A kind of synthetic method of highly selective alkyl phosphate monoester

A technique for the synthesis of alkyl phosphate monoesters, which is applied in the fields of chemical instruments and methods, compounds of Group 5/15 elements of the periodic table, organic chemistry, etc., and can solve the problems of increased production costs and energy consumption, and the ease of phosphorus oxychloride Problems such as volatilization and post-processing difficulties, to achieve the effect of low cost, convenient storage and transportation, and suitable for large-scale production

Active Publication Date: 2020-05-05
CHINA RES INST OF DAILY CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Patent CN 104804038 A uses phosphorus oxychloride as a phosphorylation reagent to synthesize alkyl phosphate, which has high reaction activity and fast reaction speed, but the raw material phosphorus oxychloride has a low boiling point and is easy to volatilize, and the generated by-product HCl will corrode equipment, and HCl is easy to react with ROH to form RCl by-product, which is not conducive to the formation of monoester
Patent CN 103012469 A uses phosphoric acid as a phosphorylation reagent, and adds a water-carrying agent to synthesize alkyl phosphates. Because organic solvents such as toluene and dichloroethane are added during the synthesis process of this process, the post-treatment of the product is difficult, increasing production costs and energy consumption

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Weigh 55.9g of natural lauryl alcohol into the reaction flask, add 0.43g of calcium sulfate, set the reaction temperature at 90°C, and when the temperature reaches 90°C, weigh 34.6g of 85% phosphoric acid, slowly add it into the reaction flask, and simultaneously Control the appropriate stirring speed and vacuum degree, wherein the stirring speed is 200r / min, and the vacuum degree is -0.08MPa. After the phosphoric acid is added dropwise, react for 7h. Sampling analysis. Wherein the dodecyl phosphate monoester content is 76wt%, the monoester selectivity is 100%, and the monoester content reaches 91wt% after purification.

Embodiment 2

[0026] Weigh 145.5g of stearyl alcohol into a reaction bottle, add 0.1g of barium sulfate and 0.1g of sodium carbonate, set the reaction temperature to 70°C, and when the temperature reaches 70°C, weigh 57.7g of 85% phosphoric acid, and slowly add it to the reaction In the bottle, control the appropriate stirring speed and vacuum at the same time, wherein the stirring speed is 400r / min, and the reading of the vacuum gauge is -0.02Mpa. After the phosphoric acid is added dropwise, react for 1h. After the reaction, take a sample for analysis. Among them, the content of octadecyl phosphate monoester is 71%, the selectivity of monoester is 100%, and the content of monoester after purification reaches 87%.

Embodiment 3

[0028] Weigh 68.6g of behenyl alcohol into the reaction flask, add 0.71g of cesium carbonate, set the reaction temperature to 120°C, and when the temperature reaches 120°C, weigh 23.1g of 85% phosphoric acid, slowly add it into the reaction flask, and simultaneously Control the appropriate stirring speed and vacuum degree, wherein the stirring speed is 500r / min, and the reading of the vacuum gauge is -0.05Mpa. After the phosphoric acid is added dropwise, react for 15h. After the reaction, take a sample for analysis. Wherein the alkyl phosphate monoester content is 74%, the monoester selectivity is 100%, and the monoester content in the purified sample is 93%.

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Abstract

The invention discloses a synthetic method of high-selectivity alkyl phosphate monoester. The synthetic method is characterized in that fatty alcohol or aliphatic ether are taken as raw materials, phosphoric acid is taken as a phosphorylation agent, a catalyst is added, and a reduced pressure reaction is performed to obtain the alkyl phosphate monoester by one step. The product synthesized by the synthetic method has the advantages of high monoester selectivity, high monoester content, high added value, and can be applied to high-end skin care products such as cosmetics; meanwhile the synthetic method is simple, is mild in reaction conditions, is high in reaction speed, and is environment-friendly.

Description

technical field [0001] The invention relates to a method for synthesizing alkyl phosphates, in particular to a method for synthesizing highly selective alkyl phosphate monoesters. [0002] technical background [0003] In recent years, phosphate ester surfactants have been widely used because of their good properties such as low toxicity, non-irritation and remarkable biodegradability. As one of the phosphoric acid ester surfactants, alkyl phosphate has high solubility, thermal stability, hard water resistance, acid and alkali resistance, inorganic salt resistance, high temperature resistance and antistatic performance are superior to general surfactants, so Widely used in chemical fiber oils, emulsifiers, antistatic agents, lubricants, etc. In particular, its chemical structure is similar to that of biofilm, and its biodegradability is excellent, so it is widely used in daily chemical products. Alkyl phosphates include monoesters, diesters and triesters. Alkyl phosphate m...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/40
CPCC07F9/4003
Inventor 赵永红师亚宁张广良李国晋
Owner CHINA RES INST OF DAILY CHEM IND
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