CN101481390A - Raw material components and production method of diphenyl phosphorus chloride - Google Patents
Raw material components and production method of diphenyl phosphorus chloride Download PDFInfo
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- CN101481390A CN101481390A CNA2008100161686A CN200810016168A CN101481390A CN 101481390 A CN101481390 A CN 101481390A CN A2008100161686 A CNA2008100161686 A CN A2008100161686A CN 200810016168 A CN200810016168 A CN 200810016168A CN 101481390 A CN101481390 A CN 101481390A
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Abstract
The invention relates to raw material components and a production method of chlorodiphenylphosphine, and belongs to the technical field of chemical product formulas and production methods. Based on mass part, the raw material components are as follows: 0.8-1.5 parts of an active metal, 1-4 parts of benzene halide, 1-3 parts of phosphorus trichloride, 1-8 parts of an organic solvent and 0.03-0.1 part of a catalyst. The production method comprises the following steps: 1. mixing and adding the organic solvent and the active metal to a dispersing kettle based on the mass part, heating and stirring to disperse the active metal, and adding the benzene halide for a first initiation; 2. cooling the materials after dispersion, adding the same amount of the benzene halide for a second initiation, cooling and adding the remaining benzene halide and the phosphorus trichloride; 3. allowing reaction, adding the catalyst, and heating for reaction; 4. filtering through a press filter cone when the materials are hot; and 5. putting the filter pressed materials in a rectifying still and stirring, distilling off the solvent at normal pressure, rectifying a finished chlorodiphenylphosphine product at negative pressure, checking and packaging. The raw material components and the production method have the advantages of 1. shortening the reaction time, reducing the side reaction and improving the yield; and 2. avoiding a hydrolysis procedure, eliminating sewage discharge and reducing the raw material consumption.
Description
One, affiliated technical field
The present invention relates to a kind of feed composition, production method of diphenyl phosphorus chloride, belong to Chemicals prescription and production method technical field.
Two, background technology
Prior art diphenyl phosphorus chloride production method is that benzene and phosphorus trichloride is synthetic under aluminum chloride catalysis:
2C
6H
6+PCl
3+AlCl
3----→Ph
2PCl+2?HCl
Use a large amount of aluminum chlorides in the reaction process, caused environmental pollution, product aftertreatment difficulty in addition, bad filtration causes difficulty for big production of industry, and product yield is low, cost is high, long reaction time.
Three, summary of the invention
The objective of the invention is to overcome the defective that the above prior art diphenyl phosphorus chloride production method exists, a kind of yield height is provided, cost is low, the reaction times is short, diphenyl phosphorus chloride feed composition, production method that pollution-free and production process is easy to control.
The present invention is that a kind of halogenide with active metal, benzene, phosphorus trichloride are raw material, under the effect of organic solvent catalyst neutralisation, and synthetic diphenyl phosphorus chloride.
The technology of the present invention solution is as follows:
A kind of feed composition of diphenyl phosphorus chloride, the halogenide, phosphorus trichloride, organic solvent, the catalyzer that comprise active metal, benzene, according to the mass parts meter, halogenide 1-4 part of active metal 0.8-1.5 part, benzene, 1～3 part of phosphorus trichloride, organic solvent 1-8 part, catalyzer 0.03-0.1 part;
Described active metal comprises sodium Na, potassium K, magnesium Mg etc.; The halogenide of described benzene comprises chlorobenzene, bromination benzene, benzene iodide etc.; Described organic solvent comprises toluene, dimethylbenzene, sherwood oil etc.; Described catalyzer is a metal chloride, comprises aluminum chloride AlCl
3, calcium chloride CaCl
2Deng;
The production method of diphenyl phosphorus chloride of the present invention,
1, in anhydrous, anaerobic and have under the protection of nitrogen gas condition, according to the mass parts meter, the adding Scattered Kettle is mixed in 1-8 part organic solvent, 0.8-1.5 part active metal, be heated to 90-130 ℃, with 300-2500 rev/min stirring velocity dispersed with stirring active metal 2～40 minutes, make the active metal be dispersed into the following particulate of 120 μ m, the halogenide that adds 0.02～0.1 part of benzene carries out the first time and causes;
When 2, treating 2-3 ℃ of temperature rising after causing for the first time, material after will disperseing is cooled to 40-70 ℃ at once, the halogenide that adds the benzene of same quantity again carries out after secondary causes, be cooled to 10-30 ℃ rapidly, after dripping halid 10～15% abundant initiations of total amount 1-4 part benzene, halogenide and 1～3 part of phosphorus trichloride that will remain benzene again mix adding simultaneously;
3, add after, temperature adds 0.03-0.1 part catalyzer of measuring 20-80 ℃ of reaction 1-2 hour again, is warming up between 80-120 ℃ reaction 0.5-2.5 hour;
4, under pressure 0.1-0.3Mpa, by press filtration bucket filtered while hot, purpose is to remove the salt and the catalyzer of generation;
5, the material after the press filtration is put into rectifying still stir, under normal pressure distilling off solvent, rectifying goes out the finished product diphenyl phosphorus chloride under the 0.005-0.009Mpa negative pressure, checks, packing.
Its chemical equation is: (halogenide chlorobenzene, phosphorus trichloride, organic solvent dimethylbenzene, catalyzer aluminum chloride with active metal sodium, benzene are example),
The production method of diphenyl phosphorus chloride of the present invention has a large amount of by-product salt or salt slag;
The production method of diphenyl phosphorus chloride of the present invention, intermediates do not separate, and remove hydrolyzing process, and directly disproportionation changes into diphenyl phosphorus chloride;
The production method of diphenyl phosphorus chloride of the present invention is compared with existing technology, has following technological merit:
1, changes feed way: halobenzene is mixed adding simultaneously with phosphorus trichloride, shortened the reaction times, reduced side reaction, improved yield;
2, the triphenyl phosphorus of Sheng Chenging does not separate, and allows it and the phenyl phosphorus dichloride that generates simultaneously finish conversion reaction under the effect of catalyzer; Having cancelled hydrolyzing process, eliminated sewage discharge, reduced raw materials consumption, is the environment-protective process of cleanliness without any pollution;
3, this process using single stage method has reclaimed salt, has reduced cost, has increased the security of producing;
4, this is the method for preparing diphenyl phosphorus chloride that present technology is the easiest, three waste discharge is minimum, production is the safest, yield is the highest.
Four, embodiment
Provide specific embodiments of the invention below:
Embodiment 1
The feed composition of a kind of diphenyl phosphorus chloride of present embodiment, include halogenide, phosphorus trichloride, organic solvent, the catalyzer of active metal, benzene, wherein according to the mass parts meter, 1 part in the halogenide of 0.8 part in active metal sodium, benzene, 1 part of phosphorus trichloride, 1 part of organic solvent, 0.03 part of catalyzer;
The production method of present embodiment diphenyl phosphorus chloride is as follows:
In following examples production method, be example with halogenide chlorobenzene, organic solvent dimethylbenzene, the catalyzer aluminum chloride of active metal sodium, benzene;
1, in anhydrous, anaerobic and have under the protection of nitrogen gas condition, according to the mass parts meter, 1 part of dimethylbenzene, 0.8 part of sodium Metal 99.5 are dropped in the Scattered Kettle, sealing pot mouth, open jacket steam and be heated to 90-130 ℃, with 300-2500 rev/min dispersed with stirring sodium Metal 99.5 2-40 minute, make sodium be dispersed into the following particulate of 120 μ m, adds 0.02 part of chlorobenzene and carry out the initiation first time;
When 2, treating 2-3 ℃ of temperature rising, material after will disperseing is cooled to 40-70 ℃ at once, the chlorobenzene that adds same quantity again carries out after secondary causes, be cooled to 10-30 ℃ rapidly, dripping total amount is after 10～15% of 1 part of chlorobenzene fully causes, material is changed in the synthesis reactor, control 10-30 ℃, more remaining chlorobenzene and 1 part of phosphorus trichloride are mixed adding simultaneously;
3, add after, temperature was 20-80 ℃ of reaction 1-2 hour, 0.03 part of aluminum chloride that will measure again adds, and is warming up between 80-120 ℃ reaction 0.5-2.5 hour;
4, under pressure 0.1-0.3Mpa,, remove the salt and the catalyzer of generation by press filtration bucket filtered while hot;
5, the material after the press filtration is put into rectifying still stir, under normal pressure distilling off solvent, rectifying goes out the finished product diphenyl phosphorus chloride under the 0.005-0.009Mpa negative pressure, checks, packing.
Its chemical equation is:
The difference of a kind of diphenyl phosphorus chloride of embodiment 2 present embodiments and embodiment 1 is,
The feed composition of a kind of diphenyl phosphorus chloride of present embodiment, include halogenide, phosphorus trichloride, organic solvent, the catalyzer of active metal, benzene, wherein according to the mass parts meter, 4 parts in the halogenide of 1.5 parts of active metals, benzene, 3 parts of phosphorus trichlorides, 8 parts of organic solvents, 0.1 part of catalyzer;
The difference of the production method of present embodiment diphenyl phosphorus chloride and embodiment 1 is,
1, in anhydrous, anaerobic and have under the protection of nitrogen gas condition, according to the mass parts meter, 8 parts of dimethylbenzene, 1.5 parts of sodium Metal 99.5s are mixed the adding Scattered Kettle, be heated to 90-130 ℃, with 300-2500 rev/min stirring velocity dispersed with stirring sodium Metal 99.5 2～40 minutes, make sodium be dispersed into the following particulate of 120 μ m, add 0.1 part of chlorobenzene and carry out the initiation first time;
When 2, treating 2-3 ℃ of temperature rising, material after will disperseing is cooled to 40-70 ℃ at once, the chlorobenzene that adds same quantity again carries out after secondary causes, be cooled to 10-30 ℃ rapidly, dripping total amount is after 10～15% of 4 parts of chlorobenzenes fully cause, more remaining chlorobenzene and 3 parts of phosphorus trichlorides to be mixed adding simultaneously;
3, add after, temperature was 20-80 ℃ of reaction 1-2 hour, 0.1 part of aluminum chloride that will measure again adds, and is warming up between 80-120 ℃ reaction 0.5-2.5 hour;
4,5 with embodiment 1.
Embodiment 3: the difference of a kind of diphenyl phosphorus chloride of present embodiment and embodiment 1 is,
The feed composition of a kind of diphenyl phosphorus chloride of present embodiment, include halogenide, phosphorus trichloride, organic solvent, the catalyzer of active metal, benzene, wherein according to the mass parts meter, 2 parts in the halogenide of 1.0 parts of active metals, benzene, 1.5 parts of phosphorus trichlorides, 2 parts of organic solvents, 0.05 part of catalyzer;
The difference of the production method of present embodiment diphenyl phosphorus chloride and embodiment 1 is,
1, in anhydrous, anaerobic and have under the protection of nitrogen gas condition, according to the mass parts meter, 2 parts of dimethylbenzene, 1.0 parts of sodium Metal 99.5s are mixed the adding Scattered Kettle, be heated to 90-130 ℃, with 300-2500 rev/min stirring velocity dispersed with stirring sodium Metal 99.5 2～40 minutes, make sodium be dispersed into the following particulate of 120 μ m, add 0.04 part of chlorobenzene and carry out the initiation first time;
When 2, treating 2-3 ℃ of temperature rising, material after will disperseing is cooled to 40-70 ℃ at once, the chlorobenzene that adds same quantity again carries out after secondary causes, be cooled to 10-30 ℃ rapidly, dripping total amount is after 10～15% of 2 parts of chlorobenzenes fully cause, more remaining chlorobenzene and 1.5 parts of phosphorus trichlorides to be mixed adding simultaneously;
3, add after, temperature was 20-80 ℃ of reaction 1-2 hour, 0.05 part of aluminum chloride that will measure again adds, and is warming up between 80-120 ℃ reaction 0.5-2.5 hour;
4,5 with embodiment 1.
The difference of a kind of diphenyl phosphorus chloride of embodiment 4 present embodiments and embodiment 1 is,
The feed composition of a kind of diphenyl phosphorus chloride of present embodiment, include halogenide, phosphorus trichloride, organic solvent, the catalyzer of active metal, benzene, wherein according to the mass parts meter, 3 parts in the halogenide of 1.2 parts of active metals, benzene, 2.5 parts of phosphorus trichlorides, 4 parts of organic solvents, 0.06 part of catalyzer;
The difference of the production method of present embodiment diphenyl phosphorus chloride and embodiment 1 is,
1, in anhydrous, anaerobic and have under the protection of nitrogen gas condition, according to the mass parts meter, 4 parts of dimethylbenzene, 1.2 parts of sodium Metal 99.5s are mixed the adding Scattered Kettle, be heated to 90-130 ℃, with 300-2500 rev/min stirring velocity dispersed with stirring sodium Metal 99.5 2～40 minutes, make sodium be dispersed into the following particulate of 120 μ m, add 0.06 part of chlorobenzene and carry out the initiation first time;
When 2, treating 2-3 ℃ of temperature rising, material after will disperseing is cooled to 40-70 ℃ at once, the chlorobenzene that adds same quantity again carries out after secondary causes, be cooled to 10-30 ℃ rapidly, dripping total amount is after 10～15% of 3 parts of chlorobenzenes fully cause, more remaining chlorobenzene and 2.5 parts of phosphorus trichlorides to be mixed adding simultaneously;
3, add after, temperature was 20-80 ℃ of reaction 1-2 hour, 0.06 part of aluminum chloride that will measure again adds, and is warming up between 80-120 ℃ reaction 0.5-2.5 hour;
4,5 with embodiment 1.
The difference of a kind of diphenyl phosphorus chloride of embodiment 5 present embodiments and embodiment 1 is,
The feed composition of a kind of diphenyl phosphorus chloride of present embodiment, include halogenide, phosphorus trichloride, organic solvent, the catalyzer of active metal, benzene, wherein according to the mass parts meter, 1.5 parts in the halogenide of 1.5 parts of active metals, benzene, 2 parts of phosphorus trichlorides, 6 parts of organic solvents, 0.08 part of catalyzer;
The difference of the production method of present embodiment diphenyl phosphorus chloride and embodiment 1 is,
1, in anhydrous, anaerobic and have under the protection of nitrogen gas condition, according to the mass parts meter, 6 parts of dimethylbenzene, 1.5 parts of sodium Metal 99.5s are mixed the adding Scattered Kettle, be heated to 90-130 ℃, with 300-2500 rev/min stirring velocity dispersed with stirring sodium Metal 99.5 2～40 minutes, make sodium be dispersed into the following particulate of 120 μ m, add 0.08 part of chlorobenzene and carry out the initiation first time;
When 2, treating 2-3 ℃ of temperature rising, material after will disperseing is cooled to 40-70 ℃ at once, the chlorobenzene that adds same quantity again carries out after secondary causes, be cooled to 10-30 ℃ rapidly, dripping total amount is after 10～15% of 1.5 parts of chlorobenzenes fully cause, more remaining chlorobenzene and 2 parts of phosphorus trichlorides to be mixed adding simultaneously;
3, add after, temperature was 20-80 ℃ of reaction 1-2 hour, 0.08 part of aluminum chloride that will measure again adds, and is warming up between 80-120 ℃ reaction 0.5-2.5 hour;
4,5 with embodiment 1.
The difference of a kind of diphenyl phosphorus chloride of embodiment 6 present embodiments and embodiment 1 is,
The feed composition of a kind of diphenyl phosphorus chloride of present embodiment, include halogenide, phosphorus trichloride, organic solvent, the catalyzer of active metal, benzene, wherein according to the mass parts meter, 3.5 parts in the halogenide of 1.4 parts of active metals, benzene, 1.3 parts of phosphorus trichlorides, 7 parts of organic solvents, 0.09 part of catalyzer;
The difference of the production method of present embodiment diphenyl phosphorus chloride and embodiment 1 is,
1, in anhydrous, anaerobic and have under the protection of nitrogen gas condition, according to the mass parts meter, 7 parts of dimethylbenzene, 1.4 parts of sodium Metal 99.5s are mixed the adding Scattered Kettle, be heated to 90-130 ℃, with 300-2500 rev/min stirring velocity dispersed with stirring sodium Metal 99.5 2～40 minutes, make sodium be dispersed into the following particulate of 120 μ m, add 0.09 part of chlorobenzene and carry out the initiation first time;
When 2, treating 2-3 ℃ of temperature rising, material after will disperseing is cooled to 40-70 ℃ at once, the chlorobenzene that adds same quantity again carries out after secondary causes, be cooled to 10-30 ℃ rapidly, dripping total amount is after 10～15% of 3.5 parts of chlorobenzenes fully cause, more remaining chlorobenzene and 1.3 parts of phosphorus trichlorides to be mixed adding simultaneously;
3, add after, temperature was 20-80 ℃ of reaction 1-2 hour, 0.09 part of aluminum chloride that will measure again adds, and is warming up between 80-120 ℃ reaction 0.5-2.5 hour;
4,5 with embodiment 1.
The above embodiment of the production method of diphenyl phosphorus chloride of the present invention compares with existing two step method technology, all can realize purpose of the present invention, has following technological merit, and through the production method effect stability of experiment and the probationary certificate diphenyl phosphorus chloride of the present invention in 1 year, the following advantage that reaches.
1, changes feed way: chlorobenzene is mixed adding simultaneously with phosphorus trichloride, shortened the reaction times, reduced side reaction, improved yield;
2, the triphenyl phosphorus of Sheng Chenging does not separate, and allows it and the phenyl phosphorus dichloride that generates simultaneously finish conversion reaction under the effect of catalyzer; Having cancelled hydrolyzing process, eliminated sewage discharge, reduced raw materials consumption, is the environment-protective process of cleanliness without any pollution;
3, this process using single stage method has reclaimed salt, has reduced cost, has increased the security of producing;
4, this is the method for preparing diphenyl phosphorus chloride that present technology is the easiest, three waste discharge is minimum, production is the safest, yield is the highest.
Claims (6)
1, a kind of feed composition of diphenyl phosphorus chloride, it is characterized in that: the halogenide, phosphorus trichloride, organic solvent, the catalyzer that comprise active metal, benzene, according to the mass parts meter, halogenide 1-4 part of active metal 0.8-1.5 part, benzene, 1～3 part of phosphorus trichloride, organic solvent 1-8 part, catalyzer 0.03-0.1 part.
2, require the feed composition of 1 described a kind of diphenyl phosphorus chloride according to right, it is characterized in that: described active metal be following any one: sodium Na, potassium K, magnesium Mg.
3 require the feed composition of 1 described a kind of diphenyl phosphorus chloride according to right, it is characterized in that: the halogenide of described benzene be following any one: chlorobenzene, bromination benzene, benzene iodide.
4, require the feed composition of 1 described a kind of diphenyl phosphorus chloride according to right, it is characterized in that: described organic solvent be following any one: toluene, dimethylbenzene, sherwood oil.
5, require the feed composition of 1 described a kind of diphenyl phosphorus chloride according to right, it is characterized in that: described catalyzer be following any one: aluminum chloride, gallium trichloride, calcium chloride.
6, right requires the production method of described a kind of diphenyl phosphorus chloride that arbitrary right requires among the 1-5, it is characterized in that:
(1), in anhydrous, anaerobic and have under the protection of nitrogen gas condition, according to the mass parts meter, 1-8 part organic solvent, 0.8-1.5 part sodium or potassium or magnesium are mixed the adding Scattered Kettle, be heated to 90-130 ℃, with 300-2500 rev/min stirring velocity dispersed with stirring sodium or potassium or magnesium 2～40 minutes, make sodium or potassium or magnesium be dispersed into the following particulate of 120 μ m, the halogenide that adds 0.02～0.1 part of benzene carries out the first time and causes;
When (2), treating 2-3 ℃ of temperature rising after causing for the first time, material after will disperseing is cooled to 40-70 ℃ at once, the halogenide that adds the benzene of same quantity again carries out after secondary causes, be cooled to 10-30 ℃ rapidly, after dripping halid 10～15% abundant initiations of total amount 1-4 part benzene, halogenide and 1～3 part of phosphorus trichloride that will remain benzene again mix adding simultaneously;
(3), add after, temperature adds 0.03-0.1 part catalyzer of measuring 20-80 ℃ of reaction 1-2 hour again, is warming up between 80-120 ℃ reaction 0.5-2.5 hour;
(4), under pressure 0.1-0.3Mpa, by press filtration bucket filtered while hot, remove the salt and the catalyzer of generation;
(5), with the material after the press filtration put into rectifying still stir, under normal pressure distilling off solvent, rectifying goes out the finished product diphenyl phosphorus chloride under the 0.005-0.009Mpa negative pressure, checks, packing.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2011083009A1 (en) | 2009-12-16 | 2011-07-14 | Basf Se | Flame retardant |
| WO2013017417A1 (en) | 2011-07-29 | 2013-02-07 | Basf Se | Polymer flame retardant |
| CN105330693A (en) * | 2015-12-08 | 2016-02-17 | 山东潍坊润丰化工股份有限公司 | Alkyl phosphorus dihalide preparing method |
| CN109575072A (en) * | 2019-01-14 | 2019-04-05 | 绍兴上虞易瑞化工有限公司 | A kind of novel synthesis of diphenyl phosphine chloride |
-
2008
- 2008-05-15 CN CNA2008100161686A patent/CN101481390A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2011083009A1 (en) | 2009-12-16 | 2011-07-14 | Basf Se | Flame retardant |
| US9234137B2 (en) | 2009-12-16 | 2016-01-12 | Basf Se | Flame retardant |
| WO2013017417A1 (en) | 2011-07-29 | 2013-02-07 | Basf Se | Polymer flame retardant |
| CN105330693A (en) * | 2015-12-08 | 2016-02-17 | 山东潍坊润丰化工股份有限公司 | Alkyl phosphorus dihalide preparing method |
| CN105330693B (en) * | 2015-12-08 | 2017-11-07 | 山东潍坊润丰化工股份有限公司 | A kind of preparation method of alkyl dihalide phosphorus |
| CN109575072A (en) * | 2019-01-14 | 2019-04-05 | 绍兴上虞易瑞化工有限公司 | A kind of novel synthesis of diphenyl phosphine chloride |
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