Norbornene organo-dialkoxysilane compound and preparation method thereof

A technology of base dialkoxy silane and alkenyl trialkoxy silane, applied in norbornenyl organo dialkoxy silane compound and preparation of the compound, in the field of external electron donor, achieving high activity and cost Advantages, the effect of good comprehensive performance

Inactive Publication Date: 2018-04-03
SINOPEC YANGZI PETROCHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] Although the commonly used silane-based external electron donors have been widely used in the production of polypropylene, their comprehensive performance needs to be further improved.

Method used

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  • Norbornene organo-dialkoxysilane compound and preparation method thereof
  • Norbornene organo-dialkoxysilane compound and preparation method thereof
  • Norbornene organo-dialkoxysilane compound and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0045] A Preparation of norbornenyltrimethoxysilane:

[0046] In a 1L stainless steel autoclave equipped with a mechanical stirrer, a thermometer, a nitrogen gas inlet, a feed port, and a liquid sampling port, add 153.8 g of vinyltrimethoxysilane, 80 g of dicyclopentene, and 300 g of methanol, and under stirring, the reaction mass It was heated up to 180°C and kept for 5 hours for reaction. Samples were taken for gas chromatographic analysis to monitor the extent of the reaction. After the reaction is completed, the solvent, unreacted raw materials such as cyclopentadiene, dicyclopentadiene, vinyltrimethoxysilane, etc. are distilled off at normal pressure, and then collected by distillation at -0.098MPa under reduced pressure at 135-156°C The distillate product is 230 grams, and the yield is 75% (based on vinyltrimethoxysilane). The reaction process can be represented by reaction formula 1:

[0047] Reaction 1

[0048]

[0049] B preparation of norbornenyltrimethoxysila...

Embodiment 2

[0052] Preparation of norbornenylcyclopentyldimethoxysilane

[0053] Replace the air with nitrogen in a 500mL dry four-necked flask equipped with an electric stirrer, a thermometer, a reflux condenser, and a constant pressure dropping funnel, and drop 12.1g (purity 99%, 0.5mol) into the reaction flask under a nitrogen atmosphere. Magnesium powder less than 100 meshes, 2.7g (purity 99%, 0.026mol) chlorocyclopentane, 20ml methyl tert-butyl ether. Add a mixed solution of 51.2g (0.49mol) cyclopentane chloride and 100ml methyl tert-butyl ether into the constant pressure dropping funnel. Add a small amount of initiator iodine to the contents of the reaction vial. After the reaction is initiated, stir. When the exothermic reaction is stable, add the mixture in the dropping funnel dropwise to the reaction flask within 30-60 minutes, and control the reaction temperature so that the solvent is in a reflux state; the mixture of chlorocyclopentane and methyl tert-butyl ether After comp...

Embodiment 3

[0060] Preparation of norbornyl isobutyldimethoxysilane

[0061] According to the conditions of Example 2, the chlorocyclopentane was replaced by an equimolar chloroisobutane; after the reaction was completed, the solvent was recovered by filtration, washing, normal pressure and the previous fraction was evaporated, and finally the vacuum distillation was collected at 118-120°C / -0.098MPa fraction. 80 g of norbornyl isobutyldimethoxysilane was obtained with a purity of 98% and a yield of 72% (calculated as norbornyl trimethoxysilane). The reaction process is represented by reaction formula 3:

[0062] Reaction 3

[0063]

[0064] The hydrogen spectrum result of norbornenyl isobutyl dimethoxysilane compound is:

[0065] 1 H NMR (600MHz, CDCl 3 )δ6.28–5.84(m,2H),3.68–3.42(m,6H),3.13–2.80(m,2H),2.31–1.07(m,6H),0.99(ddd,J=18.1,7.8,3.2 Hz,6H), 0.72–0.52(m,2H).

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Abstract

The invention discloses a norbornene organo-dialkoxysilane compound and a preparation method thereof. The norbornene organo-dialkoxysilane compound has a general formula (I), wherein R<1> is alkyl containing 1-5 carbon atoms; R<2> is branched alkyl with 3-10 carbon atoms on alpha or beta secondary carbon atoms connected with silicon atoms. The compound can be used as an external electron donor ofa propylene polymerization Ziegler-Natta catalyst system, can have better comprehensive performance as the external electron donor and can maintain the high activity of a catalyst and improve the hydrogen sensitivity of the catalyst as compared with existing external electron donors.

Description

technical field [0001] The invention belongs to the field of organic chemistry, and further relates to a norbornene-based organodialkoxysilane compound and a preparation method of the compound. The compound can be used as an external electron donor of a propylene polymerization Ziegler-Natta catalyst system. Background technique [0002] At present, the catalysts used in the industrial production of polypropylene are mainly MgCl containing diester internal electron donors. 2 Supported Ziegler-Natta catalyst. Ziegler-Natta catalyst is equipped with cocatalyst aluminum alkyl and external electron donor during the polymerization of propylene. Usually, the compounds used as external electron donors are mainly diorganodioxyl silanes, and particularly favorable organic substituents are bulky branched-chain-containing organic groups or ring-containing organic groups, which are particularly advantageous The alkoxy group is a smaller methoxy or ethoxy group. In addition to adjusti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F7/18C08F10/06C08F4/649
Inventor 高以龙缪军李娜孙海龙杨爱武
Owner SINOPEC YANGZI PETROCHEM
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