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Synthetic method of acetylene glycol polyoxyethylene ether

A kind of technology of acetylene glycol polyoxyethylene ether and synthesis method, which is applied in the field of synthesis of acetylene glycol polyoxyethylene ether, can solve the loss of unsaturation of acetylene glycol polyoxyethylene ether, and the unsaturation of acetylene glycol polyoxyethylene ether. Problems such as high saturation and carbon-carbon triple bond destruction

Active Publication Date: 2016-08-24
SHANGHAI DUOLUN CHEM
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  • Abstract
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Problems solved by technology

[0005] The present 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 synthesis method of the acetylene glycol polyoxyethylene ether. The method has the advantage of high degree of unsaturation of the synthesized acetylenic glycol polyoxyethylene ether

Method used

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  • Synthetic method of acetylene glycol polyoxyethylene ether
  • Synthetic method of acetylene glycol polyoxyethylene ether
  • Synthetic method of acetylene glycol polyoxyethylene ether

Examples

Experimental program
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Effect test

Embodiment 1

[0032] 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 calcium hydroxide), 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, dehydrate in vacuum, and filter to obtain the product 2,4,7,9-tetramethyl-5-decyne-4,7-diol polyoxyethylene ether (10).

[0033] Determine the degree of unsaturation, chroma and hydroxyl value of the product. For ease of comparison, the c...

Embodiment 2

[0035] Add 1 mole of 2,4,7,9-tetramethyl-5-decyne-4,7-diol and 5 grams of catalyst (the catalyst is N-methylmorpholine) into a 1L stirred autoclave, 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, dehydrate in vacuum, and filter to obtain the product 2,4,7,9-tetramethyl-5-decyne-4,7-diol polyoxyethylene ether (10).

[0036] Determine the degree of unsaturation, chroma and hydroxyl value of the product. For ease of comparison, the c...

Embodiment 3

[0038] 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 ammonia water, dehydrate in vacuum, and filter to obtain the product 2,4,7,9-tetramethyl-5-decyne-4,7-diol polyoxyethylene ether (10).

[0039] Determine the degree of unsaturation, ch...

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Abstract

The invention relates to a method for synthesizing an acetylene alcohol polyoxyethylene ether. The technical problem of unsaturation loss of the acetylene alcohol polyoxyethylene ether, caused by the existing synthesis method, is mainly solved. According to the method for synthesizing the acetylene alcohol polyoxyethylene ether, butynediol reacts with ethylene oxide in the presence of a catalyst to obtain the acetylene alcohol polyoxyethylene ether, wherein the catalyst comprises at least one of calcium hydroxide, a tertiary amine aliphatic compound and a protonic acid; the butynediol has a structure shown in a formula (I); R1 and R4 are independently selected from C3-C10 alkyl; R2 and R3 are independently methyl or ethyl. The technical problem is better solved, and the method can be applied to industrial production of the acetylene alcohol polyoxyethylene ether. The expression is as shown in the specification.

Description

technical field [0001] The present invention relates to the synthetic method of acetylenic diol polyoxyethylene ether, in particular to the preparation by polymerization reaction using 2,4,7,9-tetramethyl-5-decyne-4,7-diol and ethylene oxide as raw materials Method for 2,4,7,9-tetramethyl-5-decyne-4,7-diol ethoxylates. 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 2,4,7,9-tetramethyl-5-decyne-...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G65/28
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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