CN106518913A - Preparation method for producing dialkyl chlorophosphate reagent from polyethylene glycol - Google Patents
Preparation method for producing dialkyl chlorophosphate reagent from polyethylene glycol Download PDFInfo
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- CN106518913A CN106518913A CN201510587646.9A CN201510587646A CN106518913A CN 106518913 A CN106518913 A CN 106518913A CN 201510587646 A CN201510587646 A CN 201510587646A CN 106518913 A CN106518913 A CN 106518913A
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- Prior art keywords
- polyethylene glycol
- chlorine
- reaction
- dihydrocarbon
- preparation
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Abstract
The present invention provides a preparation method for producing a dialkyl chlorophosphate reagent from polyethylene glycol. The preparation method comprises: adding a preset amount of polyethylene glycol to a reaction bottle, replacing the air in the reaction bottle with an inert gas, cooling to a preset temperature, adding trisodium phosphate to the reaction bottle in a dropwise manner, diluting with a preset amount of an anhydrous solvent when the reaction is completed, filtering the product, and concentrating the product to obtain the dialkyl chlorophosphoric acid. According to the present invention, the reaction can be completely performed without any solvents in the dialkyl chlorophosphate preparation process, the reaction time is short, and the liquid waste cannot be generated; and the obtained product has the sufficient purity under the normal circumstance, the general organic synthesis requirement can be met, and the further distillation can be performed if the purity does not meet the requirement.
Description
Technical field
A kind of a kind of the present invention relates to preparation method, more particularly to Polyethylene Glycol making chlorine dihydrocarbon examination
The preparation method of agent.
Background technology
Chlorine dihydrocarbon is the important examination for synthesizing organic phosphorus compound, particularly phosphoric acid mixing ester compounds
Agent.Chlorine dihydrocarbon is prepared with gas chlorine source such as chlorine, phosgene reaction method by phosphite ester,
Need to remove the gas and acid dissolved in product with dry air and ceruse after reaction.Produce pollution environment
Solid waste.In prior art, using nitrogen-chloro-succimide or TCCA (Trichloroisocyanuric acid) as chlorine
Source.
During the present invention is realized, inventor has found that prior art at least has problems with：
The preparation method of prior art makees solvent using acetonitrile or toluene, produces unnecessary liquid debris；
Course of reaction needs heating, and the response time is long；The preparation method be only applicable in alkyl carbon atoms number compared with
Few product, increases with carbon atom number in product alkyl, and the yield of product declines, and reaction is incomplete, produces
Thing is difficult to purification.
The content of the invention
The purpose of the present invention is that to solve the above problems and provides a kind of Polyethylene Glycol and make chlorine di(2-ethylhexyl)phosphate
The preparation method of hydrocarbyl carbonate reagent.
The present invention is achieved through the following technical solutions above-mentioned purpose：
The present invention is comprised the following steps：
Step a, in reaction bulb add predetermined amount Polyethylene Glycol；
Step b, air in the reaction bulb is replaced into into noble gases, and is cooled to preset temperature；
Step c, to Deca tertiary sodium phosphate in the reaction bulb；
Step d, at the end of the reaction, diluted with predetermined amount anhydrous solvent, and product filtered；
Step e, concentration is carried out to the product, obtain chlorine di-phosphate ester.
Currently preferred, according to step a, the reaction bulb is dry.
Currently preferred, according to step c, in the reaction bulb, Deca tertiary sodium phosphate includes：
The Deca tertiary sodium phosphate while stirring in the reaction bulb, after completion of dropping, continues stirring, until
Reaction terminates.
It is currently preferred, concentration is carried out to the product, after obtaining chlorine di-phosphate ester, the side
Method also includes：
The chlorine di-phosphate ester product is distilled.
Currently preferred, the molal quantity of the predetermined amount Polyethylene Glycol is higher than the tertiary sodium phosphate.
Currently preferred, composition proportion shared by the Polyethylene Glycol is 50 70%；The tertiary sodium phosphate institute
Composition proportion is accounted for for 10 30%；Composition proportion shared by the anhydrous solvent is 30 40%.
Currently preferred, composition proportion shared by the Polyethylene Glycol is 60%；The tertiary sodium phosphate it is shared into
Part proportion is 20%；Composition proportion shared by the anhydrous solvent is 20%.
The beneficial effects of the present invention is：
The present invention does not use any solvent in the preparation process by chlorine phosphate ester, and reaction can be made to carry out completely,
Response time is short, and will not product fluid garbage.Generally products therefrom has sufficiently high purity,
Meet the needs of general organic synthesiss, it is such as dissatisfied to purity further to distill.
Description of the drawings
Fig. 1 is the preparation method that a kind of Polyethylene Glycol of the present invention makes chlorine dihydrocarbon reagent
Flow chart.
Specific embodiment
The invention will be further described below：
The present invention is comprised the following steps：
As shown in figure 1, the present invention is comprised the following steps：
Step a, in reaction bulb add predetermined amount Polyethylene Glycol；
Step b, air in the reaction bulb is replaced into into noble gases, and is cooled to preset temperature；
Step c, to Deca tertiary sodium phosphate in the reaction bulb；
Step d, at the end of the reaction, diluted with predetermined amount anhydrous solvent, and product filtered；
Step e, concentration is carried out to the product, obtain chlorine di-phosphate ester.
Currently preferred, according to step a, the reaction bulb is dry.
Currently preferred, according to step c, in the reaction bulb, Deca tertiary sodium phosphate includes：
The Deca tertiary sodium phosphate while stirring in the reaction bulb, after completion of dropping, continues stirring, until
Reaction terminates.
It is currently preferred, concentration is carried out to the product, after obtaining chlorine di-phosphate ester, the side
Method also includes：
The chlorine di-phosphate ester product is distilled.
Currently preferred, the molal quantity of the predetermined amount Polyethylene Glycol is higher than the tertiary sodium phosphate.
Currently preferred, composition proportion shared by the Polyethylene Glycol is 50 70%；The tertiary sodium phosphate institute
Composition proportion is accounted for for 10 30%；Composition proportion shared by the anhydrous solvent is 30 40%.
Embodiment one：Currently preferred, composition proportion shared by the Polyethylene Glycol is 50%；The phosphoric acid
Composition proportion shared by trisodium is 30%；Composition proportion shared by the anhydrous solvent is 20%.
Embodiment two：Currently preferred, composition proportion shared by the Polyethylene Glycol is 55%；The phosphoric acid
Composition proportion shared by trisodium is 25%；Composition proportion shared by the anhydrous solvent is 20%.
Embodiment three：Currently preferred, composition proportion shared by the Polyethylene Glycol is 60%；The phosphoric acid
Composition proportion shared by trisodium is 20%；Composition proportion shared by the anhydrous solvent is 20%.
Example IV：Currently preferred, composition proportion shared by the Polyethylene Glycol is 70%；The phosphoric acid
Composition proportion shared by trisodium is 10%；Composition proportion shared by the anhydrous solvent is 20%.
Embodiment five：Currently preferred, composition proportion shared by the Polyethylene Glycol is 65%；The phosphoric acid
Composition proportion shared by trisodium is 15%；Composition proportion shared by the anhydrous solvent is 20%.
Above-described embodiment is presently preferred embodiments of the present invention, is not the restriction to technical solution of the present invention；
As long as without the technical scheme that creative work can be realized on the basis of above-described embodiment, all should regard
For falling in the rights protection scope of patent of the present invention.
Claims (7)
1. a kind of Polyethylene Glycol makes the preparation method of chlorine dihydrocarbon reagent, it is characterised in that：Including
Following steps：
Step a, in reaction bulb add predetermined amount Polyethylene Glycol；
Step b, air in the reaction bulb is replaced into into noble gases, and is cooled to preset temperature；
Step c, to Deca tertiary sodium phosphate in the reaction bulb；
Step d, at the end of the reaction, diluted with predetermined amount anhydrous solvent, and product filtered；
Step e, concentration is carried out to the product, obtain chlorine oleate.
2. a kind of Polyethylene Glycol according to claim 1 makes the preparation side of chlorine dihydrocarbon reagent
Method, it is characterised in that：According to step a, the reaction bulb is dry.
3. a kind of Polyethylene Glycol according to claim 1 makes the preparation side of chlorine dihydrocarbon reagent
Method, it is characterised in that：According to step c, in the reaction bulb, Deca tertiary sodium phosphate includes：
The Deca tertiary sodium phosphate while stirring in the reaction bulb, after completion of dropping, continues stirring, until
Reaction terminates.
4. a kind of Polyethylene Glycol according to claim 1 makes the preparation side of chlorine dihydrocarbon reagent
Method, it is characterised in that：Concentration is carried out to the product, after obtaining chlorine di-phosphate ester, methods described
Also include：
The chlorine di-phosphate ester product is distilled.
5. a kind of Polyethylene Glycol according to claim 1 makes the preparation side of chlorine dihydrocarbon reagent
Method, it is characterised in that：The molal quantity of the predetermined amount Polyethylene Glycol is higher than the tertiary sodium phosphate.
6. a kind of Polyethylene Glycol according to claim 1 makes the preparation side of chlorine dihydrocarbon reagent
Method, it is characterised in that：Composition proportion shared by the Polyethylene Glycol is 50 70%；The tertiary sodium phosphate it is shared into
Part proportion is 10 30%；Composition proportion shared by the anhydrous solvent is 30 40%.
7. a kind of Polyethylene Glycol according to claim 6 makes the preparation side of chlorine dihydrocarbon reagent
Method, it is characterised in that：Composition proportion shared by the Polyethylene Glycol is 60%；Composition shared by the tertiary sodium phosphate
Proportion is 20%；Composition proportion shared by the anhydrous solvent is 20%.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510587646.9A CN106518913A (en) | 2015-09-15 | 2015-09-15 | Preparation method for producing dialkyl chlorophosphate reagent from polyethylene glycol |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510587646.9A CN106518913A (en) | 2015-09-15 | 2015-09-15 | Preparation method for producing dialkyl chlorophosphate reagent from polyethylene glycol |
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|---|---|
| CN106518913A true CN106518913A (en) | 2017-03-22 |
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| CN201510587646.9A Pending CN106518913A (en) | 2015-09-15 | 2015-09-15 | Preparation method for producing dialkyl chlorophosphate reagent from polyethylene glycol |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0739895A1 (en) * | 1995-04-26 | 1996-10-30 | Nippon Chemical Industrial Company Limited | Method of preparing diarylchlorophosphate |
| EP1327635A1 (en) * | 2002-01-06 | 2003-07-16 | Bromine Compounds Ltd. | Preparation of phenylphosphate esters of 4,4'-biphenol |
| CN103360309A (en) * | 2013-08-02 | 2013-10-23 | 重庆邮电大学 | Synthetic method for piperaquine phosphate intermediate 7-chloro-4-(1-piperazino)quinoline |
| CN103554175A (en) * | 2013-10-15 | 2014-02-05 | 西北农林科技大学 | Reagent preparation method |
-
2015
- 2015-09-15 CN CN201510587646.9A patent/CN106518913A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0739895A1 (en) * | 1995-04-26 | 1996-10-30 | Nippon Chemical Industrial Company Limited | Method of preparing diarylchlorophosphate |
| EP1327635A1 (en) * | 2002-01-06 | 2003-07-16 | Bromine Compounds Ltd. | Preparation of phenylphosphate esters of 4,4'-biphenol |
| CN103360309A (en) * | 2013-08-02 | 2013-10-23 | 重庆邮电大学 | Synthetic method for piperaquine phosphate intermediate 7-chloro-4-(1-piperazino)quinoline |
| CN103554175A (en) * | 2013-10-15 | 2014-02-05 | 西北农林科技大学 | Reagent preparation method |
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Application publication date: 20170322 |
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