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A kind of method that adopts copper carbene catalyst to prepare alkynyl polyether modified organosilicon surfactant

A technology of surfactant and carbene catalyst, 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, low equipment requirements, and simple formula

Active Publication Date: 2022-02-18
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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  • A kind of method that adopts copper carbene catalyst to prepare alkynyl polyether modified organosilicon surfactant
  • A kind of method that adopts copper carbene catalyst to prepare alkynyl polyether modified organosilicon surfactant
  • A kind of method that adopts copper carbene catalyst to prepare alkynyl polyether modified organosilicon surfactant

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Example 1 Preparation of Copper Cabin Catalyst:

[0026] The preparation method of copper Cabin catalyst used in the present invention refers to the literature: Organic Letters2011 Vol 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] Its specific preparation method, with the above structure, the steps are as follows:

(1)

[0029]

[0030] 23 grams (5-isopropyl-2-pyridyl) phenylmethone, 200 ml of methanol, 5.4 g of phenylenediamine were sequentially added in 500 ml of reaction vessel, and hydrochloric acid was accepted. The solution was saturated, and the room temperature was filtered after 5 hours, and the filter cake was washed three times with 20 ml of methanol.

(2)

[0031]

[0032] The double imidazole salt was dispersed in 100 ml of tetrahydrofuran, cooled to 0 ° C, and then added to ...

Embodiment 2

[0034] A silicone surfactant (200≥ M ≥ 0, 200 ≥ n ≥ 0) is synthesized from alkynylene polyether to raw material.

[0035]

[0036] In a reactor having a fixing device, a constant temperature function, a mechanical stirring, a thermocouple, a 250L of nitrogen, an alkynyl polyether having an average molecular weight of 850, and 43 kg shown above. The hydrogen-containing polysiloxane is stirred, and the heating sleeve is heated to 60 ° C, stirred for 5 minutes, add 1 kg of catalyst, after 4 hours, to obtain a clear and translucent pale yellow silicone copolymer liquid, and the silicone copolymer is vacuum Under the conditions, the film evaporator with vacuum, heating and stirring is pumped. The temperature of the evaporator is 120 ° C, relative vacuum pressure -0.1MPa, the vacuum time is 12 hours, and the last vacuum is slowly cooled to 30 ° C, that is, oxide The radical modified silicone surfactant.

[0037] The above-described alkynyl polyether synthesis method is as follows:

[...

Embodiment 3

[0041] A silicone surfactant-modified silicone surfactant-synthetic polyether-modified silicone surfactant is synthesized by alkynyl polyether derived from methylphenylacetylene:

[0042]

[0043] In a reactor having a fixture, constant temperature function, mechanical stirring, thermocouple, and has a nitrogen, an alkynyl polyether having an average molecular weight of 950 as shown above, and 43kg shown above The hydrogen-containing polysiloxane is started, and the heating sleeve is heated to 60 ° C, stirred for 5 minutes, add 1.1 kg of catalyst, after 4 hours, to obtain a clear and translucent pale yellow silicone copolymer liquid, and the organic silicone copolymer Under vacuum conditions, a thin film evaporator with vacuum, heating and stirring is pumped, and the temperature of the evaporator is 120 ° C, relative vacuum pressure - 0.1 MPa, the vacuum time is 12 hours, and the last vacuum is slowly lowered to 30 ° C, that is, Alkynyl polyether modified silicone surfactant.

...

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Abstract

The invention belongs to the field of chemical industry, and provides a method for preparing alkynyl polyether modified organic silicon surfactant by using copper carbene catalyst, using alkynyl polyether, under the action of copper carbene catalyst, using alkynyl polyether and organic silicon High-efficiency preparation of alkynyl polyether-modified silicone surfactants. The present invention compares with the preparation method that adopts allyl polyether and acetylene glycol polyether, the alkynyl polyether in the present invention has higher activity, and its addition reaction condition with organosilane hydrogen compound is gentler, and equipment The requirements are lower, and the prepared silicone surfactant is applied in rigid polyurethane foam, showing more excellent physical properties.

Description

Technical field [0001] The present invention belongs to the field of chemical industry, and involves a method of polyether modified silicon, in particular to prepare a method of preparing a copper Cassin catalyst to prepare a method of modifying the silicone surfactant. Background technique [0002] The conventional unsaturated polyether is a pendant with an alcohol containing an unsaturated double bond, a polyether obtained from an epoxy monomer such as ethylene oxide (EO), and propylene oxide (PO). The alcohol containing the unsaturated double bond includes allyl alcohol, methanol, or the like. The most important use of unsaturated polyether is to use its unsaturated double bond to react with hydrogen-containing silicone oil to prepare polyether modified silicone surfactants. [0003] The polyether structure of the silicon hydrogenation reaction is different to obtain a polyether modified silicon having different molecular structures. At present, the most demand in the market i...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G77/46C09K23/54
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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