CN102167709A - Method for preparing Tetrakis (hydroxymethyl) phosphonium chloride - Google Patents
Method for preparing Tetrakis (hydroxymethyl) phosphonium chloride Download PDFInfo
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- CN102167709A CN102167709A CN2011100579650A CN201110057965A CN102167709A CN 102167709 A CN102167709 A CN 102167709A CN 2011100579650 A CN2011100579650 A CN 2011100579650A CN 201110057965 A CN201110057965 A CN 201110057965A CN 102167709 A CN102167709 A CN 102167709A
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Abstract
The invention relates to a method of preparing Tetrakis (hydroxymethyl) phosphonium chloride, Comprising adding hydrochloric acid and formaldehyde into a reaction vessel 1, Opening a gas-liquid mixing reaction pump 2, Adding hydrogen phosphide into the gas-liquid mixing reaction pump 2, Then absorbing hydrogen phosphide through gas-liquid mixing reaction apparatus at a temperature of 50 to 60 degrees, The unabsorbed hydrogen phosphide entering a next gas-liquid mixing reaction apparatus, Determining reaction terminal point by detecting formaldehyde content in process, Decompressing and condensing to achieve Tetrakis (hydroxymethyl) phosphonium chloride after the reaction, The invention has advantages of simple method, Low cost, 40% of reaction speed improving, Non obstruction appeared in equipment, Easy equipment installation and simple operation, And suitable for industrialization production of exhaust gas reutilizationoun.
Description
Technical field
The invention belongs to the organic preparation field of tetra methylol, particularly relate to a kind of preparation method of Tetrakis hydroxymethyl phosphonium chloride.
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 Tetrakis hydroxymethyl phosphonium chloride,, as CN101224378, open day 2008.07.23; CN101143877, open day 2008.03.19; CN101333228, open day 2008.12.31; CN101143878, open day 2008.3.19; 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 Tetrakis hydroxymethyl phosphonium chloride, 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:
PH
3+4HCHO+HCl→(HOCH
2)
4Pa
The preparation method of a kind of Tetrakis hydroxymethyl phosphonium chloride of the present invention comprises:
Hydrochloric 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 Tetrakis hydroxymethyl phosphonium chloride.
The mass ratio of described hydrochloric acid and formaldehyde is 1: 3.1-3.2.
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, feed phosphine gas simultaneously and carry out absorption reaction, on the gas-liquid circulation hybrid reaction pump liquids and gases import is arranged, the flow of this pump can reach 30m3/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 appear, and speed of response can improve about 40%, and equipment installs and 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.
A kind of preparation method of Tetrakis hydroxymethyl phosphonium chloride comprises:
In hydrochloric acid (30%) and the logical adding of formaldehyde (37%) 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 Tetrakis hydroxymethyl phosphonium chloride; Wherein the mass ratio of hydrochloric acid and formaldehyde is 1: 3.1-3.2.
Product effective constituent 80-82%, available phosphorus content 13-13.3%, PH 3-5.0, iron ion＜0.0015%, viscosity＜50cps, colourity＜100APHA is than smoked 1.320-1.400g/ml.
Claims (3)
1. the preparation method of a Tetrakis hydroxymethyl phosphonium chloride comprises:
Hydrochloric 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 Tetrakis hydroxymethyl phosphonium chloride.
2. the preparation method of a kind of Tetrakis hydroxymethyl phosphonium chloride according to claim 1, it is characterized in that: the mass ratio of described hydrochloric acid and formaldehyde is 1: 3.1-3.2.
3. the preparation method of a kind of Tetrakis hydroxymethyl phosphonium chloride 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 201110057965 CN102167709B (en) | 2011-03-10 | 2011-03-10 | Method for preparing Tetrakis (hydroxymethyl) phosphonium chloride |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110057965 CN102167709B (en) | 2011-03-10 | 2011-03-10 | Method for preparing Tetrakis (hydroxymethyl) phosphonium chloride |
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| CN102167709A true CN102167709A (en) | 2011-08-31 |
| CN102167709B CN102167709B (en) | 2013-11-06 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102924517A (en) * | 2012-10-18 | 2013-02-13 | 昆明理工大学 | Process for preparing tetramethylolphosphonium chloride by catalyzing phosphines with copper chlorides |
Citations (4)
| 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 |
| CN2920979Y (en) * | 2006-07-10 | 2007-07-11 | 重庆工学院 | Reaction system for treating sewage containing chromium by gas-liquid static mixing reduction method |
| CN101134763A (en) * | 2007-10-08 | 2008-03-05 | 江苏康祥集团公司 | Method for preparing tetra hydroxymethyl phosphorus trichloride-urea primary condensed polymer |
| CN101143878A (en) * | 2007-10-08 | 2008-03-19 | 江苏康祥集团公司 | Method for preparing tetrakis(hydroxymethyl)phosphonium chloride from phosphine generated in sodium hypophosphite production |
-
2011
- 2011-03-10 CN CN 201110057965 patent/CN102167709B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2920979Y (en) * | 2006-07-10 | 2007-07-11 | 重庆工学院 | Reaction system for treating sewage containing chromium by gas-liquid static mixing reduction method |
| 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 |
| CN101134763A (en) * | 2007-10-08 | 2008-03-05 | 江苏康祥集团公司 | Method for preparing tetra hydroxymethyl phosphorus trichloride-urea primary condensed polymer |
| CN101143878A (en) * | 2007-10-08 | 2008-03-19 | 江苏康祥集团公司 | Method for preparing tetrakis(hydroxymethyl)phosphonium chloride from phosphine generated in sodium hypophosphite production |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102924517A (en) * | 2012-10-18 | 2013-02-13 | 昆明理工大学 | Process for preparing tetramethylolphosphonium chloride by catalyzing phosphines with copper chlorides |
| CN102924517B (en) * | 2012-10-18 | 2015-06-03 | 昆明理工大学 | Process for preparing tetramethylolphosphonium chloride by catalyzing phosphines with copper chlorides |
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| CN102167709B (en) | 2013-11-06 |
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