CN101181983B - Method for producing hypophosphorous acid - Google Patents
Method for producing hypophosphorous acid Download PDFInfo
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- CN101181983B CN101181983B CN200710168768XA CN200710168768A CN101181983B CN 101181983 B CN101181983 B CN 101181983B CN 200710168768X A CN200710168768X A CN 200710168768XA CN 200710168768 A CN200710168768 A CN 200710168768A CN 101181983 B CN101181983 B CN 101181983B
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- hypophosphorous acid
- hypophosporous acid
- feed liquid
- acid
- sulfate
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Abstract
The invention relates to a method of producing hypophosphorous acid, which comprises the following steps: a. a portion of concentrated sulfuric acid is put into a reaction vessel, in which two portions of hypophosphorous acid are fed, and then the mixture solution is stirred and reacts for 1-2 hours; b. after the reaction is finished, residue and feed liquid are separated by a centrifuge, the feed liquid separated is 70-75 percent of the hypophosphorous acid by content and the residue is sodium sulfate; c. adequate barium hydroxide solution is added into the feed liquid of the hypophosphorousacid separated, which causes sulfate radical to generate barium sulfate deposition, and the barium sulfate is removed through filtration, thus obtaining the hypophosphorous acid; d. the concentrationof the hypophosphorous acid obtained in the step c is adjusted to 50 percent by adding water and then the solution obtained is packed, thus obtaining the hypophosphorous acid product. The invention uses the concentrated sulfuric acid and sodium hypophosphite to generate the hypophosphorous acid and the sodium sulfate through reaction, and the technique process does not cause environmental problems such as wastewater, etc. Furthermore, the velocity ratio of double decomposition reaction is very fast, thus being especially applicable for mass production and greatly improving the production capacity of the hypophosphorous acid.
Description
Technical field
The present invention relates to a kind of method of producing Hypophosporous Acid, 50.
Background technology
The existing Hypophosporous Acid, 50 of producing all adopts ion exchange method, is that sodium hypophosphite solution is passed through ion-exchange techniques, obtains the low concentration Hypophosporous Acid, 50, through concentrating, obtains product again.This method yields poorly, and can produce waste water.
Summary of the invention
Purpose of the present invention is exactly that a kind of method of producing Hypophosporous Acid, 50 will be provided, and it uses sulfuric acid and sodium hypophosphite to be the raw material production Hypophosporous Acid, 50, need not pass through ion-exchange, can not produce discharge of wastewater.
The object of the present invention is achieved like this: a kind of method of producing Hypophosporous Acid, 50, and it may further comprise the steps:
A. earlier 1 part the vitriol oil is squeezed in the reactor, squeezed into 2 parts sodium hypophosphite stirring reaction 1-2 hour again;
B. after reaction finishes, separate slag and feed liquid with whizzer, the feed liquid of being separated is the Hypophosporous Acid, 50 of content at 70-75%, and slag is a sodium sulfate;
C. the barium hydroxide solution that adds capacity in isolated Hypophosporous Acid, 50 feed liquid makes sulfate radical generate barium sulfate precipitate, removes by filter barium sulfate and promptly obtains Hypophosporous Acid, 50;
D. the Hypophosporous Acid, 50 that the c step is obtained adds water and is adjusted to after 50% the concentration again that packing promptly obtains the Hypophosporous Acid, 50 product.
The present invention uses the vitriol oil and sodium hypophosphite reaction to produce Hypophosporous Acid, 50 and sodium sulfate, technological process can not brought environmental problems such as waste water, and,, improved the throughput of Hypophosporous Acid, 50 greatly so be particularly suitable for producing in enormous quantities because the replacement(metathesis)reaction velocity ratio is very fast.
Embodiment
A kind of method of producing Hypophosporous Acid, 50, it may further comprise the steps:
A. earlier 1 part the vitriol oil is squeezed in the reactor, squeezed into 2 parts sodium hypophosphite stirring reaction 1-2 hour again;
B. after reaction finishes, separate slag and feed liquid with whizzer, the feed liquid of being separated is the Hypophosporous Acid, 50 of content at 70-75%, and slag is a sodium sulfate;
C. the barium hydroxide solution that adds capacity in isolated Hypophosporous Acid, 50 feed liquid makes sulfate radical generate barium sulfate precipitate, removes by filter barium sulfate and promptly obtains Hypophosporous Acid, 50;
D. the Hypophosporous Acid, 50 that the c step is obtained adds water and is adjusted to after 50% the concentration again that packing promptly obtains the Hypophosporous Acid, 50 product.
The Hypophosporous Acid, 50 product of producing with the present invention reaches following standard:
Project | Hypophosporous Acid, 50 | Phosphorous acid | Iron | Chlorine | Vitriol |
Index (%) | >50.0 | <0.5 | <0.0005 | <0.005 | <0.005 |
Claims (1)
1. method of producing Hypophosporous Acid, 50 is characterized in that it may further comprise the steps:
A. earlier 1 part the vitriol oil is squeezed in the reactor, squeezed into 2 parts sodium hypophosphite stirring reaction 1-2 hour again;
B. after reaction finishes, separate slag and feed liquid with whizzer, the feed liquid of being separated is the Hypophosporous Acid, 50 of content at 70-75%, and slag is a sodium sulfate;
C. the barium hydroxide solution that adds capacity in isolated Hypophosporous Acid, 50 feed liquid makes sulfate radical generate barium sulfate precipitate, removes by filter barium sulfate and promptly obtains Hypophosporous Acid, 50;
D. the Hypophosporous Acid, 50 that the c step is obtained adds water and is adjusted to after 50% the concentration again that packing promptly obtains the Hypophosporous Acid, 50 product.
Priority Applications (1)
Application Number | Priority Date | Filing Date | Title |
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CN200710168768XA CN101181983B (en) | 2007-12-12 | 2007-12-12 | Method for producing hypophosphorous acid |
Applications Claiming Priority (1)
Application Number | Priority Date | Filing Date | Title |
---|---|---|---|
CN200710168768XA CN101181983B (en) | 2007-12-12 | 2007-12-12 | Method for producing hypophosphorous acid |
Publications (2)
Publication Number | Publication Date |
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CN101181983A CN101181983A (en) | 2008-05-21 |
CN101181983B true CN101181983B (en) | 2010-12-22 |
Family
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Family Applications (1)
Application Number | Title | Priority Date | Filing Date |
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CN200710168768XA Active CN101181983B (en) | 2007-12-12 | 2007-12-12 | Method for producing hypophosphorous acid |
Country Status (1)
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CN (1) | CN101181983B (en) |
Families Citing this family (3)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN104386659B (en) * | 2014-11-15 | 2019-10-25 | 周骏宏 | A method of hypophosphorous acid is produced with phosphorous chemical industry waste material |
CN114873613B (en) * | 2022-05-16 | 2023-10-27 | 湖北吉星化工集团有限责任公司 | Method for refining and recovering sodium hypophosphite by using byproduct sodium sulfate |
CN115744848A (en) * | 2022-12-29 | 2023-03-07 | 河南红东方化工股份有限公司 | Phosphorus pentafluoride synthesis method |
Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5897848A (en) * | 1997-09-19 | 1999-04-27 | Learonal Inc. | Process for producing hypophosphite compounds |
CN1762796A (en) * | 2005-09-07 | 2006-04-26 | 南开大学 | High grade sodium hypophosphite preparation method |
-
2007
- 2007-12-12 CN CN200710168768XA patent/CN101181983B/en active Active
Patent Citations (2)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US5897848A (en) * | 1997-09-19 | 1999-04-27 | Learonal Inc. | Process for producing hypophosphite compounds |
CN1762796A (en) * | 2005-09-07 | 2006-04-26 | 南开大学 | High grade sodium hypophosphite preparation method |
Non-Patent Citations (2)
Title |
---|
毛谙章等.次磷酸及其盐的制备与副产物的回收利用综述.广东化工.2004,(1),1-3. * |
程建忠等.次磷酸的新型生产方法的研究.离子交换与吸附.2001,17(3),271-275. * |
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CN101181983A (en) | 2008-05-21 |
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