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A kind of piperazinyl silane compound and its preparation method and application and olefin polymerization method

A siloxane compound and olefin polymerization technology, which is applied in the field of olefin polymerization, can solve problems such as harsh operating conditions, bumping, explosion, etc., and achieve the effects of low product cost, complete reaction, and few by-products

Active Publication Date: 2016-03-30
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The operating conditions of this method are very harsh. If the speed of material addition or temperature control is not good during the reaction, bumping or even explosion will easily occur.

Method used

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  • A kind of piperazinyl silane compound and its preparation method and application and olefin polymerization method
  • A kind of piperazinyl silane compound and its preparation method and application and olefin polymerization method
  • A kind of piperazinyl silane compound and its preparation method and application and olefin polymerization method

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Experimental program
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Effect test

Embodiment approach

[0056] According to a preferred embodiment of the present invention, the preparation method of the piperazinyl silane compound adopts the following steps: 2 Under protective conditions, in an aprotic solvent, add (N-alkyl)piperazine to the reaction flask in sequence, and stir evenly; under the condition of preferably 0-10°C, add n-butyllithium-n-hexane solution dropwise , the n-butyllithium-n-hexane solution is a commercially available reagent; then tetraalkoxysilane or alkyl trialkoxysilane is added dropwise; then the reaction solution is centrifuged and washed with the above aprotic solvent Once, the filtrate was collected, and the above-mentioned aprotic solvent was evaporated with a rotary evaporator, distilled under reduced pressure, and fractions were collected.

[0057] Since the olefin polymerization method provided by the present invention mainly relates to the improvement of the external electron donor compound therein, that is, the above-mentioned piperazinyl silane...

Embodiment 1

[0062] The preparation of embodiment 1 methyl (N-methyl) piperazinyl dimethoxysilane

[0063] in N 2 Under protective conditions, add 2.7g N-methylpiperazine and 30ml n-hexane to the reaction flask in sequence, and stir; at a temperature of 5°C, add 12ml (2.5M) butyllithium-n-hexane solution dropwise, dropwise The addition time is 30min; after the dropwise addition, react at 5°C for 50min, then add 5.54g methyltrimethoxysilane dropwise to the reaction solution, and continue the reaction for 17h after the dropwise addition; centrifuge the reaction solution and filter it, and precipitate Wash twice with n-hexane, and combine the washing liquid with the filtrate; evaporate the n-hexane solvent with a rotary evaporator, distill under reduced pressure, collect the fraction at 73°C / 90Pa, weighing 3.02g, and perform nuclear magnetic resonance test to obtain the following peaks:

[0064] 1 HNMR (CDCl 3 / TMS, 300MHz) δ (ppm): 0.08 (s, 3H, CH 3 ), 2.27 (s+m, 7H, 2NCH 2 , NCH 3 ), ...

Embodiment 2

[0065] The preparation of embodiment 2 isopropyl (N-methyl) piperazinyl dimethoxysilane

[0066] in N 2 Under protective conditions, add 2.7g N-methylpiperazine and 30ml n-hexane to the reaction flask in turn, and stir; at a temperature of 8°C, add 11.3ml (2.5M) butyllithium-n-hexane solution dropwise, drop The addition time is 40min; after the dropwise addition, react at 8°C for 20min, then add 4.63g of isopropyltrimethoxysilane dropwise to the reaction solution, and continue the reaction for 17h after the dropwise addition; centrifuge the reaction solution and filter it, and use it for precipitation Wash twice with n-hexane, and combine the lotion with the filtrate; evaporate the n-hexane solvent with a rotary evaporator, distill under reduced pressure, collect a fraction at 128-130°C / 60Pa, weighing 3.1g, and perform NMR testing to obtain the following peaks:

[0067] 1 HNMR (CDCl 3 / TMS, 300MHz) δ (ppm): 1.03 (m, 7H, CH, 2CH 3 ), 2.27 (s+m, 7H, 2NCH 2 , NCH 3 ), 3.02(...

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Abstract

The invention relates to a piperazinyl silane compound, a preparation method and application of the piperazinyl silane compound and a method for polymerization of olefin, wherein the piperazinyl silane compound has a structure shown in formula (I). When being used as an external electron donor compound of olefin polymerization catalyst, the piperazinyl silane compound prepared by the inventive method can make the catalyst activity high and make isotacticity of the prepared polymer meet the requirement; and the preparation method of the piperazinyl silane compound has the advantages of complete reaction, few byproducts, easy separation of products, low product cost, etc.

Description

technical field [0001] The invention relates to a piperazinyl silane compound, a preparation method and application of the piperazinyl silane compound and an olefin polymerization method. Background technique [0002] It is well known that catalysts for olefin polymerization and copolymerization, especially propylene polymerization catalysts, use silane compounds as external electron donors to increase the isotacticity of the polymer, thereby improving the machinability of the polymer. [0003] The general structural formula of the commonly used silane compounds is: R n Si(OR') 4-n (where n is a natural number of 1-3), such as diphenyldimethoxysilane (WO8805056, EP283011), methylcyclohexyldimethoxysilane (JP02-170803, JP02-229807), diisopropyl Dimethoxysilane (EP350170), diisobutyldimethoxysilane (EP250229, EP376145) and dicyclopentyldimethoxysilane (JP02-229807), etc. [0004] However, some of the above-mentioned known silane compounds contain benzene rings, which may re...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F7/18C07F7/04C08F10/00C08F4/646
Inventor 孙竹芳赵思源谢伦嘉凌永泰田宇冯再兴
Owner CHINA PETROLEUM & CHEM CORP