CN102167709B - Method for preparing Tetrakis (hydroxymethyl) phosphonium chloride - Google Patents
Method for preparing Tetrakis (hydroxymethyl) phosphonium chloride Download PDFInfo
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- CN102167709B CN102167709B CN 201110057965 CN201110057965A CN102167709B CN 102167709 B CN102167709 B CN 102167709B CN 201110057965 CN201110057965 CN 201110057965 CN 201110057965 A CN201110057965 A CN 201110057965A CN 102167709 B CN102167709 B CN 102167709B
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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 through inhaling the spray absorber reaction, absorbing the tail gas phosphuret-(t)ed hydrogen that sodium hypophosphite produces, 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 gas tank is sent in the absorption tower, under the temperature condition of 40-50 ℃ to once spraying from tower top, reaction is synthetic, makes tetrakis hydroxymetyl phosphonium sulfuric 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 Contacting form.To be gas be dispersed in tray column, bubble absorbing tower, stirring bubble absorbing tower in liquid phase with bubble shape to the first kind; To be liquid be dispersed in injector, Venturi meter, spray tower in gas phase with droplet-like to Equations of The Second Kind; The 3rd class is packed absorber and the film-falling absorption tower that liquid contacts with gas phase with membranaceous motion.In tower, the flow pattern of gas-liquid two-phase can adverse current also can and flow.Usually adopt counter-current operation, absorption agent adds mobile from top to bottom with tower top, contact with the gas that flows from bottom to top, and the liquid that has absorbed absorbent is discharged at the bottom of tower, and purified gas is discharged from tower top.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of preparation method of Tetrakis hydroxymethyl phosphonium chloride, and the method is simple, and cost is low, and speed of response is fast, can not occur stopping up, and is suitable for waste gas recycling suitability for industrialized production.
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 reactor, open gas-liquid cycle hybrid reaction pump, phosphuret-(t)ed hydrogen is added in gas-liquid cycle hybrid reaction pump, absorb phosphuret-(t)ed hydrogen at 50-60 ℃ by the gas-liquid cycle mixed reactor, the phosphuret-(t)ed hydrogen that is not completely absorbed enters next gas-liquid cycle hybrid reaction pump, and (two gas-liquid cycle mixed reactors are the same, just be together in series, so more be conducive to the utilization of phosphuret-(t)ed hydrogen), detect the content judgement reaction end of formaldehyde by middle control, reaction finishes to obtain Tetrakis hydroxymethyl phosphonium chloride by concentrating under reduced pressure.
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 parity sodium phosphate process is through purifying treatment.
Beneficial effect
the present invention allows reaction circulate in reaction unit by gas-liquid cycle hybrid reaction pump, pass into simultaneously phosphine gas and carry out absorption reaction, on gas-liquid cycle hybrid reaction pump, the 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 40% left and right, and equipment is installed and is simple to operate, be suitable for waste gas recycling suitability for industrialized production.
Description of drawings
The schematic diagram of Fig. 1 gas-liquid cycle mixed reactor, 1 reactor wherein, 2 gas-liquid cycle 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 for explanation the present invention 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 limited range equally.
Embodiment 1
A kind of preparation method of Tetrakis hydroxymethyl phosphonium chloride comprises:
Add in reactor 1 hydrochloric acid (30%) and formaldehyde (37%) are logical, open gas-liquid cycle hybrid reaction pump 2, phosphine containing (80% left and right) tail gas that produces in will the production sodium hypophosphite process through purifying treatment adds in gas-liquid cycle hybrid reaction pump 2 by gas feed, absorb phosphuret-(t)ed hydrogen at 50-60 ℃ by the gas-liquid cycle mixed reactor, the phosphuret-(t)ed hydrogen that is not completely absorbed enters the next stage reactor, detect the content judgement reaction end of formaldehyde by middle control, reaction finishes to obtain Tetrakis hydroxymethyl phosphonium chloride by concentrating under reduced pressure; 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 (2)
1. the preparation method of a Tetrakis hydroxymethyl phosphonium chloride comprises:
Hydrochloric acid and formaldehyde are added in reactor (1), open gas-liquid cycle hybrid reaction pump (2), phosphuret-(t)ed hydrogen is added in gas-liquid cycle hybrid reaction pump (2), absorb phosphuret-(t)ed hydrogen at 50-60 ℃ by the gas-liquid cycle mixed reactor, the phosphuret-(t)ed hydrogen that is not completely absorbed enters next gas-liquid cycle hybrid reaction pump, detect the content judgement reaction end of formaldehyde by middle control, reaction finishes to obtain Tetrakis hydroxymethyl phosphonium chloride by concentrating under reduced pressure; Wherein, the mass ratio of hydrochloric acid and formaldehyde is 1:3.1-3.2.
2. 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 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 CN102167709A (en) | 2011-08-31 |
| CN102167709B true CN102167709B (en) | 2013-11-06 |
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| 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 |
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 |
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