Catalyst for synthesis of acetylene alcohol polyoxyethylene ether

A technology of acetylene glycol polyoxyethylene ether and catalyst, which is applied in the field of catalysts, and can solve the problems of loss of unsaturation of acetylene glycol polyoxyethylene ether, destruction of carbon-carbon triple bonds, high degree of unsaturation of acetylene glycol polyoxyethylene ether, etc. question

Active Publication Date: 2014-08-06
SHANGHAI DUOLUN CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The invention mainly solves the technical problem that the existing synthesis method easily causes the destruction of the carbon-carbon triple bond and causes the loss of unsaturation of the acetylene glycol polyoxyethylene ether, and provides a new catalyst for the synthesis of the acetylene glycol polyoxyethylene ether , the catalyst has the advantage of high unsaturation of the synthesized acetylenic glycol polyoxyethylene ether

Method used

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  • Catalyst for synthesis of acetylene alcohol polyoxyethylene ether
  • Catalyst for synthesis of acetylene alcohol polyoxyethylene ether
  • Catalyst for synthesis of acetylene alcohol polyoxyethylene ether

Examples

Experimental program
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Effect test

Embodiment 1

[0031] Add 1 mole of 2,4,7,9-tetramethyl-5-decyne-4,7-diol and 5 grams of catalyst (catalyst is calcium hydroxide) in a 1L stirred autoclave, seal the reactor, Turn on stirring. The air in the reactor was replaced with nitrogen three times, and then vacuumed at 60° C. and a pressure of −0.05 MPa for 30 min. Then feed oxirane in the reactor, control reaction temperature to be 120 ℃ and reaction pressure be 0.2MPa, be 10 moles until the total amount of passing oxirane, then stop feeding oxirane to complete subject response. The temperature of the reactor was maintained at 120° C. until the pressure of the reactor no longer dropped, indicating that the aging reaction was completed. Lower the temperature to 80°C, neutralize with citric acid, vacuum dehydrate, and filter to obtain the product 2,4,7,9-tetramethyl-5-decyne-4,7-diol polyoxyethylene ether (10).

[0032] Determine the degree of unsaturation, chroma and hydroxyl value of the product. For ease of comparison, the compo...

Embodiment 2

[0034] In a 1L stirred autoclave, add 1 mole of 2,4,7,9-tetramethyl-5-decyne-4,7-diol and 5 grams of catalyst (catalyst is N-methylmorpholine), seal Reactor, start stirring. The air in the reactor was replaced with nitrogen three times, and then vacuumed at 60° C. and a pressure of −0.05 MPa for 30 min. Then feed oxirane in the reactor, control reaction temperature to be 120 ℃ and reaction pressure be 0.2MPa, be 10 moles until the total amount of passing oxirane, then stop feeding oxirane to complete subject response. The temperature of the reactor was maintained at 120° C. until the pressure of the reactor no longer dropped, indicating that the aging reaction was completed. Lower the temperature to 80°C, neutralize with citric acid, vacuum dehydrate, and filter to obtain the product 2,4,7,9-tetramethyl-5-decyne-4,7-diol polyoxyethylene ether (10).

[0035] Determine the degree of unsaturation, chroma and hydroxyl value of the product. For ease of comparison, the compositi...

Embodiment 3

[0037] In a 1L stirred autoclave, add 1 mole of 2,4,7,9-tetramethyl-5-decyne-4,7-diol and 5 grams of catalyst (the catalyst is H 3 PO 4, with a concentration of 85w% in the form of commercially available concentrated phosphoric acid), seal the reactor, and start stirring. The air in the reactor was replaced with nitrogen three times, and then vacuumed at 60° C. and a pressure of −0.05 MPa for 30 min. Then feed oxirane in the reactor, control reaction temperature to be 120 ℃ and reaction pressure be 0.2MPa, be 10 moles until the total amount of passing oxirane, then stop feeding oxirane to complete subject response. The temperature of the reactor was maintained at 120° C. until the pressure of the reactor no longer dropped, indicating that the aging reaction was completed. Lower the temperature to 80°C, neutralize with aqueous ammonia, dehydrate in vacuum, and filter to obtain the product 2,4,7,9-tetramethyl-5-decyne-4,7-diol polyoxyethylene ether (10).

[0038] Determine t...

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Abstract

The invention relates to a catalyst for synthesis of an acetylene alcohol polyoxyethylene ether, and mainly aims to solve the technical problem of unsaturation loss of the acetylene alcohol polyoxyethylene ether caused by the existing catalyst. The catalyst for synthesis of the acetylene alcohol polyoxyethylene ether comprises at least one of calcium hydroxide, a tertiary amine aliphatic compound and a protonic acid. Thus, the technical problem is well solved, and the catalyst can be applied to industrial production of the acetylene alcohol polyoxyethylene ether.

Description

technical field [0001] The invention relates to a catalyst for the synthesis of acetylene glycol polyoxyethylene ether, in particular to a catalyst for the synthesis of 2,4,7,9-tetramethyl-5-decyne-4,7-diol and ethylene oxide as raw materials A catalyst for preparing 2,4,7,9-tetramethyl-5-decyne-4,7-diol polyoxyethylene ether by polymerization. Background technique [0002] 2,4,7,9-tetramethyl-5-decyne-4,7-diol polyoxyethylene ether is 2,4,7,9-tetramethyl-5-decyne-4,7- Diol (TMDD), English name: 5-Decyne-4, 7-diol-2, 4, 7, 9-tetramethyl (CAS NO: 126-86-3) as the initiator to initiate the polymerization of ethylene oxide Products, this series of products are harmless to humans and animals, and are harmless to the environment. They are environmentally friendly non-ionic surfactants, with unique dihydroxy groups and alkynyl groups in their structure, and unique surface activity. Compared with traditional surfactants, it has better performance. [0003] CN103601881A discloses...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/28B01J23/02B01J31/02B01J27/16B01J23/04B01J31/26C07C43/14C07C41/03
Inventor 徐兴建孟益权舒建生朱学文林真意侯海育张江锋
Owner SHANGHAI DUOLUN CHEM
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