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A kind of preparation method of diallyl terminated polyether

A technology of diallyl capping and allyl chloride, which is applied in the field of preparation of diallyl capping polyether, can solve the problem of unsuitable green chemical process and product color protection, limited intermediate polyether structure, propenyl Low degree of problems, to achieve the effects of reducing solvent recovery costs, mild reaction process, and lower viscosity

Active Publication Date: 2017-10-10
ZHEJIANG HUANGMA TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The limitation of this method is that there are many by-products; the structure of the intermediate polyether is limited; the process is also very complicated, and it is necessary to synthesize polyether diol diglycidyl ether and monoallyl polyether first, and add water washing process before post-treatment
[0006] CN101885839A discloses a method for preparing end-capped allyl polyether, using a machine solvent to azeotropically remove water, alcoholizing the polyether under the action of an alkali, and then adding allyl chloride or allyl bromide, the The method uses toxic organic solvents toluene or xylene, which does not meet the protection of green chemical technology and product color
[0007] CN101982481A discloses a preparation method of alkyl-terminated allyl polyether, which uses polyether and alkali metal hydroxide as raw materials, directly drops allyl chloride in one-step method without alkoxide reaction, and the method Simple, low degree of allyl isomerization to propenyl, but insufficient end-capping ratio

Method used

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  • A kind of preparation method of diallyl terminated polyether
  • A kind of preparation method of diallyl terminated polyether
  • A kind of preparation method of diallyl terminated polyether

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Put 1200g allyl alcohol polyoxyethylene ether (m=25.5, molecular weight 1200) and 52g NaOH into the reaction kettle, start stirring, put nitrogen in the kettle, add 68.9g allyl chloride at 25°C, and then Raise the temperature to 80°C for 4.5 hours; after the end, control the temperature in the kettle to 110°C, vacuumize to remove excess allyl chloride, dehydrate for 3 hours, then cool down to 85°C at 1°C / min, and continue to add 76.5g of allyl chloride Chlorine reacted for 4 hours, and the crude product was obtained so far; neutralizer, adsorbent and filter aid were added to the crude product, and refined to obtain the product bisallyl-terminated polyoxyethylene ether (m=25.5). Among them, the neutralizing agent is 50% phosphoric acid aqueous solution, and the addition amount is 25 g; the adsorbent is acid clay, and the addition amount is 6 g; the filter aid is diatomite, and the addition amount is 6 g.

[0037] The end-capping rate of the finished bisallyl-terminated p...

Embodiment 2

[0039] Put 1200g allyl alcohol random polyether (m=24.6, n=6.6, molecular weight 1510) and 93.4g KOH into the reaction kettle, start stirring, and slowly add 103.4g allyl chloride at 30°C through nitrogen built into the kettle, Then heat up to 60°C at 2°C / min and react for 7 hours; after the end, control the temperature in the kettle to 110°C, vacuumize and degas and dehydrate for 3 hours, then cool down to 75°C at 2°C / min, and continue to add 24.3g allyl Chlorine reaction 4.5h, so far obtain crude product; (3) add neutralizer, adsorbent and filter aid in crude product, refine and obtain product bisallyl capped random polyether (m=24.6, n=6.6 ). Among them, the neutralizing agent is glacial acetic acid, and the addition amount is 53 g; the adsorbent is acid clay, and the addition amount is 12 g; the filter aid is diatomaceous earth, and the addition amount is 12 g.

[0040] The bisallyl terminated atactic polyether (m=24.6, n=6.6) obtained in this example has a capping rate o...

Embodiment 3

[0042]Put 1200g of allyl alcohol random polyether (m=23.5, n=4.6, molecular weight 1350), 106.7g of NaOH and KOH mixture (molar ratio is 1:1) into the reaction kettle, start stirring, and put nitrogen in the kettle, Slowly add 136g of allyl chloride at 20°C, then raise the temperature to 70°C at 0.5°C / min and react for 3 hours; after the end, control the temperature in the kettle to 115°C, vacuumize and degas and dehydrate for 3 hours, and then lower the temperature at 0.5°C / min To 80°C, continue to add 13.6g allyl chloride to react for 3h, so far to obtain the crude product; (3) add neutralizer, adsorbent and filter aid to the crude product, and refine to obtain the product diallyl-terminated random Polyether (m=23.5, n=4.6). Among them, the neutralizing agent is 50% phosphoric acid aqueous solution, and the addition amount is 87g; the adsorbent is acid clay, and the addition amount is 24g; the filter aid is diatomite, and the addition amount is 24g.

[0043] The bisallyl-te...

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Abstract

The invention relates to a preparation method of diallyl-terminated polyether, which belongs to the technical field of organic chemical industry. Using polyether and alkali as raw materials, first add part of the end-capping agent for pre-reaction, after the pre-reaction, vacuum degassing and dehydration, then add the remaining end-capping agent for further reaction to obtain the crude product, and refine the crude product to obtain finished product. It has the advantages of good color, high end-capping rate, low degree of allyl isomerization, and simple process.

Description

technical field [0001] The invention belongs to the technical field of organic chemical industry, and in particular relates to a preparation method of diallyl-terminated polyether. Background technique [0002] Diallyl-terminated polyether contains double bonds at both ends of the molecular chain, and is an important bridging agent for organic synthesis. It is widely used in industries such as polyurethane, pharmaceuticals, papermaking, new silicone materials, and chemical fibers. In the field of silicone, grafted silicone oil is prepared by reacting the C=C double bond of diallyl-terminated polyether with the Si-H of hydrogen-containing silicone oil. When allyl isomerized to propenyl, the reaction will not Therefore, the degree of isomerization of bisallyl-terminated polyether directly affects the quality of grafted silicone oil. [0003] At present, the main preparation process of dialkyl-terminated polyether is to react polyether with alkali to generate alkoxide, and the...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G65/00
Inventor 张美军金一丰陈荧杰马定连俞芳
Owner ZHEJIANG HUANGMA TECH
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