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Preparation method of phosphate monoester

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. problem, to achieve the effect of good technical effect

Active Publication Date: 2018-10-16
SHANGHAI DUOLUN CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

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

Method used

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  • Preparation method of phosphate monoester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] 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, start stirring and heat up; when the temperature rises to 70°C, start to add 74.28g of phosphorus pentoxide in stages, control the temperature at 75±5°C, and control the feeding time for 1.5 hours; after adding, keep warm at 85°C for 4.5 hours , then add pure water 5.18g and catalyst (the catalyst is SnCl 4 , MnO 2 and CuSO 4 Mass ratio is 0.9:1:0.3 mixture) 0.88g, control temperature is 85 ℃, keep at this temperature for 2 hours, cool down to 75 ℃ and filter to obtain phosphate ester product. Analysis by double indicator titration method: monoester: 90.6%, diester: 6.9%, phosphoric acid 2.5%.

Embodiment 2

[0047] The difference from Example 1 is that the catalyst is SnCl 4 .

[0048] Add 200.00 g of tetradecyl alcohol (the mass ratio of dodecyl alcohol to tetradecyl alcohol is 70:30), 0.42 g of hypophosphorous acid and 14.80 g of pure water in a round bottom flask, start stirring and heat up; when the temperature rises to 70 At ℃, 74.28g of phosphorus pentoxide was added in stages, the temperature was controlled at 75±5℃, and the feeding time was controlled at 1.5 hours; after the addition, it was kept at 85℃ for 4.5 hours, and then 5.18g of pure water and SnCl 4 0.88g, the temperature is controlled at 85±2°C, 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: monoester 79.6%, diester: 16.9%, phosphoric acid 3.5%.

Embodiment 3

[0050] The difference from Example 1 is that the catalyst is MnO 2 .

[0051] Add 200.00 g of tetradecyl alcohol (the mass ratio of dodecyl alcohol to tetradecyl alcohol is 70:30), 0.42 g of hypophosphorous acid and 14.80 g of pure water in a round bottom flask, start stirring and heat up; when the temperature rises to 70 At ℃, 74.28g of phosphorus pentoxide was added in stages, the temperature was controlled at 75±5℃, and the feeding time was controlled at 1.5 hours; after the addition, it was kept at 85℃ for 4.5 hours, and then 5.18g of pure water and 20.88g of MnO were added. The temperature is controlled at 85±2°C, 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: 80.6%, diester: 13.9%, phosphoric acid 5.5%.

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Abstract

The invention relates to a preparation method of phosphomonoester and mainly solves problems of complex preparation technology of phosphomonoester and low content of phosphomonoester existing in the prior art. The preparation method of the invention comprises the following steps: (1) adding a hydroxy compound and water into a reactor, and heating to 55-80 DEG C; (2) slowly pouring P2O5, controlling temperature of materials in the reactor to 55-95 DEG C, and controlling pouring time within 1-2 h; (3) carrying out thermal insulation at 75-95 DEG C for 3-6 h so as to obtain a material A; and (4) adding water and a catalyst X into the material A, controlling temperature to 70-90 DEG C, and carrying out thermal insulation at the temperature for 2-3 h so as to obtain phosphomonoester. The hydroxy compound accords with the following general formula: RO(EO)m(PO)nH. The catalyst X is at least one compound selected from SnCl4, MnO2 and CuSO4. The preparation method can be used in preparation of phosphomonoester.

Description

technical field [0001] The present invention relates to the preparation method of phosphoric 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 mono...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/11C07F9/09
CPCC07F9/091C07F9/11
Inventor 钟敏陈静徐兴建李翔
Owner SHANGHAI DUOLUN CHEM
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