A microwave synthesis method of 1,3-bis[2-(3,4-epoxycyclohexyl)ethyl]tetramethyldisiloxane

A technology of tetramethyldisiloxane and epoxycyclohexyl, which is applied in the field of microwave synthesis of 1,3-bis[2-ethyl]tetramethyldisiloxane, can solve the problem of low product yield and reaction Long time, high cost and other problems, to achieve the effect of simplified recovery steps, short reaction time and fast heating speed

Active Publication Date: 2022-04-08
CHANGZHOU HIGH TECH RES INST OF NANJING UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] At present, 1,3-bis[2-(3,4-epoxycyclohexyl)ethyl]tetramethyldisiloxane is synthesized by traditional techniques such as conventional oil bath or electric heating, usually at 60-75 The reaction at ℃ for more than 6 hours, the reaction time is long and the energy consumption is large, especially the prolonged reaction time leads to the opening of the epoxy ring, resulting in low product yield and high cost

Method used

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  • A microwave synthesis method of 1,3-bis[2-(3,4-epoxycyclohexyl)ethyl]tetramethyldisiloxane
  • A microwave synthesis method of 1,3-bis[2-(3,4-epoxycyclohexyl)ethyl]tetramethyldisiloxane
  • A microwave synthesis method of 1,3-bis[2-(3,4-epoxycyclohexyl)ethyl]tetramethyldisiloxane

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Experimental program
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Effect test

Embodiment 1

[0023] (1) Under the protection of inert gas, 26.86g (0.20mol) tetramethyldisiloxane, 20.00mL dry toluene, 52.16g (0.42mol) 4-vinyl-1,2-epoxycyclohexene Add it into a dry reaction flask and stir at room temperature, then add 0.54g (wherein the Pt load is 0.4wt%) Pt / NaY molecular sieve supported catalyst, and finally add 0.60mL absolute ethanol, and continue stirring to obtain a uniform suspension;

[0024] (2) Move the suspension into the microwave synthesis reactor, and use the temperature control mode for heating in the microwave oven. The reaction was monitored by layer chromatography (TLC). After reacting for 20 minutes, the reaction liquid was distilled off under reduced pressure to remove solvent and low boilers, and then the product was centrifuged to separate the Pt / NaY molecular sieve supported catalyst to obtain 1,3-bis[2- (3,4-epoxycyclohexyl)ethyl]tetramethyldisiloxane, the yield is 97.5%, the active hydrogen conversion rate of the raw material is 95.6%, and the ep...

Embodiment 2

[0030] (1) Under the protection of inert gas, 33.58g (0.25mol) tetramethyldisiloxane, 25.00mL dry n-hexane, 69.60g (0.56mol) 4-vinyl-1,2-epoxycyclohexane Add ene into the dry reaction flask and stir at room temperature, then add 0.52g (Pt loading is 0.3wt%) Pt / NaY molecular sieve supported catalyst, finally add 1.25mL absolute ethanol, continue stirring to obtain a uniform suspension;

[0031] (2) Move the suspension into the microwave synthesis reactor, use the temperature control mode for heating in the microwave oven, set the microwave radiation frequency of the microwave synthesis reactor to 2400MHz, set the microwave synthesis reactor power to 700W, and the reaction temperature to 70°C, The reaction was monitored by layer chromatography (TLC). After reacting for 10 minutes, the reaction solution was distilled off under reduced pressure to remove solvent and low boilers, and then the product was centrifuged to separate the Pt / NaY molecular sieve supported catalyst to obtain...

Embodiment 3

[0035] (1) Under the protection of an inert gas, 96.71g (0.72mol) of tetramethyldisilane, 72.00mL of dry tetrahydrofuran, and 205.60g (1.65mol) of 4-vinyl-1,2-epoxycyclohexene were added to the In the dry reaction bottle, stir at room temperature, then add 1.65g (the loading capacity of Pt is 0.6wt%) Pt / USY molecular sieve supported catalyst, finally add 5.04mL absolute ethanol, continue to stir to obtain a uniform suspension;

[0036] (2) Move the suspension into the microwave synthesis reactor, and use the temperature control mode for heating in the microwave oven. Layer chromatography (TLC) monitors reaction, and after 15 minutes of reaction finishes, the reaction solution is distilled off under reduced pressure to remove solvent and low boiling matter, then the product is centrifuged, and the Pt / USY molecular sieve supported catalyst is separated to obtain 1,3-bis[ 2-(3,4-epoxycyclohexyl)ethyl]tetramethyldisiloxane, the yield is 97.8%, the active hydrogen conversion rate o...

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Abstract

The invention discloses a microwave synthesis method of 1,3-bis[2-(3,4-epoxycyclohexyl)ethyl]tetramethyldisiloxane. Including: (1) Under the protection of inert gas, sequentially add tetramethyldisiloxane, organic solvent, 4-vinyl-1,2-epoxycyclohexene into the reaction flask and stir, and then add the supported Pt / Y molecular sieve catalyst, finally add absolute ethanol, continue to stir to obtain a suspension; (2) move the suspension into a microwave synthesis reactor for reaction, after the reaction, the reaction solution is decompressed to remove solvents and low boilers, and then centrifuged , to give 1,3-bis[2-(3,4-epoxycyclohexyl)ethyl]tetramethyldisiloxane. The invention has mild reaction conditions, short reaction time, high conversion rate of raw material active hydrogen, excellent activity and stability of the catalyst, recyclable reuse, reduced cost, high yield of the prepared target product, and good industrialization prospect.

Description

technical field [0001] The invention relates to the technical fields of microwave synthesis and organic silicon chemistry, in particular to a microwave synthesis method of 1,3-bis[2-(3,4-epoxycyclohexyl)ethyl]tetramethyldisiloxane. Background technique [0002] The molecular structural formula of 1,3-bis[2-(3,4-epoxycyclohexyl)ethyl]tetramethyldisiloxane is: [0003] The reaction to synthesize 1,3-bis[2-(3,4-epoxycyclohexyl)ethyl]tetramethyldisiloxane belongs to hydrosilylation. The hydrosilylation reaction is an addition reaction between Si-H-containing organosilicon compounds and unsaturated hydrocarbon compounds under certain catalytic conditions, and plays an important role in the industrialization of organosilicon (Platinum Catalysis Revisited Unraveling Principles of Catalytic Olefin Hydrosilylation[J].ACS Catalysis,2016,6(2):1274-1284.). It is widely used in silane polymer modification, silicone coupling agent, and functional silicone polymer compounds. The selec...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/08B01J29/12B01J37/34
CPCC07F7/0889B01J29/126B01J37/346Y02P20/584
Inventor 张秀芹陈强贾照丽
Owner CHANGZHOU HIGH TECH RES INST OF NANJING UNIV
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