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Method for preparing butyl end-capping allyl polyethenoxy ether

A technology of allyl polyoxyethylene ether and allyl polyoxyethylene alkoxide, which is applied in the field of preparation of butyl-terminated allyl polyoxyethylene ether, can solve the problem of increasing side reactions, inapplicability of end-capping agents, Affect product quality and other issues, to achieve the effect of fast response and high utilization rate

Active Publication Date: 2010-01-20
ZHEJIANG HUANGMA TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Chinese patents CN1563146A, CN1311264A, and CN1311265A report polyether alkyl end-capping methods all adopt a one-step method, and its shortcoming is that moisture will be generated during the alkoxide reaction process, and if the etherification end-capping reaction is carried out simultaneously, the side reaction will be increased. Occurrence, in order to improve the capping efficiency will inevitably increase the amount of capping agent, which increases the cost and increases the pressure of product refining
Its ratio is relatively high. The disadvantage is that it increases the cost on the one hand, and on the other hand, too much alkaline substance will affect the quality of the product.
The disadvantage is that the process control is more difficult, and the end-capping agent is not suitable for the preparation of butyl-capped allyl polyoxyethylene ether

Method used

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  • Method for preparing butyl end-capping allyl polyethenoxy ether
  • Method for preparing butyl end-capping allyl polyethenoxy ether

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] In this embodiment, potassium hydroxide is used as an alkoxide reagent, and bromobutane is used as an end-capping agent to react:

[0026] Allyl polyoxyethylene ether has the following general formula (I):

[0027] CH 2 =CHCH 2 (OCH 2 -CH 2 ) n OH (I)

[0028] Among them: n<20;

[0029] The prepared butyl-terminated allyl polyoxyethylene ether has the following general formula (II):

[0030] CH 2 =CHCH 2 (OCH 2 -CH 2 ) n OCH 2 CH 2 CH 2 CH 3 (II)

[0031] Among them: n<20;

[0032] The reaction equation is:

[0033]

[0034] Where: R is CH 2 =CHCH 2 (OCH 2 -CH 2 ) n , n<20.

[0035] The definition of capping efficiency in the embodiment of the present invention is:

[0036]

[0037]Add 1,000 grams of allyl polyoxyethylene ether (purchased from Zhejiang Huangma Chemical Group Co., Ltd., with a molecular weight of 498) and 146 grams of solid potassium hydroxide into a 2L reactor, and stir vigorously. The temperature is 100-110°C, under ...

Embodiment 2

[0039] Add 1,000 grams of allyl polyoxyethylene ether (purchased from Zhejiang Huangma Chemical Group Co., Ltd., with a molecular weight of 938) and 90 grams of solid potassium hydroxide into a 2-liter reactor, and stir vigorously. The temperature is 100-110°C, under vacuum conditions (pressure -0.09--0.1MPa) and dehydration at the same time, and the reaction is 3 hours. The temperature was lowered to 60-70°C, 219 g of bromobutane was slowly introduced, and the pressure was maintained at 0.3 MPa, and the reaction was continued for 5 hours. Excess bromobutane was distilled off under reduced pressure, and solid impurities were removed by filtration to obtain a blocked polyether product.

Embodiment 3

[0041] Add 1,000 grams of allyl polyoxyethylene ether (purchased from Zhejiang Huangma Chemical Group Co., Ltd., with a molecular weight of 278) and 144 grams of solid sodium hydroxide into a 2-liter reactor, and stir vigorously. The temperature is 100-110°C, under vacuum conditions (pressure -0.09--0.1MPa) and dehydration at the same time, and the reaction is 3 hours. The temperature was lowered to 60-70°C, 493 g of bromobutane was slowly introduced, and the pressure was maintained at 0.3 MPa, and the reaction was continued for 4 hours. Excess bromobutane was distilled off under reduced pressure, and solid impurities were removed by filtration to obtain a blocked polyether product.

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Abstract

The invention discloses a method for preparing butyl end-capping allyl polyethenoxy ether, which comprises the following steps: adopting allyl polyethenoxy ether and bromobutane as raw materials to react with allyl polyethenoxy ether under the condition of adopting alkali as an alkoxide reagent to generate allyl polyoxyethylene alcoholate, and then the allyl polyoxyethylene alcoholate reacts with the bromobutane as an end capping reagent to prepare the butyl end-capping allyl polyethenoxy ether, wherein the alkoxide reagent adopts any one or a mixture of solid potassium hydroxide or sodium hydroxide, and the charging molar ratio of the allyl polyethenoxy ether to the alkoxide reagent is 1:1-1.5. The invention has high reaction speed, no pollution and higher end capping efficiency.

Description

technical field [0001] The invention relates to a preparation method of butyl-terminated allyl polyoxyethylene ether. It belongs to the technical field of preparation of alkyl-terminated polyether. Background technique [0002] Butyl-terminated allyl polyoxyethylene ether has oil solubility, high temperature resistance, acid and alkali resistance, foam suppression, etc. Abilities are enhanced and have unique features. Butyl-terminated allyl polyoxyethylene ether can be used in the high-speed spinning oil of chemical fiber; it can also be used as an additive in high-temperature-resistant lubricating oil or heat-conducting oil; it can also be used in strong alkaline detergent formulations In addition, it is an excellent cell opener and silicone foam stabilizer in the polyurethane industry. [0003] Butyl-capped allyl polyoxyethylene ether is a new type of capped polyether product, and its preparation method has not been reported. The relevant preparation method is the exis...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/329C08G65/328C07C43/15C07C41/01
Inventor 王伟松王新荣金一丰郭晓锋张月江
Owner ZHEJIANG HUANGMA TECH