Preparation method of fatty alcohol polyoxyethylene phosphate ester potassium salt

A technology of alcohol phosphate polyoxyethylene ester potassium salt and fatty alcohol, which is applied in the field of synthesis of anionic surfactants in organic chemistry, can solve the problems of inconvenient use, low solid content of potassium salt, increased transportation cost, etc., and achieves convenient storage. and use, good economic benefits, and the effect of reducing transportation costs

Inactive Publication Date: 2013-10-30
NINGBO LIANKAI CHEM
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Problems solved by technology

Due to the low solid content and paste-like characteristics of fatty alcohol polyoxyethylene ether phosphate potassiu

Method used

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  • Preparation method of fatty alcohol polyoxyethylene phosphate ester potassium salt
  • Preparation method of fatty alcohol polyoxyethylene phosphate ester potassium salt
  • Preparation method of fatty alcohol polyoxyethylene phosphate ester potassium salt

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preparation example Construction

[0020] A preparation method of fatty alcohol polyoxyethylene phosphate potassium salt, comprising the following steps: (1) using fatty alcohol as a raw material to carry out esterification reaction with phosphorus pentoxide; (2) adding deionized water for hydrolysis to obtain A mixture of fatty alcohol phosphate esters based on phosphoric acid monoesters and phosphoric diesters is directly condensed with ethylene oxide under the condition of no catalyst; (3) neutralizing the pH to 6 with 60% potassium hydroxide aqueous solution ~8, the potassium salt of fatty alcohol polyoxyethylene ether phosphate with a solid content of more than 90% was prepared; the main synthetic route is as follows:

[0021] Esterification reaction:

[0022]

[0023] Condensation reaction:

[0024]

[0025] Neutralization reaction:

[0026]

[0027] R is C in the reaction equation 12～１４ or C 18～１６ A saturated branched alkyl group, where m=a+b.

[0028] Preferably, the molar ratio of the fa...

Embodiment 1C12

[0041] Example 1C 12～１４ Preparation of Potassium Salt of Polyoxyethylene Ether Alcohol Phosphate

[0042] Esterification reaction: In a 500mL four-necked flask, add 0.75mol (144.8g) C 12～１４ Alcohol, add 36.0g of phosphorus pentoxide in five batches, react at a temperature of 50-55°C for 8.0 hours, then add 0.9g of deionized water, hydrolyze at a temperature of 75-80°C for 1.0 hour, cool to obtain the esterification product C 12～１４ alcohol phosphate.

[0043] Condensation reaction and neutralization reaction: Add the above-mentioned esterification product into a 2.5L pressure reactor, and connect the ethylene oxide metering tank to the pressure reactor. The air was replaced with nitrogen for 3 times, and when the temperature of the kettle rose to 125-130° C., 198.0 g of ethylene oxide was introduced into the reaction mixture for 2.5 hours, and the reaction was continued for 0.5 hours. After the reaction is complete, cool down and release the pressure. The obtained intermedi...

Embodiment 2C18

[0044] Example 2C 18～１６ Preparation of Potassium Salt of Polyoxyethylene Ether Alcohol Phosphate

[0045] Esterification reaction: In a 500mL four-necked flask, add 1.0mol (263.0g) C 18～１6 Alcohol, add 72.0g of phosphorus pentoxide in two batches, react at 90-95°C for 3.0 hours, then add 6.7g of deionized water, hydrolyze at 65-70°C for 2.0 hours, cool to obtain the esterification product C 18～１６ alcohol phosphate.

[0046] Condensation reaction and neutralization reaction: Add the above-mentioned esterification product into a 2.5L pressure reactor, and connect the ethylene oxide metering tank to the pressure reactor. The air was replaced with nitrogen for 3 times, and when the temperature of the kettle rose to 50-55° C., 396.0 g of ethylene oxide was introduced into the mixture for 5.5 hours, and the reaction was continued for 0.5 hours. After the reaction is complete, cool down and release the pressure. The obtained intermediate product was transferred to a 1000mL four-n...

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Abstract

The invention discloses a preparation method of fatty alcohol polyoxyethylene phosphate ester potassium salt, which comprises the following steps: (1) performing esterification reaction on fatty alcohol used as a raw material and phosphorus pentoxide; (2) adding deionized water, hydrolyzing to obtain a fatty alcohol phosphate ester mixture mainly containing phosphate monoester and phosphate diester, and directly performing condensation reaction with epoxyethane in the absence of a catalyst; and (3) neutralizing with a 60% potassium hydroxide water solution until the pH value is 6-8, thus preparing to obtain fatty alcohol polyoxyethylene ether phosphate ester potassium salt of which the solid content is 90% or above. In the above mode, in comparison with the fatty alcohol polyoxyethylene ether phosphate ester potassium salt, the fatty alcohol polyoxyethylene phosphate ester potassium salt synthesized by the invention has the advantages of high solid content and liquid flow, reduces the transportation cost, and facilitates storage and use by users, thus having better economic benefits.

Description

technical field [0001] The invention relates to a preparation method of fatty alcohol polyoxyethylene phosphate potassium salt, which belongs to the technical field of synthesis of anionic surfactants in organic chemistry. Background technique [0002] In recent years, foreign phosphate ester surfactants have developed rapidly, and the main production companies include Japan Matsumoto Oil Company, Kao Stone Alkaline Company, German BASF Company, and American Monsanto Company. The average annual growth rate in the United States over the past ten years was 5.8%. However, the research and development of such surfactants in my country started relatively late, and there is a big gap compared with foreign countries in terms of product variety, quantity and quality, but it has developed rapidly in recent years, with an annual rate of 8% to 10%. Increasingly, the application of such surfactants has attracted more and more attention. Fatty alcohol polyoxyethylene ether phosphate pot...

Claims

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Application Information

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IPC IPC(8): C07F9/11
Inventor 曾红舟陈雪董威
Owner NINGBO LIANKAI CHEM
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