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Esterification and termination synthesis method of allyl polyether

A technology of allyl polyether and synthesis method, which is applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., and can solve problems such as high cost, little practical significance, and environmental pollution by sodium chloride

Inactive Publication Date: 2010-06-16
NANJING FORESTRY UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although it can achieve a good end-capping effect, its cost is relatively high, and toxic thionyl chloride is used in the reaction process, and a large amount of by-product sodium chloride is generated to pollute the environment
Therefore, this method only stays in the stage of laboratory research and has little practical significance.
3. Acid anhydride end-capping, acid anhydride end-capping esterification can achieve high end-capping effect, the patent application with publication number EP0675147 proposes to use an acid anhydride end-capping with a suitable catalyst, and the esterification rate can almost reach 100%, but the method cost higher
However, this method generally has a low end-capping rate and high cost, making it difficult to meet industrial requirements.

Method used

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  • Esterification and termination synthesis method of allyl polyether

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Add 414g allyl polyoxyethylene ether (hydroxyl value 135.5mgKOH / g), 1.53g p-toluenesulfonic acid, 153g toluene, 96g acetic acid into a 1L four-neck flask equipped with a mechanical stirrer, reflux condenser and water trap. , Turn on the condensed water, turn on the stirring device, and heat to make the reaction proceed. When the temperature is raised to boiling, the time is started, and the water separation operation 5h ends. Then, when the temperature drops to normal temperature, the reaction device is switched to a vacuum distillation device to remove toluene and unreacted acetic acid, and then undergo a refining process to obtain a colorless esterified end-capped polyether product. The measured hydroxyl value of the product was 3.7 mgKOH / g, and the esterification end-capping rate was 97.3%.

Embodiment 2

[0038] Add 414g allyl polyoxyethylene ether (hydroxyl value 135.5mgKOH / g), 2.04g p-toluenesulfonic acid, 204g toluene, 96g acetic acid into a 1L four-neck flask equipped with a mechanical stirrer, reflux condenser and water trap. , Turn on the cooling water, turn on the stirrer, heat up to boiling and start timing, and the water splitting operation ends for 7 hours. Then, when the temperature drops to normal temperature, the reaction device is switched to a vacuum distillation device to remove toluene and unreacted acetic acid, and then undergo a refining process to obtain a colorless esterified end-capped polyether product. The measured hydroxyl value of the product was 2.2 mgKOH / g, and the esterification capping rate was 98.4%.

Embodiment 3

[0040] Add 414g allyl polyoxyethylene ether (hydroxyl value 135.5mgKOH / g), 1.05g p-toluenesulfonic acid, 209g toluene, 108g acetic acid into a 1L four-neck flask equipped with a mechanical stirrer, reflux condenser and water trap. , Turn on the cooling water, turn on the stirrer, heat up to boiling and start timing, and the water splitting operation ends for 3 hours. Then, when the temperature drops to normal temperature, the reaction device is switched to a vacuum distillation device to remove toluene and unreacted acetic acid, and then undergo a refining process to obtain a colorless esterified end-capped polyether product. The measured hydroxyl value of the product is 11.5 mgKOH / g, and the esterification end-capping rate is 91.5%.

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Abstract

The invention relates to an esterification and termination synthesis method of allyl polyether, which comprises the steps of taking allyl polyether and acetic acid as raw materials, and carrying out esterification in a reactor under the action of a catalyst and a dehydrating agent, wherein the molar mixing ratio of the allyl polyether to the acetic acid is 1: 1.0-3.0; the catalyst is p-toluenesulfonic acid, and the using quantity by weight thereof accounts for 0.1-2.0% of the total weight of fed materials; and the dehydrating agent is toluene, and the using quantity by weight thereof accounts for 20-50% of the total weight of the fed materials. The esterification and termination synthesis method of the allyl polyether has the advantages of simple and easy operation, low cost and high termination ratio, thereby being applicable to the large-scale industrial production of the esterified terminated allyl polyether.

Description

Technical field [0001] The invention relates to a polyether esterification end-capping process, in particular to an allyl polyether esterification end-capping synthesis method. Background technique [0002] Allyl polyether is a monofunctional polyether prepared by homopolymerizing, block or random polymerization with ethylene oxide (EO) or propylene oxide (PO) with propylene alcohol as an initiator. Because its double bond can react with some active groups to modify the polyether, it has attracted attention. Its structural formula is as follows: [0003] CH 2 =CHCH 2 O(CH 2 CHR 1 O) x (CH 2 CHR 2 O) y (CH 2 CHR 3 O) z H [0004] In the formula: x = an integer from 0 to 70, y = an integer from 0 to 70, z = an integer from 0 to 70, x+y+z = 3 to 70; R 1 , R 2 , R 3 Is H or CH 3 ; Allyl polyether segment polymerization mode is random, homopolymerization or block. [0005] Allyl polyether is not resistant to acid, alkali and high temperature due to the presence of terminal active hydroxy...

Claims

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Application Information

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IPC IPC(8): C08G65/332C07C67/08C07C69/14
Inventor 朱新宝陈华于子洲董晓红郝思珍郝静琳
Owner NANJING FORESTRY UNIV
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