Method for preparing alkynyl polyether modified organic silicon surfactant by adopting copper carbene catalyst

A surfactant and carbene catalyst technology, which is applied in the field of polyether-based modified silicone, can solve the problem of unsatisfactory activity of modified silicone, and achieve excellent physical properties, convenient operation, and high activity.

Active Publication Date: 2021-01-22
SHANGHAI MAIPU NEW MATERIAL TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0008] Aiming at the problems existing in the prior art, the present invention provides a method for preparing alkynyl polyether modified silicone surfactant using copper carbene catalyst, which uses copper carbene catalyst to prepare alkynyl polyether modified The method of organosilicon surfactant should solve the unsatisfactory technical problem of unsaturated polyether modified organosilicon activity prepared in the prior art

Method used

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  • Method for preparing alkynyl polyether modified organic silicon surfactant by adopting copper carbene catalyst
  • Method for preparing alkynyl polyether modified organic silicon surfactant by adopting copper carbene catalyst
  • Method for preparing alkynyl polyether modified organic silicon surfactant by adopting copper carbene catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025]Example 1 Preparation of copper carbene catalyst:

[0026]The preparation method of the copper carbene catalyst used in the present invention refers to the literature: ORGANIC LETTERS2011Vol.13, No.195256-5259; Journal of Organometallic Chemistry 775(2015)155-163; Journal of Organometallic Chemistry 820(2016)1-7; Journal of Catalysis 319 (2014) 119-126; Tetrahedron: Asymmetry 24 (2013) 492-498.

[0027]

[0028]The specific preparation method takes the above structure as an example, and the steps are as follows:

[0029](1)

[0030]

[0031]In a 500 ml reaction vessel, add 23 g (5-isopropyl-2-pyridyl) phenyl ketone, 200 ml methanol, and 5.4 g o-phenylenediamine in sequence. Under the condition of sufficient stirring, add hydrochloric acid gas to The solution was saturated, reacted at room temperature for 5 hours, and then filtered. The filter cake was washed three times with 20 ml of methanol to obtain 28 g of bisimidazole salt with a yield of 90%.

[0032](2)

[0033]

[0034]Disperse 6.2 g of the bisi...

Embodiment 2

[0036]Synthesize an alkynyl polyether-modified organosilicon surfactant with alkynyl polyether derived from phenylacetylene as raw material (200≥m≥0, 200≥n≥0):

[0037]

[0038]In a 250L reactor with a fixed device, constant temperature function, mechanical stirring, thermocouple and nitrogen gas, 100kg of alkynyl polyether with an average molecular weight of 850 as shown above, and 43kg Hydrogen-containing polysiloxane, start stirring, use a heating mantle to heat to 60°C, stir for 5 minutes, add 1kg of catalyst, and react for 4 hours to obtain a clear and transparent light yellow silicone copolymer liquid. Put the silicone copolymer in a vacuum Under the conditions, a thin film evaporator with vacuum, heating and stirring is pumped in. The temperature of the evaporator is 120°C, the relative vacuum pressure is -0.1MPa, and the vacuum time is 12 hours. Finally, the temperature is slowly reduced to 30°C under vacuum, which is alkyne -Based polyether modified silicone surfactant.

[0039]The ...

Embodiment 3

[0043]Synthesize an alkynyl polyether modified silicone surfactant with alkynyl polyether derived from p-toluene acetylene as a raw material:

[0044]

[0045]In a 250L reactor with a fixed device, constant temperature function, mechanical stirring, thermocouple and nitrogen gas, 105kg of alkynyl polyether with an average molecular weight of 950 as shown above is added, and 43kg as shown above Hydrogen-containing polysiloxane, start stirring, use a heating mantle to heat to 60°C, stir for 5 minutes, add 1.1 kg of catalyst, and react for 4 hours to obtain a clear and transparent light yellow silicone copolymer liquid. A thin film evaporator with vacuum, heating and stirring is pumped in under vacuum. The temperature of the evaporator is 120°C, the relative vacuum pressure is -0.1MPa, and the vacuum time is 12 hours. Finally, the temperature is slowly reduced to 30°C under vacuum. Alkynyl polyether modified silicone surfactant.

[0046]The synthesis method of the above-mentioned alkynyl polyet...

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Abstract

The invention belongs to the field of chemical engineering, and provides a method for preparing an alkynyl polyether modified organic silicon surfactant by using a copper carbene catalyst, which is used for efficiently preparing the alkynyl polyether modified organic silicon surfactant by reacting alkynyl polyether with organic silicon under the action of the copper carbene catalyst. Compared witha preparation method adopting allyl polyether and alkynediol polyether, alkynyl polyether has higher activity, the addition reaction condition of alkynyl polyether and an organic silicone hydrogen compound is milder, the equipment requirement is lower, and the prepared organic silicone surfactant is applied to hard polyurethane foam, and the surfactant has more excellent physical properties.

Description

Technical field[0001]The invention belongs to the field of chemical industry, and relates to a base polyether modified organic silicon, specifically a method for preparing an alkynyl polyether modified organic silicon surfactant using a copper carbene catalyst.Background technique[0002]The traditional unsaturated polyether is a polyether obtained by reacting an alcohol containing an unsaturated double bond as an initiator and an epoxy monomer such as ethylene oxide (EO) and propylene oxide (PO). Alcohols containing unsaturated double bonds include allyl alcohol, methallyl alcohol and the like. The main purpose of unsaturated polyether is to use its unsaturated double bond to react with hydrogen-containing silicone oil to prepare polyether modified silicone surfactant.[0003]The polyether structure used in the hydrosilation reaction is different, and polyether-modified silicones with different molecular structures are obtained. At present, allyl polyoxyethylene ether, allyl polyoxyeth...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G77/46B01F17/54C09K23/54
CPCC08G77/46C09K23/00
Inventor 张文凯信延垒龚国安
Owner SHANGHAI MAIPU NEW MATERIAL TECH CO LTD
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