CN1424255A - Method for qualifying industrial ammonium chloride products - Google Patents
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- CN1424255A CN1424255A CN 02157284 CN02157284A CN1424255A CN 1424255 A CN1424255 A CN 1424255A CN 02157284 CN02157284 CN 02157284 CN 02157284 A CN02157284 A CN 02157284A CN 1424255 A CN1424255 A CN 1424255A
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Abstract
A process for improving the quality of industrial ammonium chloride includes such steps as dissolving ammonium chloride in water or unsaturated solution of ammonium chloride at 40-70 deg.C to obtain saturated solution, cooling to 10-25 deg.C to educe out ammonium chloride crystal, thickening the crystal liquid to increase its solid/liquid ratio, centrifugal dewatering to obtain finished ammonium chloride, adding solution of barium chloride to the mother liquid generated by said dewatering to generate barium sulfate deposit, filtering, and heating the filtrate to 40-70 deg.C for cyclic use.
Description
Technical Field
The invention relates to a method for improving the qualityof industrial ammonium chloride products, in particular to a method for improving the quality of industrial ammonium chloride products by reducing the content of sulfate ion removed from ammonium chloride.
Background
One of the main raw materials for producing sodium carbonate and ammonium chloride by adopting the combined soda process is sodium chloride, and the sodium chloride contains a certain amount of sulfate ions SO4 2-Meanwhile, because the desulfurization post of the production system has a small amount of residual hydrogen sulfide H2The S is oxidized and the oxidation reaction is carried out,SO that the content of sulfate ions in the produced ammonium chloride product is high, generally about 0.04-0.06%, and the ammonium chloride product can not meet the requirements of producing high-grade batteries and using in the electrochromic industry, therefore, how to remove the sulfate ions SO from the ammonium chloride4 2-It is especially important to improve the quality of industrial ammonium chloride products and to convert a part of low-grade ammonium chloride into high-grade industrial ammonium chloride products to meet the requirements of battery and electrochromic industries. In the prior art, the sulfate ions SO in the raw material sodium chloride are generally controlled4 2-To reduce sulfate ion SO in ammonium chloride products4 2-The process comprises washing raw material sodium chloride with saturated sodium chloride solution to remove sulfate ions SO4 2-And (4) removing. The disadvantage is that the process requires high production investment, which results in high production costs; remove sulfate radical ion SO4 2-Has poor effect, and generally only can lead sulfate ions SO in raw material sodium chloride4 2-The content of the sulfate ions is reduced to about O.5 percent, and the sulfate ions SO in the ammonium chloride product produced by the raw material4 2-Is present in an amount of about 0.02% to about 0.03%; and can be generated after salt washingA large amount of sewage needs to be discharged, which is not beneficial to environmental protection.
Disclosure of Invention
The invention aims to solve the technical problem of the prior art and provides a method for removing sulfate ions from ammonium chloride to improve the quality of industrial ammonium chloride products, which has low cost, good effect and no emission.
The technical problem to be solved by the present invention is achieved by the following technical means. The invention relates to a method for improving the quality of industrial ammonium chloride products, which is characterized by comprising the following steps,
(1) firstly, dissolving ammonium chloride into saturated ammonium chloride solution by using water or unsaturated ammonium chloride solution with the temperature of 40-70 ℃;
(2) cooling the saturated solution of ammonium chloride to 10-25 ℃ to separate out ammonium chloride crystals;
(3) increasing the solid-liquid ratio of the ammonium chloride crystal liquid by a thickener, and when the solid-liquid ratio reaches (16-25) to (84-75), dewatering in a centrifugal machine, and drying to obtain the finished product ammonium chloride;
(4) and adding a non-excessive barium chloride solution into the mother liquor I thrown out during the dehydration of the centrifuge to generate barium sulfate precipitate, filtering to obtain filtered mother liquor II, heating the mother liquor II to 40-70 ℃, and dissolvingammonium chloride for recycling.
According to the invention, the sulfate ions SO4 2-The characteristic of dissolving in water is that the process of dissolving first and then crystallizing is adopted to lead most of sulfate radical ions SO4 2-Remaining in the mother liquor I, and then utilizing the sulfate radical ions SO in the barium chloride solution and the mother liquor I4 2-The reaction has the following reaction equation:
The technical problem to be solved by the present invention can be further realized by the following technical means. The method for improving the quality of the industrial ammonium chloride product is characterized in that hydrochloric acid or ammonia water is added to adjust the pH value of the mother liquor II according to the pH value of the mother liquor II, so that the pH value of the mother liquor II is 4.0-5.8. Therefore, the quality of the ammonium chloride product can be further improved, and impurities can be prevented from being brought in while the pH value of the mother liquor II is adjusted.
The technical problem to be solved by the present invention can be further realized by the following technical means. The method for improving the quality of the industrial ammonium chloride product is characterized in that the concentration of the added barium chloride solution is 25-28%.
Compared with the prior art, the invention has the following advantages: first, the method of the invention is implementedThe method is simple, the investment is less, and the required cost is lower; secondly, sulfate ions SO in the finished product ammonium chloride obtained by the method4 2-The content is low, generally between 0 and 0.02 percent, is a superior industrial grade ammonium chloride, and can be used for high-grade batteries and the electro-chromic industry; thirdly, due to the invention, the requirement on the grade of sodium chloride which is one of the raw materials is lower in the process for producing the soda ash and the ammonium chloride by using the combined soda process, especially for the SO containing sulfate ions4 2-Higher sodium chloride can also be used, thereby reducing the limitation on raw materials; the mother liquor of the method can be recycled, and finally no discharge is realized, thereby being beneficial to environmental protection; and fifthly, the barium sulfate obtained by applying the method has wide application, so that resources can be fully utilized, and resource waste is avoided.
Drawings
The attached figure is a flow chart of the method of the invention.
Detailed Description
Embodiments of the present invention are further described below with reference to the accompanying drawings.
Example 1. Reference is made to the accompanying drawings. A method for improving the quality of industrial ammonium chloride products comprises the following steps,
(1) firstly, dissolving ammonium chloride into saturated solution of ammonium chloride by using water with the temperature of 50 ℃, wherein sulfate ions SO in the ammonium chloride4 2-Is about 0.05%;
(2) cooling the saturated solution of ammonium chloride to 12 ℃ to separate out ammonium chloride crystals;
(3) increasing solid-liquid ratio of ammonium chloride crystal liquid by thickener, dewatering in centrifuge when solid-liquid ratio reaches 16: 84, and drying to obtain ammonium chloride product containing sulfate ion SO4 2-Is about 0.01%;
(4) and adding a non-excessive barium chloride solution into the mother liquor I thrown out during the dehydration of the centrifuge to generate barium sulfate precipitate, filtering to obtain filtered mother liquor II, heating the mother liquor II to 50 ℃, dissolving ammonium chloride, and recycling.
The first step can be carried out in a hydrothermal solution container, and after the ammonium chloride solution is fully dissolved into a saturated ammonium chloride solution, the ammonium chloride solution enters a cold liquid container to separate out ammonium chloride crystals after heat exchange and temperature reduction are carried out by a heat exchanger. In the fourth step, the mother liquor II is heated to 50 ℃ and then put into the hydrothermal liquid container in the first step to dissolve ammonium chloride for recycling.
Example 2. Reference is made to the accompanying drawings. A method for improving the quality of industrial ammonium chloride products comprises the following steps,
(1) firstly, using unsaturated ammonium chloride solution with 60 deg.C to dissolve ammonium chloride to obtain saturated ammonium chloride solution in which the sulfate radical ion SO in the ammonium chloride is4 2-Is about 0.06%;
(2) cooling the saturated solution of ammonium chloride to 16 ℃ to separate outammonium chloride crystals;
(3) the ammonium chloride crystal liquid is passed through a thickener to raise the solid-liquid ratio until the solid-liquid ratio reaches 2080, dewatering in a centrifuge, and drying to obtain ammonium chloride product with sulfate ion SO4 2-Is about 0.02%;
(4) and adding a non-excessive barium chloride solution into the mother liquor I thrown out during the dehydration of the centrifuge to generate barium sulfate precipitate, filtering to obtain filtered mother liquor II, heating the mother liquor II to 60 ℃, dissolving ammonium chloride, and recycling.
Example 3. Reference is made to the accompanying drawings. A method for improving the quality of industrial ammonium chloride products comprises the following steps,
(1) firstly, using unsaturated ammonium chloride solution with 70 deg.C to dissolve ammonium chloride to obtain saturated ammonium chloride solution in which the sulfate radical ion SO in the ammonium chloride is4 2-Is about 0.04%;
(2) cooling the saturated solution of ammonium chloride to 22 ℃ to separate out ammonium chloride crystals;
(3) will chloridizeIncreasing solid-liquid ratio of the ammonium crystal liquid by a thickener, dewatering in a centrifuge when the solid-liquid ratio reaches 25: 75, and drying to obtain ammonium chloride product containing sulfate ions SO4 2-Is about 0.005%; and (4) adding a non-excessive barium chloride solution with the concentration of 28% into the mother liquor I thrown out during the dehydration of the centrifuge, filtering after generating barium sulfate precipitate to obtain filtered mother liquor II, simultaneously adding dilute hydrochloric acid or dilute ammonia water to adjust the pH value of the mother liquor II according to the pH value of the mother liquor II, heating the mother liquor II to 70 ℃ after the pH value of the mother liquor II is 5, dissolving ammonium chloride, and recycling.
Example 4. Reference is made to the accompanying drawings. A method for improving the quality of industrial ammonium chloride products comprises the following steps,
(1) firstly, dissolving ammonium chloride into saturated solution of ammonium chloride by using water with the temperature of 40 ℃, wherein sulfate ions SO in the ammonium chloride4 2-Is about 0.05%;
(2) cooling the saturated solution of ammonium chloride to 18 ℃ to separate out ammonium chloride crystals;
(3) increasing solid-liquid ratio of ammonium chloride crystal liquid by thickener, dewatering in centrifuge when solid-liquid ratio reaches 22: 78, and drying to obtain ammonium chloride product containing sulfate ion SO4 2-Is about 0.001%;
(4) and adding a non-excessive barium chloride solution with the concentration of 25% into the mother liquor I thrown out during the dehydration of the centrifuge to generate barium sulfate precipitate, filtering to obtain filtered mother liquor II, simultaneously adding dilute hydrochloric acid or dilute ammonia water to adjust the pH value of the mother liquor II according to the pH value of the mother liquor II to ensure that the pH value of the mother liquor II is 4, heating the mother liquor II to 40 ℃, and dissolving ammonium chloride for recycling.
Example 5. Reference is made to the accompanying drawings. A method for improving the quality of industrial ammonium chloride products comprises the following steps,
(1) firstly, dissolving ammonium chloride into saturated solution of ammonium chloride by using water with the temperature of55 ℃, wherein sulfate ions SO in the ammonium chloride4 2-Is about 0.06%;
(2) cooling the saturated solution of ammonium chloride to 20 ℃ to separate out ammonium chloride crystals;
(3) increasing solid-liquid ratio of ammonium chloride crystal liquid by thickener, dewatering in centrifuge when solid-liquid ratio reaches 18: 82, and drying to obtain ammonium chloride product containing sulfate ion SO4 2-Is about 0.015%;
(4) and adding a non-excessive barium chloride solution with the concentration of 26% into the mother liquor I thrown out during the dehydration of the centrifuge to generate barium sulfate precipitate, filtering to obtain filtered mother liquor II, simultaneously adding dilute hydrochloric acid or dilute ammonia water to adjust the pH value of the mother liquor II according to the pH value of the mother liquor II to ensure that the pH value of the mother liquor II is 5.8, heating the mother liquor II to 55 ℃, and dissolving ammonium chloride for recycling.
Claims (3)
1. A method for improving the quality of industrial ammonium chloride products is characterized by comprising the following steps,
(1) firstly, dissolving ammonium chloride into saturated ammonium chloride solution by using water or unsaturated ammonium chloride solution with the temperature of 40-70 ℃;
(2) cooling the saturated solution of ammonium chloride to 10-25 ℃ to separate out ammonium chloride crystals;
(3) increasing the solid-liquid ratio of the ammonium chloride crystal liquid by a thickener, and when the solid-liquid ratio reaches (16-25) to (84-75), dewatering in a centrifugal machine, and drying to obtain the finished product ammonium chloride;
(4) and adding a non-excessive barium chloride solution into the mother liquor I thrown out during the dehydration of the centrifuge to generate barium sulfate precipitate, filtering to obtain filtered mother liquor II, heating the mother liquor II to 40-70 ℃, and dissolving ammonium chloride for recycling.
2. The method for improving the quality of industrial ammonium chloride products as claimed in claim 1, wherein hydrochloric acid or ammonia water is added to adjust the pH value of the mother liquor II according to the pH value of the mother liquor II, so that the pH value of the mother liquor II is 4.0-5.8.
3. The method for improving the quality of industrial ammonium chloride products according to claim 1 or 2, wherein the concentration of the added barium chloride solution is 25-28%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02157284 CN1197772C (en) | 2002-12-24 | 2002-12-24 | Method for qualifying industrial ammonium chloride products |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 02157284 CN1197772C (en) | 2002-12-24 | 2002-12-24 | Method for qualifying industrial ammonium chloride products |
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| CN1424255A true CN1424255A (en) | 2003-06-18 |
| CN1197772C CN1197772C (en) | 2005-04-20 |
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| CN 02157284 Expired - Lifetime CN1197772C (en) | 2002-12-24 | 2002-12-24 | Method for qualifying industrial ammonium chloride products |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103232046A (en) * | 2013-04-13 | 2013-08-07 | 马鞍山市德科新材料有限公司 | Method for removing sulfate from ammonium salt |
| CN107572551A (en) * | 2017-08-31 | 2018-01-12 | 湖北双环科技股份有限公司 | A kind of method of winter production essence ammonium |
| CN111661853A (en) * | 2020-01-03 | 2020-09-15 | 宁夏云泰科技有限公司 | Production process of industrial ammonium chloride |
| CN112142068A (en) * | 2020-09-07 | 2020-12-29 | 湖北兴福电子材料有限公司 | Method for producing high-purity ammonium chloride from industrial-grade ammonium chloride |
| CN112340912A (en) * | 2020-09-29 | 2021-02-09 | 陕西陕焦化工有限公司 | Method for recovering inorganic salt in ammonia desulphurization waste liquid |
| CN113698020A (en) * | 2021-08-30 | 2021-11-26 | 衢州华友钴新材料有限公司 | Method for reducing chlorine and COD (chemical oxygen demand) of ammonium sulfate concentrated mother liquor |
-
2002
- 2002-12-24 CN CN 02157284 patent/CN1197772C/en not_active Expired - Lifetime
Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103232046A (en) * | 2013-04-13 | 2013-08-07 | 马鞍山市德科新材料有限公司 | Method for removing sulfate from ammonium salt |
| CN103232046B (en) * | 2013-04-13 | 2015-07-15 | 马鞍山市德科新材料有限公司 | Method for removing sulfate from ammonium salt |
| CN107572551A (en) * | 2017-08-31 | 2018-01-12 | 湖北双环科技股份有限公司 | A kind of method of winter production essence ammonium |
| CN107572551B (en) * | 2017-08-31 | 2020-06-09 | 湖北双环科技股份有限公司 | Method for producing refined ammonium in winter |
| CN111661853A (en) * | 2020-01-03 | 2020-09-15 | 宁夏云泰科技有限公司 | Production process of industrial ammonium chloride |
| CN112142068A (en) * | 2020-09-07 | 2020-12-29 | 湖北兴福电子材料有限公司 | Method for producing high-purity ammonium chloride from industrial-grade ammonium chloride |
| CN112340912A (en) * | 2020-09-29 | 2021-02-09 | 陕西陕焦化工有限公司 | Method for recovering inorganic salt in ammonia desulphurization waste liquid |
| CN113698020A (en) * | 2021-08-30 | 2021-11-26 | 衢州华友钴新材料有限公司 | Method for reducing chlorine and COD (chemical oxygen demand) of ammonium sulfate concentrated mother liquor |
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| Publication number | Publication date |
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| CN1197772C (en) | 2005-04-20 |
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Owner name: DAI ZHAORONG Effective date: 20050812 Owner name: ZHAO XIANGHAI Free format text: FORMER OWNER: DEBANG CHEMICAL INDUSTRY GROUP CO. LTD., JIANGSU |
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Effective date of registration: 20050812 Address after: Room 2, unit 21, building 6, 401, neat Road, Sinpo District, Jiangsu, Lianyungang, 222001 Co-patentee after: Dai Chaorong Patentee after: Zhao Xianghai Address before: 222023 No. 51, Jiang Nan Road, Lianyungang, Jiangsu, Haizhou Patentee before: JIANGSU DEBANG CHEMICAL INDUSTRY GROUP CO.,LTD. |
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Owner name: DEBANG CHEMICAL INDUSTRY GROUP CO. LTD., JIANGSU Free format text: FORMER OWNER: ZHAO XIANGHAI Effective date: 20141020 Free format text: FORMER OWNER: DAI CHAORONG Effective date: 20141020 |
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Effective date of registration: 20141020 Address after: 222000 No. 51, South South Road, Haizhou District, Jiangsu, Lianyungang Patentee after: JIANGSU DEBANG CHEMICAL INDUSTRY GROUP CO.,LTD. Address before: Room 2, unit 21, building 6, 401, neat Road, Sinpo District, Jiangsu, Lianyungang, 222001 Patentee before: Zhao Xianghai Patentee before: Dai Chaorong |
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