Preparation method of phosphomonoester

A phosphoric acid monoester and temperature control technology, which is applied in chemical instruments and methods, phosphorus organic compounds, compounds of group 5/15 elements of the periodic table, etc., can solve the problem of low content of phosphoric acid monoester and complex preparation process of phosphoric acid monoester, etc. problem, to achieve the effect of good technical effect

Inactive Publication Date: 2016-06-29
SHANGHAI DUOLUN CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved by the present invention is the complex preparation process of phosphoric acid monoester and the low content of phosphoric acid monoester in the prior art. It provides a new preparation method of phosphoric acid monoester, which has the advantages of simple process, simple phosphoric acid monoester Advantages of high ester content

Method used

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  • Preparation method of phosphomonoester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0040] Preparation of Tetradecyl Phosphate Monoester: 200.00 g of tetradecyl mixed alcohol (mass ratio of dodecyl alcohol to tetradecyl alcohol is 70:30), 0.42 g of hypophosphorous acid and pure water are added to a round bottom flask 14.80g, open and stir and heat up; When temperature rises to 70 ℃, add catalyzer (the catalyzer is SnCl 4 , MnO 2 and CuSO 4 Mixture with a mass ratio of 0.9:1:0.3) 0.88g, and then 74.28g of phosphorus pentoxide was added in sections, the temperature was controlled at 75±5°C, and the feeding time was controlled at 1.5 hours; after the addition, it was kept at 85°C for 4.5 hours , and then add 5.18g of pure water, control the temperature to 85°C, keep the temperature at this temperature for 2 hours, then cool down to 75°C and filter to obtain the phosphoric acid ester product. Analysis by double indicator titration method: monoester: 92.3%, diester: 5.0%, phosphoric acid 2.7%.

Embodiment 2

[0048] The difference from Example 1 is that the catalyst is SnCl 4 .

[0049] Add 200.00g of tetradecyl alcohol (mass ratio of dodecanol to tetradecyl alcohol is 70:30), 0.42g of hypophosphorous acid and 14.80g of pure water in the round bottom flask, start stirring and heat up; when the temperature rises to Add 40.88g of SnCl to the round bottom flask at 70°C, then add 74.28g of phosphorus pentoxide in stages, control the temperature at 75±5°C, and control the feeding time for 1.5 hours; Then add 5.18g of pure water, control the temperature at 85±2°C, keep at this temperature for 2 hours, then cool down to 75°C and filter to obtain the phosphate ester product. Analysis by double indicator titration: monoester: 83.9%, diester: 12.6%, phosphoric acid 3.5%.

Embodiment 3

[0051] The difference from Example 1 is that the catalyst is MnO 2 .

[0052] Add 200.00g of tetradecyl alcohol (mass ratio of dodecanol to tetradecyl alcohol is 70:30), 0.42g of hypophosphorous acid and 14.80g of pure water in the round bottom flask, start stirring and heat up; when the temperature rises to Add MnO to the round bottom flask at 70°C 2 0.88g, then 74.28g of phosphorus pentoxide was added in sections, the temperature was controlled at 75±5°C, and the feeding time was controlled at 1.5 hours; 85±2°C, and kept at this temperature for 2 hours, then cooled to 75°C and filtered to obtain the phosphate ester product. Analysis by double indicator titration method: monoester: 84.3%, diester: 11.4%, phosphoric acid 4.3%.

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Abstract

The invention relates to a preparation method of phosphomonoester, and mainly solves problems of complex phosphomonoester preparation technique and lower phosphomonoester content in the prior art. The method comprises the following steps: (1) adding hydroxyl compounds and water into a reactor, and heating to 55-80 DEG C; (2) adding a catalyst X into the reactor, slowly adding P2O5, and controlling the material temperature in the reactor at 55-95 DEG C and the material addition time at 1-2 hours; (3) keeping the temperature at 75-95 DEG C for 3-6 hours to obtain a material A; and (4) adding water into the material A, controlling the temperature at 70-90 DEG C, and keeping the temperature for 2-3 hours to obtain the phosphomonoester, wherein the general formula of the hydroxyl compounds is RO(EO)m(PO)nH, and the catalyst X is selected from at least one of SnCl4, MnO2 and CuSO4 and can be used for preparing the phosphomonoester.

Description

technical field [0001] The invention relates to a preparation method of phosphoric acid monoester. Background technique [0002] Phosphate monoester refers to a product with a monoester content of 80.0% or more. Phosphate monoesters have a biofilm-like structure, and their antistatic properties, foaming properties, water solubility, and emulsification are superior to phosphate diesters, and they are less irritating to the skin than anionic surfaces such as alkyl sulfonates and alkyl sulfates. Active agent, very suitable for skin cleansing, cosmetic emulsification, etc. Phosphate monoester has stronger dispersing ability than phosphoric diester, and has higher foaming property and moderate foam stability. It can be used as collector in flotation deinking process to flotation and separate ink particles. It is an environmentally friendly surfactant with excellent performance in washing and flotation deinking processes. Therefore, increasing the content of phosphate monoester...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/11C07F9/09
CPCC07F9/11C07F9/091C07F9/094
Inventor 钟敏舒建生陈静徐兴建李翔杨健
Owner SHANGHAI DUOLUN CHEM
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