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Styrylphenol polyoxyethylene ether and preparation method thereof

A technology of styryl phenol and polyoxyethylene ether, which is applied in the field of styryl phenol polyoxyethylene ether and its preparation, can solve the problems of wide distribution, deep color and the like, and achieves narrow distribution, light color and strong selectivity. Effect

Active Publication Date: 2017-09-08
ZHEJIANG HUANGMA TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The styrene-based phenol polyoxyethylene ether product prepared by this type of existing technology has deep color (Pt-Co value greater than 150), wide distribution (molecular weight dispersion coefficient greater than 1.2), high K+ / Na+ ion content (greater than 500ppm), long-term It is easy to delaminate when placed, and is only suitable for pesticide emulsifier products with low quality requirements, while the high-end coating field requires polyether products to have a color value of less than 50 and a K+ / Na+ ion content of less than 50ppm

Method used

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  • Styrylphenol polyoxyethylene ether and preparation method thereof
  • Styrylphenol polyoxyethylene ether and preparation method thereof
  • Styrylphenol polyoxyethylene ether and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Embodiment 1: the influence of phenol alkylation reaction catalyst on product color and luster

[0032] Alkylation reaction: Weigh 253.4g of phenol and 2.03g of methanesulfonic acid catalyst into a four-neck flask, put nitrogen and raise the temperature to 90°C, add 560.6g of styrene dropwise under rapid stirring, complete the dropwise addition in 1.5 hours, and then keep the temperature until The refractive index (25°C) of the product reaches 1.5985-1.6020, the reaction is completely cooled to room temperature, and NaOH is added to adjust the pH to 7.0 to obtain 814g of styrylphenol.

[0033] Ethylene oxide polyaddition reaction: Weigh 500g of styrylphenol into the autoclave, heat up to 100°C under nitrogen, dehydrate in vacuum for 1 hour, then cool down to 40°C, add 0.55g of organic phosphazene salt, heat up to 100°C under nitrogen , 728.5g of ethylene oxide was added, the reaction was complete at 95°C and 0.025MPa, and 1228.5g of styrylphenol polyoxyethylene ether (a...

Embodiment 2

[0040] Embodiment 2: the influence of methylsulfonic acid catalyst dosage on product color and luster

[0041] On the basis of embodiment 1, continue to test the optimal phenol alkylation reaction catalyst selected, i.e. the addition of methanesulfonic acid, specifically expressed as follows:

[0042] (1) Alkylation reaction: Weigh 126.7g of phenol and 1.02g of methanesulfonic acid catalyst into a four-neck flask, put nitrogen and raise the temperature to 90°C, add 280.3g of styrene dropwise under rapid stirring, and dropwise add in 1.5 hours, then Insulate the reaction until the product's refractive index (25°C) reaches 1.5985-1.6020, and the reaction is completely cooled to room temperature. NaOH is added to adjust the pH to 7.0, and 407g of styrylphenol is obtained.

[0043] (2) Ethylene oxide polyaddition reaction: add styryl phenol into the autoclave, heat up to 100°C under nitrogen, cool down to 40°C after vacuum dehydration for 1 hour, add 0.45 g of organic phosphazene ...

Embodiment 3

[0046] Embodiment 3: the impact of ethylene oxide polyaddition catalyst on product index

[0047] Alkylation reaction: Weigh 126.7g of phenol and 0.81g of methanesulfonic acid catalyst into a four-necked flask, put nitrogen and raise the temperature to 90°C, add 280.3g of styrene dropwise under rapid stirring, complete the dropwise addition in 1.5 hours, and then keep warm for the reaction until The refractive index (25°C) of the product reaches 1.5985-1.6020, the reaction is completely cooled to room temperature, and NaOH is added to adjust the pH to 7.0 to obtain 407g of styrylphenol.

[0048] Ethylene oxide polyaddition reaction: Weigh 407g of styrylphenol into the autoclave, heat up to 100°C under nitrogen, dehydrate in vacuum for 1 hour, then cool down to 40°C, add 0.6g of organic phosphazene salt, heat up to 100°C under nitrogen , add 593g of ethylene oxide, complete the reaction at 100°C and 0.035MPa, and cool down to room temperature to obtain styrene-based phenol poly...

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Abstract

The invention relates to styrylphenol polyoxyethylene ether and a preparation method thereof, and belongs to the technical field of carbocyclic compounds. The method includes three steps of phenol alkylation reaction, ethylene oxide addition polymerization, polyether aftertreatment; to be more specific, feeding nitrogen in phenol and alkylation catalyst for heating up 80-100 DEG C, and dropwise adding styrene prior to heat reaction till the refractive index of the product reaches 1.5985-1.6020; heating up to 100-110 DEG C, performing vacuum dehydration prior to cooling and adding polymerization catalyst, heating to 80-120 DEG C under the atmosphere of nitrogen, and adding ethylene oxide for complete reaction at the temperature of 80-120 DEG C under the pressure of 0.01-0.04MPa; adding deionized water prior to heating to 60-70 DEG C, adding phosphoric acid and adsorbent with stirring prior to vacuum dehydration, and performing filtering to obtain the finished product. The preparation method can be applied to preparation of nonionic surfactants such as styrylphenol polyoxyethylene ether, and the product has the advantages of narrow distribution, light color, low content of K + / Na + ions and the like.

Description

technical field [0001] The invention relates to a styrylphenol polyoxyethylene ether and a preparation method thereof, belonging to the technical field of carbocyclic compounds. Background technique [0002] Styrylphenol polyoxyethylene ether products are a class of non-ionic surfactants with excellent performance and wide application. They have excellent emulsifying properties, warm viscosity and bactericidal properties, low volatility and stable performance. , An important component of cleaning agent products, the annual domestic demand is more than 10,000 tons. [0003] The preparation process of styrylphenol polyoxyethylene ether is divided into two steps, which are the alkylation reaction of phenol and the polyaddition reaction of ethylene oxide. Catalysts for the synthesis of styryl phenol (alkylation reaction) are mainly divided into two categories, one is inorganic acids: hydrochloric acid, sulfuric acid, phosphoric acid, oxalic acid, aluminum trichloride, etc. The ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/28C08G65/30
Inventor 陈世明金一丰高洪军万庆梅贺丽丹
Owner ZHEJIANG HUANGMA TECH
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