temperature is 90 +/-3 ℃, the distillation time is 5 hours, the temperature is reduced after the distillation is finished, the temperature reduction rate is 0.5 ℃/min, the temperature is reduced to 75 ℃, and then the filtering is carried out to obtain a filter cake and a coarse filtrate; feeding the filter cake into a dissolving tank, completely dissolving the filter cake with water at 50 +/-3 ℃, feeding the obtained solution into an oxidation tank, adding hydrogen peroxide for oxidation, wherein the ratio of the filter cake to the hydrogen peroxide is 100, and then filtering to obtain a sulfur and ammonium sulfate solution; feeding the ammonium sulfate solution into a concentration kettle, distilling and concentrating at the temperature of 90 +/-4 ℃, observing crystallization conditions through a sight glass of the distillation kettle, finishing distillation when a large number of solid particles appear in the solution, feeding the solution into a transfer kettle for cooling after the distillation is finished, performing centrifugal separation after the cooling is finished, feeding the separated solid into an ammonium sulfate dissolving tank for dissolving again, and feeding the centrifugal liquid into an ammonium sulfate mother liquor storage tank; and (3) after the solution in the dissolving tank reaches 80%, carrying out secondary centrifugation to obtain a solid, namely an ammonium sulfate finished product, sending the centrifugate into an ammonium sulfate mother liquor storage tank for later use, and mixing the solution in the ammonium sulfate mother liquor storage tank with the ammonium sulfate solution obtained by oxidation filtration.
Through material accounting, 83kg of ammonium sulfate and 15kg of sulfur are produced per 1000kg of coking desulfurization waste liquid on average, and the purity of the obtained ammonium sulfate finished product is 99.8 percent, and the nitrogen content is 21.0 percent.
As can be seen by comparing example 1 with comparative example 2, the yield of ammonium sulfate and sulfur is significantly reduced after the first filtration temperature is increased, but the purity is basically maintained to be equal, which indicates that ammonium thiosulfate and ammonium sulfate are not completely separated out.
Comparative example 3
Pouring the coking desulfurization waste liquid into a decoloring kettle, and decoloring at the temperature of 75 ℃ for 4 hours; pouring the decolored coking desulfurization waste liquid into a concentration kettle for distillation concentration, wherein the distillation concentration temperature is 90 +/-3 ℃, the distillation time is 5 hours, the temperature is reduced after the distillation is finished, the temperature reduction rate is 0.5 ℃/min, the temperature is reduced to 60 ℃, and then the filtering is carried out to obtain a filter cake and a coarse filtrate; feeding the filter cake into a dissolving tank, completely dissolving the filter cake with water at 50 +/-3 ℃, feeding the obtained solution into an oxidation tank, adding hydrogen peroxide for oxidation, and filtering to obtain a sulfur and ammonium sulfate solution, wherein the ratio of the filter cake to the hydrogen peroxide is 100; feeding the ammonium sulfate solution into a concentration kettle, distilling and concentrating at the temperature of 90 +/-4 ℃, observing crystallization conditions through a sight glass of the distillation kettle, finishing distillation when a large number of solid particles appear in the solution, feeding the solution into a transfer kettle for cooling after the distillation is finished, performing centrifugal separation after the cooling is finished, feeding the separated solid into an ammonium sulfate dissolving tank for dissolving again, and feeding the centrifugal liquid into an ammonium sulfate mother liquor storage tank; and (3) after the solution in the dissolving tank reaches 80%, carrying out secondary centrifugation to obtain a solid, namely an ammonium sulfate finished product, sending the centrifugate into an ammonium sulfate mother liquor storage tank for later use, and mixing the solution in the ammonium sulfate mother liquor storage tank with the ammonium sulfate solution obtained by oxidation filtration.
Through material accounting, 109kg of ammonium sulfate and 26kg of sulfur are produced per 1000kg of coking desulfurization waste liquid on average, and the purity of the obtained ammonium sulfate finished product is 94.8 percent, and the nitrogen content is 20.3 percent.
As can be seen by comparing example 1 with comparative example 2, the yield of ammonium sulfate is increased but the purity is obviously reduced after the first filtration temperature is reduced, and the filter cake contains ammonium thiocyanate through detection and analysis.
In conclusion, the working condition parameters for extracting ammonium sulfate in the embodiment 2 are better, the yields of ammonium sulfate and sulfur are highest, and the purity and the nitrogen content of the ammonium sulfate are higher.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (8)
1. A method for extracting ammonium sulfate from coking desulfurization waste liquid is characterized by comprising the following steps:
s1: pouring the coking desulfurization waste liquid into a decoloring kettle for decoloring;
s2: pouring the decolored coking desulfurization waste liquid into a concentration kettle for distillation and concentration, cooling after the distillation is finished, and filtering to obtain a filter cake and coarse filtrate;
s3: feeding the filter cake into a dissolving tank for dissolving by water, feeding the obtained solution into an oxidation tank for oxidation, and then filtering to obtain sulfur and ammonium sulfate solution;
s4: feeding the ammonium sulfate solution into a concentration kettle for distillation and concentration, feeding the ammonium sulfate solution into a transfer kettle for cooling after the distillation is finished, carrying out centrifugal separation after the cooling is finished, feeding the separated solid into an ammonium sulfate dissolving tank, and feeding the centrifugal liquid into an ammonium sulfate mother liquor storage tank;
s5: and (4) after the solution in the dissolving tank reaches a certain concentration, carrying out secondary centrifugation to obtain a solid ammonium sulfate finished product, and sending the centrifugate into an ammonium sulfate mother liquor storage tank.
2. The method for extracting ammonium sulfate from coking desulfurization waste liquid according to claim 1, wherein in step S1, the decolorizing temperature is 75-80 ℃ and the decolorizing time is 3.5-4.5 h.
3. The method for extracting ammonium sulfate from coking desulfurization waste liquid according to claim 1, wherein in the step S2, the distillation concentration temperature is 85-95 ℃, and the concentration time is 4-6 h.
4. The method for extracting ammonium sulfate from coking desulfurization waste liquid according to claim 1, wherein in step S2, the temperature reduction rate is 0.1-2.0 ℃/min, and the filtration is started after the temperature is reduced to 65-70 ℃.
5. The method for extracting ammonium sulfate from coking desulfurization waste liquid according to claim 1, wherein the dissolution temperature in step S3 is 50 to 55 ℃.
6. The method for extracting ammonium sulfate from coking desulfurization waste liquid according to claim 1, characterized in that in step S3, hydrogen peroxide is used as the oxidizing agent, and the mass ratio of the filter cake to the oxidizing agent is 50.
7. The method for extracting ammonium sulfate from coking desulfurization waste liquid according to claim 1, wherein the distillation temperature in step S4 is 90 to 95 ℃, and the distillation is terminated when a large amount of solid particles appear in the solution.
8. The method of claim 1, wherein in step S5, the ammonium sulfate concentration in the solution reaches 80% and then secondary centrifugation is performed.
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2022
- 2022-10-28 CN CN202211337970.1A patent/CN115583659A/en active Pending
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| JPH02279514A (en) * | 1989-04-21 | 1990-11-15 | Ube Ind Ltd | Production of decolored and rearranged ammonium sulfate |
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