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Method for synthesizing allyl fatty alcohol-polyoxyethylene ether or allyl alkylphenol ethoxylate

A technology of allyl alkylphenol polyoxyethylene ether and alkylphenol polyoxyethylene ether, which can be applied in ether preparation, ester reaction preparation ether, organic chemistry, etc., can solve the problem of difficult separation of phase transfer catalyst, increase reaction cost, Environmental problems and other problems, to achieve the effect of reducing solvent removal units, low cost and mild process conditions

Inactive Publication Date: 2012-07-18
CHINA RES INST OF DAILY CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In order to improve the reactivity of the above two methods, water, a phase transfer catalyst and an organic solvent were added to the reaction system, and allyl ether was synthesized in an aqueous hydroxide solution. The water in the system affected the reaction balance and the conversion rate was low. ; Need to add phase transfer catalyst in the reaction process, phase transfer catalyst is difficult to separate from the product; adopted organic solvent, although the reaction conversion rate has been improved, but the use of organic solvent will inevitably bring environmental problems, also need to increase the solvent in the project Removal and other equipment units increase the cost of the reaction

Method used

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  • Method for synthesizing allyl fatty alcohol-polyoxyethylene ether or allyl alkylphenol ethoxylate
  • Method for synthesizing allyl fatty alcohol-polyoxyethylene ether or allyl alkylphenol ethoxylate
  • Method for synthesizing allyl fatty alcohol-polyoxyethylene ether or allyl alkylphenol ethoxylate

Examples

Experimental program
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Effect test

Embodiment 1

[0032] The first step reaction: put 200 grams of fatty alcohol polyoxyethylene ether AEO-7 (molecular weight 501) and 22 grams of solid sodium hydroxide (particle size 1mm) into a 500ml stainless steel autoclave, the molar ratio is 1: 1, and feed simultaneously Stir the materials, close the reactor after feeding, replace the air in the reactor with nitrogen, start the vacuum system after the replacement, keep the vacuum of the reactor at 0.085MPa, keep stirring the materials during this process, and raise the temperature of the reactor to 200°C , after reacting for 5 hours, stop heating, cool to room temperature, and close the vacuum system;

[0033] The second step reaction: add 39 grams of allyl chloride dropwise to the above reaction kettle, the molar ratio of fatty alcohol polyoxyethylene ether or alkylphenol polyoxyethylene ether to allyl chloride is 1:1, during the dropwise addition process Stir the material continuously, after the dropwise addition, the reaction exother...

Embodiment 2

[0036] The first step reaction: 200 grams of alkylphenol polyoxyethylene ether NP-8 (molecular weight 520) and 12 grams of solid lithium hydroxide (particle size 0.1mm) were dropped into a 500ml stainless steel autoclave, and the molar ratio was 1: 1.3. Stir the material at the same time as feeding, seal the reactor after feeding, replace the air in the reactor with nitrogen, start the vacuum system after the replacement, keep the vacuum of the reactor at 0.1MPa, keep stirring the materials during this process, and the temperature of the reactor rises to 140°C, after 3 hours of reaction, stop heating, cool to room temperature, and turn off the vacuum system;

[0037] The second step reaction: add 60 grams of allyl bromide dropwise to the above reaction kettle, the molar ratio of fatty alcohol polyoxyethylene ether or alkylphenol polyoxyethylene ether to allyl bromide is 1: 1.3, during the dropwise addition process Stir the material continuously, after the dropwise addition, th...

Embodiment 3

[0040] The first step reaction: 200 grams of alkylphenol polyoxyethylene ether TX-10 (molecular weight 601) and 28 grams of solid potassium hydroxide (particle diameter 0.01mm) were dropped into a 500ml stainless steel autoclave, and the molar ratio was 1: 1.5. Stir the material at the same time as feeding, seal the reactor after feeding, replace the air in the reactor with nitrogen, start the vacuum system after the replacement, keep the vacuum of the reactor at 0.1MPa, keep stirring the materials during this process, and the temperature of the reactor rises to 70°C, after 1 hour of reaction, stop heating, cool to room temperature, and turn off the vacuum system;

[0041]The second step reaction: add 38 grams of allyl chloride dropwise to the above reaction kettle, the molar ratio of fatty alcohol polyoxyethylene ether or alkylphenol polyoxyethylene ether to allyl chloride is 1: 1.5, and the dripping process continues Stir the material, drop the reaction heat to 100°C after t...

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Abstract

The invention discloses a method for synthesizing allyl fatty alcohol-polyoxyethylene ether or allyl alkylphenol ethoxylate. The method comprises the following steps of: adding fatty alcohol-polyoxyethylene ether or alkylphenol ethoxylate and a solid alkali hydroxide into a stainless steel high pressure reactor, keeping the vacuum degree of the reactor to be 0.085 to 0.1MPa, rising the temperature of the reactor to 70 to 200 DEG C, performing reaction for 1 to 5 hours, stopping a vacuum system, continuing adding allyl halide dropwise into the reactor with continuously stirring, performing reaction under 30 to 100 DEG C and 0.1 to 0.5MPa for 1 to 8 hours, starting the vacuum system to remove residual allyl halide from a product, and discharging a raw product; and adding hot water into the raw product, uniformly mixing the hot water and the raw product, and standing and demixing the mixture to obtain the allyl fatty alcohol-polyoxyethylene ether or the allyl alkylphenol ethoxylate. The method has the advantages of no pollution, low cost and high conversion rate.

Description

technical field [0001] The invention relates to a method for synthesizing allyl fatty alcohol polyoxyethylene ether or allyl alkylphenol polyoxyethylene ether. Background technique [0002] The molecular structure of allyl fatty alcohol polyoxyethylene ether or allyl alkylphenol polyoxyethylene ether contains polyoxyethylene groups, and the end group contains double bonds. It has active chemical properties and can be used as an intermediate in the synthesis of surfactants. , such as alcohol ether sulfonate, etc. Its synthesis is carried out by Williamson reaction. Fatty alcohol polyoxyethylene ether or alkylphenol polyoxyethylene ether reacts with alkali metal hydroxide to generate the corresponding alcohol ether salt, and allyl halide is added to the alcohol ether salt for hydrophilic Nucleus substitution reaction to produce allyl fatty alcohol polyoxyethylene ether or allyl alkylphenol polyoxyethylene ether and alkali metal halide. [0003] The preparation method of ally...

Claims

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Application Information

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IPC IPC(8): C08G65/00C08G65/338C07C41/16C07C43/15C07C43/164
Inventor 康保安杨卉艳孙永强史修启孙晋源武华萍张勇
Owner CHINA RES INST OF DAILY CHEM IND
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