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. problem, to achieve the effect of good technical effect

Active Publication Date: 2016-04-27
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 mono

Method used

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  • Preparation method of phosphomonoester

Examples

Experimental program
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Effect test

Embodiment 1

[0039] Preparation of dodecyl tetradecyl phosphate monoester: Add 200.00 g of dodecyl alcohol (the mass ratio of dodecanol to tetradecyl alcohol is 70:30), 0.42 g of hypophosphorous acid and pure water in a round bottom flask 14.80g, turn on the stirring and increase the temperature; when the temperature rises 70℃, start to add 74.28g of phosphorus pentoxide, the temperature is controlled at 75±5℃, the feeding time is controlled for 1.5 hours; after the addition, keep the temperature at 85℃ for 4.5 hours , And then add 5.18g of pure water and catalyst (the catalyst is SnCl 4 , MnO 2 And CuSO 4 A mixture with a mass ratio of 0.9:1:0.3) 0.88g, the temperature is controlled to 85°C, and the temperature is kept at this temperature for 2 hours, and then the temperature is lowered to 75°C and filtered to obtain a phosphate product. Analyzed by double indicator titration method, we found that: 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] In the round bottom flask, add 200.00 g of dodecatetraol (the mass ratio of dodecanol to tetradecanol is 70:30), 0.42 g of hypophosphorous acid and 14.80 g of pure water, turn on the stirring and increase the temperature; when the temperature rises by 70 Start adding 74.28g of phosphorus pentoxide in stages at ℃, the temperature is controlled at 75±5℃, and the feeding time is controlled to 1.5 hours; after the addition, keep it at 85℃ for 4.5 hours, and then add 5.18g of pure water and SnCl 4 0.88g, control the temperature to 85±2℃, keep it at this temperature for 2 hours and then cool to 75℃ to filter to obtain the phosphate product. Analyzed by double indicator titration method: 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] In the round bottom flask, add 200.00 g of dodecatetraol (the mass ratio of dodecanol to tetradecanol is 70:30), 0.42 g of hypophosphorous acid and 14.80 g of pure water, turn on the stirring and increase the temperature; when the temperature rises by 70 Begin to add 74.28g of phosphorus pentoxide in stages at ℃, control the temperature at 75±5℃, and control the feeding time to 1.5 hours; after the addition, keep it at 85℃ for 4.5 hours, then add 5.18g of pure water and 20.88g of MnO. Control the temperature to 85±2°C, keep it at this temperature for 2 hours and then lower the temperature to 75°C to filter to obtain the phosphate product. Analyzed 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 invention relates to a preparation method of phosphoric acid monoester. Background technique [0002] Phosphoric acid monoester refers to a product with a monoester content of 80.0% or more. Phosphoric acid monoester has a biofilm-like structure, and its antistatic, foaming, water-soluble and emulsifying properties are better than phosphate diesters, and its skin irritation is less than that of anionic surfaces such as alkyl sulfonates and alkyl sulfates Active agent, very suitable for skin cleansing and cosmetic emulsification. Compared with the phosphate diester, the phosphate monoester has stronger dispersing ability, higher foamability and moderate foam stability. It can be used as a collector in the flotation deinking process to separate ink particles. It is a kind of simultaneous application It is an environmentally friendly surfactant with excellent performance for washing and flotation deinking processes. Therefore, increasing the content of ...

Claims

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Application Information

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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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