CN101143877A - Method for preparing tetrakis(hydroxymethyl)phosphonium sulfate from phosphine generated in sodium hypophosphite production - Google Patents
Method for preparing tetrakis(hydroxymethyl)phosphonium sulfate from phosphine generated in sodium hypophosphite production Download PDFInfo
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- CN101143877A CN101143877A CNA2007101334851A CN200710133485A CN101143877A CN 101143877 A CN101143877 A CN 101143877A CN A2007101334851 A CNA2007101334851 A CN A2007101334851A CN 200710133485 A CN200710133485 A CN 200710133485A CN 101143877 A CN101143877 A CN 101143877A
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- sodium hypophosphite
- hydroxymethyl
- aqueous solution
- phosphine
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Abstract
The present invention relates to a method which prepares tetrakis (hydroxymethyl) phosphonium sulfate by utilizing the phosphine generated in the process of producing sodium hypophosphite. From the waste gas generated in the process of producing the sodium hypophosphite, the phosphine is collected and stored; aqueous solution is prepared with formaldehyde and sulfuric acid according to the molar ratio of 8.1 to 8.2:1; the aqueous solution is pumped into an absorption column by an erosion-resistant pump and is sprayed down from the top of the column, the phosphine gas in a gas vessel is pumped into the absorption column by a gas pump, and under the condition of temperature between 40 DEG C and 50 DEG C, a synthesis reaction is carried out, so that the aqueous solution of the tetrakis (hydroxymethyl) phosphonium sulfate is prepared. The tetrakis (hydroxymethyl) phosphonium sulfate (THPS) prepared with the harmful gas (phosphine) generated in the process of producing sodium hypophosphite is a quaternary alkylphosphonium salt bactericidal algicide, which has the advantages of high efficiency, broad spectrum, low toxicity, low dosage, low foamability and environmental protection. The tetrakis (hydroxymethyl) phosphonium sulfate can be biologically self-degraded, so no environmental pollution occurs. The present invention resolves the problem of environmental pollution caused by the waste gas generated in the process of producing sodium hypophosphite.
Description
Technical field
What the present invention relates to is a kind of method of producing the preparing tetra hydroxymethyl phosphorus sulfuric acid phosphorus in the waste gas that is produced in the sodium hypophosphite process of utilizing, and belongs to tetra methylol sulfuric acid phosphorus Technology field.
Background technology
Inferior sodium phosphate (Sodium Hypophosphite) has another name called sodium hypophosphite: be called for short SHPP/HYPO.Molecular formula: NaH
2PO
2.H
2O, molecular weight: 105.99.This product gives off pollutents such as a large amount of waste water,wastes gas and industrial residue in process of production.Wherein the waste gas main component is a phosphuret-(t)ed hydrogen, the method for existing processing:
One: phosphuret-(t)ed hydrogen is collected and stored, hydrogen peroxide is made into the certain density aqueous solution, under certain temperature condition, absorb phosphine gas with hydrogen peroxide solution, reaction generates Hypophosporous Acid, 50, absorb saturated after, in negative pressure, under the vacuum condition, be condensed into 50% Hypophosporous Acid, 50.50% Hypophosporous Acid, 50 that this method obtains contains 5% left and right sides phosphorous acid, and product is defective.
Two: will directly send in the tower with pipeline from the phosphuret-(t)ed hydrogen that reactor comes out and burn, and produce Vanadium Pentoxide in FLAKES, the water spray absorbs and obtains low value-added dilute phosphoric acid.When phosphine gas concentration less than 5% the time, can not produce burning, the poisonous phosphuret-(t)ed hydrogen of part enters in the atmosphere, and environment has been caused certain pollution.
Summary of the invention
The present invention is intended to make full use of the phosphuret-(t)ed hydrogen in the waste gas that gives off in the sodium hypophosphite production course, preparation tetra methylol sulfuric acid phosphorus, utilization of waste material.Practical toxic gas zero release simultaneously.
Technical solution of the present invention: the processing step of this method is divided into,
(1) in the waste gas that from sodium hypophosphite production course, is produced, collects and stores phosphuret-(t)ed hydrogen;
(2) with formaldehyde, sulfuric acid be in molar ratio: 8.1～8.2: 1 is made into the aqueous solution; This aqueous solution is squeezed into the absorption tower with noncorrosive pump, spray downwards, the phosphine gas in the gas tank is sent in the absorption tower, under 40～50 ℃ temperature condition, react synthetic, make the tetra methylol sulfuric acid phosphorus aqueous solution with air delivery pump from cat head;
Reaction formula is as follows:
8?HCHO+H
2SO
4+2?PH
3＝[(CH
2OH)
4P]
2SO
4，
Advantage of the present invention:
With producing the preparing tetra hydroxymethyl phosphorus sulfuric acid phosphorus in the waste gas in the sodium hypophosphite process, it is the quaternary alkylphosphonium salt Biocidal algae-killing agent, is a kind of novel, good, efficient, wide spectrum, low toxicity, low dosage, low foaming, environmentally friendly sterilant.Biological degradation can self take place in it, can not cause any pollution to environment.With formaldehyde, sulfuric acid phosphuret-(t)ed hydrogen is thoroughly absorbed.Realize toxic gas zero release in the sodium hypophosphite production course.Solved the problem of toxic gas environmental pollution in the sodium hypophosphite production course.
Embodiment
Embodiment 1:
Behind the sodium hypophosphite reactor feed 5 minutes, constantly there is phosphine gas to produce in the still, utilizes the pressure of gas reactor, phosphuret-(t)ed hydrogen is delivered directly in the gas holder tank collects.With formaldehyde, sulfuric acid is in molar ratio, is made into the aqueous solution at 8.2: 1.This aqueous solution is squeezed into the absorption tower with noncorrosive pump, spray downwards, the phosphine gas in the gas tank is sent in the absorption tower, under 50 ℃ temperature condition, react synthetic, make the tetra methylol sulfuric acid phosphorus aqueous solution with air delivery pump from cat head.
Reaction formula is as follows:
8?HCHO+H
2SO
4+2?PH
3＝[(CH
2OH)
4P]
2SO
4.
Embodiment 2:
Behind the sodium hypophosphite reactor feed 5 minutes, constantly there is phosphine gas to produce in the still, utilizes the pressure of gas reactor, phosphuret-(t)ed hydrogen is delivered directly in the gas holder tank collects.With formaldehyde, sulfuric acid is in molar ratio: be made into the aqueous solution at 8.1: 1.This aqueous solution is squeezed into the absorption tower with noncorrosive pump, spray downwards, the phosphine gas in the gas tank is sent in the absorption tower, under 40 ℃ temperature condition, react synthetic, make the tetra methylol sulfuric acid phosphorus aqueous solution with air delivery pump from cat head.
Reaction formula is as follows:
8?HCHO+H
2SO
4+2?PH
3＝[(CH
2OH)
4P]
2SO
4.
The biodegradable sterilant of tetra methylol sulfuric acid phosphorus (THPS).And this added value of product height, profit thoroughly absorbs phosphuret-(t)ed hydrogen with formaldehyde, sulfuric acid all more than 50%.Realize the toxic gas zero release.
Claims (2)
1. with the preparing tetra hydroxymethyl phosphorus sulfuric acid phosphorus method of producing in the sodium hypophosphite process, it is characterized in that the processing step of this method is divided into,
(1) in the waste gas that from sodium hypophosphite production course, is produced, collects and stores phosphuret-(t)ed hydrogen;
(2) with formaldehyde and sulfuric acid be in molar ratio: 8.1～8.2: 1 is made into the aqueous solution; This aqueous solution is squeezed into the absorption tower with noncorrosive pump, spray downwards, the phosphine gas in the gas tank is sent in the absorption tower, under 40～50 ℃ temperature condition, react synthetic, make the tetra methylol sulfuric acid phosphorus aqueous solution with air delivery pump from cat head;
Reaction formula is as follows:
8HCHO+H
2SO
4+2PH
3＝[(CH
2OH)
4P]
2SO
4.
2. the method for off gas treatment in the sodium hypophosphite production course according to claim 1, it is characterized in that the sodium hypophosphite reactor feed is after 5 minutes, constantly there is phosphine gas to produce in the still, utilizes the pressure of gas reactor, phosphuret-(t)ed hydrogen is delivered directly in the gas holder tank collects.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2007101334851A CN101143877B (en) | 2007-10-08 | 2007-10-08 | Method for preparing tetrakis(hydroxymethyl)phosphonium sulfate from phosphine generated in sodium hypophosphite production |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2007101334851A CN101143877B (en) | 2007-10-08 | 2007-10-08 | Method for preparing tetrakis(hydroxymethyl)phosphonium sulfate from phosphine generated in sodium hypophosphite production |
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| Publication Number | Publication Date |
|---|---|
| CN101143877A true CN101143877A (en) | 2008-03-19 |
| CN101143877B CN101143877B (en) | 2011-08-17 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102180904A (en) * | 2011-03-10 | 2011-09-14 | 常熟新特化工有限公司 | Preparation method for tetrakis hydroxymetyl phosphonium sulfuric |
-
2007
- 2007-10-08 CN CN2007101334851A patent/CN101143877B/en active Active
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102180904A (en) * | 2011-03-10 | 2011-09-14 | 常熟新特化工有限公司 | Preparation method for tetrakis hydroxymetyl phosphonium sulfuric |
| CN102180904B (en) * | 2011-03-10 | 2013-09-18 | 常熟新特化工有限公司 | Preparation method for tetrakis hydroxymetyl phosphonium sulfuric |
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|---|---|
| CN101143877B (en) | 2011-08-17 |
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Application publication date: 20080319 Assignee: Jiangsu Combined chemical co., Ltd Assignor: Jiangsu Kangxiang Group Company Contract record no.: 2014320000150 Denomination of invention: Method for preparing tetrakis(hydroxymethyl)phosphonium sulfate from phosphine generated in sodium hypophosphite production Granted publication date: 20110817 License type: Exclusive License Record date: 20140305 |
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Effective date of registration: 20180719 Address after: 212212 Yangtze River bridge, Zhenjiang, Jiangsu Province, east side of Yangtze River bridge, Yangzhong Patentee after: Jiangsu pure chemical industry Co., Ltd. Address before: 212212 Yangtze River bridge, Yangzhong, Jiangsu Province, east side of Yangtze River Bridge Patentee before: Jiangsu Kangxiang Group Company |