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
- Publication number
- 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
- Authority
- CN
- China
- Prior art keywords
- gas
- sodium hypophosphite
- hydroxymethyl
- aqueous solution
- phosphine
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
- XYFCBTPGUUZFHI-UHFFFAOYSA-N Phosphine Chemical compound P XYFCBTPGUUZFHI-UHFFFAOYSA-N 0.000 title claims abstract description 28
- KWSLGOVYXMQPPX-UHFFFAOYSA-N 5-[3-(trifluoromethyl)phenyl]-2h-tetrazole Chemical compound FC(F)(F)C1=CC=CC(C2=NNN=N2)=C1 KWSLGOVYXMQPPX-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 229910001379 sodium hypophosphite Inorganic materials 0.000 title claims abstract description 20
- 238000000034 method Methods 0.000 title claims abstract description 19
- 229910000073 phosphorus hydride Inorganic materials 0.000 title claims abstract description 14
- 238000004519 manufacturing process Methods 0.000 title claims description 8
- YIEDHPBKGZGLIK-UHFFFAOYSA-L tetrakis(hydroxymethyl)phosphanium;sulfate Chemical compound [O-]S([O-])(=O)=O.OC[P+](CO)(CO)CO.OC[P+](CO)(CO)CO YIEDHPBKGZGLIK-UHFFFAOYSA-L 0.000 title abstract 6
- 239000007789 gas Substances 0.000 claims abstract description 25
- 239000007864 aqueous solution Substances 0.000 claims abstract description 16
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000010521 absorption reaction Methods 0.000 claims abstract description 10
- WSFSSNUMVMOOMR-UHFFFAOYSA-N Formaldehyde Chemical compound O=C WSFSSNUMVMOOMR-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000002912 waste gas Substances 0.000 claims abstract description 8
- 229910052739 hydrogen Inorganic materials 0.000 claims description 12
- 239000001257 hydrogen Substances 0.000 claims description 12
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 11
- DSMLVDLNGGAGGK-UHFFFAOYSA-N [P].C(O)OS(O)(=O)=O Chemical compound [P].C(O)OS(O)(=O)=O DSMLVDLNGGAGGK-UHFFFAOYSA-N 0.000 claims description 7
- 238000006243 chemical reaction Methods 0.000 claims description 5
- 239000007921 spray Substances 0.000 claims description 5
- 241000282326 Felis catus Species 0.000 claims description 4
- HPLZINFXTFTTMD-UHFFFAOYSA-N [P].S(O)(O)(=O)=O.OC[P] Chemical compound [P].S(O)(O)(=O)=O.OC[P] HPLZINFXTFTTMD-UHFFFAOYSA-N 0.000 claims description 4
- 230000009972 noncorrosive effect Effects 0.000 claims description 4
- 238000003912 environmental pollution Methods 0.000 abstract description 3
- 231100000053 low toxicity Toxicity 0.000 abstract description 2
- 150000003839 salts Chemical class 0.000 abstract description 2
- 239000003619 algicide Substances 0.000 abstract 1
- 230000000844 anti-bacterial effect Effects 0.000 abstract 1
- 230000007613 environmental effect Effects 0.000 abstract 1
- 230000003628 erosive effect Effects 0.000 abstract 1
- 238000003786 synthesis reaction Methods 0.000 abstract 1
- WSFSSNUMVMOOMR-NJFSPNSNSA-N methanone Chemical compound O=[14CH2] WSFSSNUMVMOOMR-NJFSPNSNSA-N 0.000 description 5
- 239000002341 toxic gas Substances 0.000 description 4
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 3
- 239000002253 acid Substances 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 description 2
- GNTDGMZSJNCJKK-UHFFFAOYSA-N divanadium pentaoxide Chemical compound O=[V](=O)O[V](=O)=O GNTDGMZSJNCJKK-UHFFFAOYSA-N 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 239000003139 biocide Substances 0.000 description 1
- 230000015556 catabolic process Effects 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000006731 degradation reaction Methods 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 150000002431 hydrogen Chemical class 0.000 description 1
- 231100000614 poison Toxicity 0.000 description 1
- 230000007096 poisonous effect Effects 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000001488 sodium phosphate Substances 0.000 description 1
- 229910000162 sodium phosphate Inorganic materials 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- ISIJQEHRDSCQIU-UHFFFAOYSA-N tert-butyl 2,7-diazaspiro[4.5]decane-7-carboxylate Chemical compound C1N(C(=O)OC(C)(C)C)CCCC11CNCC1 ISIJQEHRDSCQIU-UHFFFAOYSA-N 0.000 description 1
- RYFMWSXOAZQYPI-UHFFFAOYSA-K trisodium phosphate Chemical compound [Na+].[Na+].[Na+].[O-]P([O-])([O-])=O RYFMWSXOAZQYPI-UHFFFAOYSA-K 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Treating Waste Gases (AREA)
- Gas Separation By Absorption (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
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 |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN101143877A true CN101143877A (en) | 2008-03-19 |
| CN101143877B CN101143877B (en) | 2011-08-17 |
Family
ID=39206626
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2007101334851A Active CN101143877B (en) | 2007-10-08 | 2007-10-08 | Method for preparing tetrakis(hydroxymethyl)phosphonium sulfate from phosphine generated in sodium hypophosphite production |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN101143877B (en) |
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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| Publication number | Publication date |
|---|---|
| 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 |