CN102180904A - Preparation method for tetrakis hydroxymetyl phosphonium sulfuric - Google Patents
Preparation method for tetrakis hydroxymetyl phosphonium sulfuric Download PDFInfo
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- CN102180904A CN102180904A CN2011100579491A CN201110057949A CN102180904A CN 102180904 A CN102180904 A CN 102180904A CN 2011100579491 A CN2011100579491 A CN 2011100579491A CN 201110057949 A CN201110057949 A CN 201110057949A CN 102180904 A CN102180904 A CN 102180904A
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Abstract
The invention relates to a preparation method for tetrakis hydroxymetyl phosphonium sulfuric. The preparation method comprises the following steps of: adding sulfuric acid and formaldehyde into a reaction kettle (1); opening a gas-liquid circulation mixed reaction pump (2); adding hydrogen phosphide into the gas-liquid circulation mixed reaction pump (2); absorbing the hydrogen phosphide by using a gas-liquid circulation mixed reaction device at the temperature of between 50 and 60 DEG C; allowing the hydrogen phosphide which is not absorbed completely to enter the next gas liquid circulation mixed reaction pump; detecting the formaldehyde content through central control to determine the finishing point of the reaction; and after the reaction is finished, concentrating under reduced pressure to obtain the tetrakis hydroxymetyl phosphonium sulfuric. The preparation method is simple, and low in cost; the reaction speed can be improved by about 40 percent; equipment cannot be blocked; the equipment is easy to install and operate; and the preparation method is suitable for waste gas recycling industrialized production.
Description
Technical field
The invention belongs to the organic preparation field of tetra methylol, particularly relate to a kind of preparation method of tetra methylol sulfuric acid phosphorus.
Background technology
At present, produce the tail gas phosphuret-(t)ed hydrogen that sodium hypophosphite produces through inhaling the spray absorber reaction, absorbing, the existing bibliographical information of preparation tetra methylol sulfuric acid phosphorus, as CN101224378, open day 2008.07.23; CN101143877, open day 2008.03.19.Wherein CN101224378 has introduced the method for off gas treatment in the sodium hypophosphite production course, and processing step is divided into, and phosphuret-(t)ed hydrogen is collected and stored; With formaldehyde, sulfuric acid or hydrochloric acid are 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,, with air delivery pump the phosphine gas in the gas tank is sent in the absorption tower, under 40-50 ℃ temperature condition to once spraying from cat head, reaction is synthetic, makes the tetra methylol sulfuric acid phosphorus or the Tetrakis hydroxymethyl phosphonium chloride aqueous solution.But traditional spray column absorption tower speed of response is slow, easily stops up, and cleaning is inconvenient.
The absorption tower is divided three classes by the gas-liquid form that contacts.To be gas be dispersed in tray column, bubble absorbing tower, stirring bubble absorbing tower in the liquid phase with bubble shape to the first kind; To be liquid be dispersed in injector, Venturi meter, spray tower in the gas phase with droplet-like to second class; The 3rd class is packed absorber and the film-falling absorption tower that liquid contacts with gas phase with membranaceous motion.The flow pattern of gas-liquid two-phase can adverse current also can and flow in the tower.Usually adopt counter-current operation, absorption agent adds from top to bottom with cat head and flows, and contact with mobile gas from bottom to top, the liquid that has absorbed absorbent discharge at the bottom of the tower, and purified gas is discharged from cat head.
Summary of the invention
Technical problem to be solved by this invention provides a kind of preparation method of tetra methylol sulfuric acid phosphorus, and this method is simple, and cost is low, and speed of response is fast, can not occur stopping up, and is suitable for waste gas and utilizes suitability for industrialized production again.
Reaction formula of the present invention is as follows:
2PH
3+8HCHO+H
2SO
4→(HOCH
2)
4PSO
4O(CH
2OH)
4
The preparation method of a kind of tetra methylol sulfuric acid phosphorus of the present invention comprises:
Sulfuric acid and formaldehyde are added in the reactor, open gas-liquid circulation hybrid reaction pump, phosphuret-(t)ed hydrogen is added in the gas-liquid circulation hybrid reaction pump, absorb phosphuret-(t)ed hydrogen at 50-60 ℃ by gas-liquid circulation mixed reactor, the phosphuret-(t)ed hydrogen that is not absorbed fully enters next gas-liquid circulation hybrid reaction pump, and (two gas-liquid circulation mixed reactors are the same, just be together in series, so more help the utilization of phosphuret-(t)ed hydrogen), detect the content of formaldehyde by middle control and judge reaction end, reaction finishes after concentrating under reduced pressure obtains tetra methylol sulfuric acid phosphorus.
The mass ratio of described sulfuric acid and formaldehyde is 1: 7.0-7.1.
The tail gas containing phosphine that described phosphuret-(t)ed hydrogen is made a living and produced in the parity sodium phosphate process is through purifying treatment.
Beneficial effect
The present invention allows be reflected in the reaction unit by gas-liquid circulation hybrid reaction pump circulate, and feeds phosphine gas simultaneously and carries out absorption reaction, on the gas-liquid circulation hybrid reaction pump liquids and gases import is arranged, and the flow of this pump can reach 30m
3/ h, its content 40% of the highest permission, phosphine gas and reaction solution are by this pump powerful mixing and then be absorbed reaction, compare with traditional spray column absorption pattern, such reaction unit is simple, blocked situation can not occur, and speed of response can improve about 40%, and equipment is installed and is simple to operate, is suitable for waste gas and utilizes suitability for industrialized production again.
Description of drawings
The synoptic diagram of Fig. 1 gas-liquid circulation mixed reactor, 1 reactor wherein, 2 gas-liquid circulation hybrid reaction pumps.
Embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Embodiment 1
A kind of preparation method of tetra methylol sulfuric acid phosphorus comprises:
Sulfuric acid (98%) and formaldehyde (37%) are added in the reactor 1, open gas-liquid circulation hybrid reaction pump 2, phosphine containing (about the 80%) tail gas that produces in will the production sodium hypophosphite process through purifying treatment adds in the gas-liquid circulation hybrid reaction pump 2 by gas feed, absorb phosphuret-(t)ed hydrogen at 50-60 ℃ by gas-liquid circulation mixed reactor, the phosphuret-(t)ed hydrogen that is not absorbed fully enters the next stage reactor, detect the content of formaldehyde by middle control and judge reaction end, reaction finishes after concentrating under reduced pressure obtains tetra methylol sulfuric acid phosphorus.Wherein the mass ratio of sulfuric acid and formaldehyde is 1: 7.0-7.1.
Product master content 75-77%, available phosphorus content 11.0-12.0%, PH 3.0-5.0, iron ion＜0.0015%, viscosity＜50cps, colourity＜100APHA, proportion 1.370-1.400g/ml.
Claims (3)
1. the preparation method of a tetra methylol sulfuric acid phosphorus comprises:
Sulfuric acid and formaldehyde are added in the reactor (1), open gas-liquid circulation hybrid reaction pump (2), phosphuret-(t)ed hydrogen is added in the gas-liquid circulation hybrid reaction pump (2), absorb phosphuret-(t)ed hydrogen at 50-60 ℃ by gas-liquid circulation mixed reactor, the phosphuret-(t)ed hydrogen that is not absorbed fully enters next gas-liquid circulation hybrid reaction pump, detect the content of formaldehyde by middle control and judge reaction end, reaction finishes after concentrating under reduced pressure obtains tetra methylol sulfuric acid phosphorus.
2. the preparation method of a kind of tetra methylol sulfuric acid phosphorus according to claim 1 is characterized in that: the mass ratio of described sulfuric acid and formaldehyde is 1: 7.0-7.1.
3. the preparation method of a kind of tetra methylol sulfuric acid phosphorus according to claim 1 is characterized in that: the tail gas containing phosphine that described phosphuret-(t)ed hydrogen is made a living and produced in the parity sodium phosphate process, and through purifying treatment.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110057949 CN102180904B (en) | 2011-03-10 | 2011-03-10 | Preparation method for tetrakis hydroxymetyl phosphonium sulfuric |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110057949 CN102180904B (en) | 2011-03-10 | 2011-03-10 | Preparation method for tetrakis hydroxymetyl phosphonium sulfuric |
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| CN102180904A true CN102180904A (en) | 2011-09-14 |
| CN102180904B CN102180904B (en) | 2013-09-18 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117680083A (en) * | 2024-02-04 | 2024-03-12 | 常熟新特化工有限公司 | Preparation process and preparation device of tetrakis (hydroxymethyl) phosphonium sulfate |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1948247A (en) * | 2006-11-07 | 2007-04-18 | 中唯炼焦技术国家工程研究中心有限责任公司 | New method of preparing tert-butyl phenol by alkylation of phenol and isobutene |
| CN101143877A (en) * | 2007-10-08 | 2008-03-19 | 江苏康祥集团公司 | Method for preparing tetrakis(hydroxymethyl)phosphonium sulfate from phosphine generated in sodium hypophosphite production |
| CN101560225A (en) * | 2009-05-27 | 2009-10-21 | 江苏省丹爱化工有限公司 | Preparation method of tetrakis hydroxymetyl phosphonium sulfuric-urea polymer |
-
2011
- 2011-03-10 CN CN 201110057949 patent/CN102180904B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1948247A (en) * | 2006-11-07 | 2007-04-18 | 中唯炼焦技术国家工程研究中心有限责任公司 | New method of preparing tert-butyl phenol by alkylation of phenol and isobutene |
| CN101143877A (en) * | 2007-10-08 | 2008-03-19 | 江苏康祥集团公司 | Method for preparing tetrakis(hydroxymethyl)phosphonium sulfate from phosphine generated in sodium hypophosphite production |
| CN101560225A (en) * | 2009-05-27 | 2009-10-21 | 江苏省丹爱化工有限公司 | Preparation method of tetrakis hydroxymetyl phosphonium sulfuric-urea polymer |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117680083A (en) * | 2024-02-04 | 2024-03-12 | 常熟新特化工有限公司 | Preparation process and preparation device of tetrakis (hydroxymethyl) phosphonium sulfate |
| CN117680083B (en) * | 2024-02-04 | 2024-05-24 | 常熟新特化工有限公司 | Preparation process and preparation device of tetrakis (hydroxymethyl) phosphonium sulfate |
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|---|---|
| CN102180904B (en) | 2013-09-18 |
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