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Method for preparing high transpolybutadiene by utilizing gas-phase polymerization and catalyst used in method

A gas-phase polymerization and polybutadiene technology, which is applied in the field of gas-phase polymerization and its catalyst preparation, can solve problems affecting rubber processing and application performance, etc.

Active Publication Date: 2014-12-31
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Therefore, although this method has a certain anti-sticking effect, it is necessary to introduce a large amount of inorganic particles to obtain granular rubber, which affects the processing and application performance of rubber.

Method used

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  • Method for preparing high transpolybutadiene by utilizing gas-phase polymerization and catalyst used in method
  • Method for preparing high transpolybutadiene by utilizing gas-phase polymerization and catalyst used in method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] (1) Preparation of catalyst

[0031] The catalyst consists of VCl 3 , AlEt 3 It is composed of four components, including silicon dioxide with a particle size range of 10-250 μm and nano-particle carbon black with a particle size range of 5-300 nm. The solvent used in the catalyst preparation process is n-hexane, the first component VCl 3 The amount is 1.2mmol, the second component AlEt 3 The amount of carbon black is 3.6mmol, the amount of the third component silicon dioxide is 4.8g, and the amount of the fourth component carbon black is 2.9g. After stirring evenly, the solvent was removed, and finally 8.3g of powdered catalyst A was obtained 1 .

[0032] (2) Butadiene gas phase polymerization process

[0033] In the purified stirred reactor, add the 8.3g powder catalyst A prepared above under the protection of nitrogen 1 , evacuate nitrogen, start stirring, feed butadiene gas, react under 0.1MPa pressure, 70°C for 1 hour, and dry after post-treatment to obtain ...

Embodiment 2

[0041] (1) Preparation of catalyst

[0042] The catalyst consists of VOCl 3 , AlEt 3 , carbon black with a particle size range of 10-250 μm, and nano-particle titanium dioxide with a particle size range of 5-300 nm. The solvent used in the catalyst preparation process is toluene, the first component VOCl 3 The amount is 1.0mmol, the second component AlEt 3 The amount of carbon black is 5.0mmol, the amount of the third component carbon black is 10.0g, and the amount of the fourth component titanium dioxide is 10.0g. After stirring evenly, the solvent is removed, and the powdered catalyst B is finally obtained. 1 20.7 g.

[0043] (2) Butadiene gas phase polymerization process

[0044] In the purified stirred reactor, add the powder catalyst B prepared above under the protection of nitrogen 1 20.7g, evacuate nitrogen, start stirring, feed butadiene gas, react at 70°C for 1 hour under 0.1MPa pressure, and dry after post-treatment to obtain 1801.6g of polymer product. Cata...

Embodiment 3

[0052] (1) Catalyst preparation

[0053] The catalyst consists of TiCl 4 , AlEt 3 , magnesium chloride with a particle size range of 10-250 μm, and nano-particle silica with a particle size range of 5-300 nm. The solvent used in the catalyst preparation process is n-heptane, of which the first component TiCl 4 The amount is 1.0mmol, the second component AlEt 3 The amount of the magnesium chloride is 10.0mmol, the amount of the third component magnesium chloride is 25.0g, and the amount of the fourth component silicon dioxide is 50.0g. After stirring evenly, the solvent is removed, and the powdery catalyst C is finally obtained. 1 76.3g.

[0054] (2) Butadiene gas phase polymerization process

[0055] In the purified stirred reactor, add the powder catalyst C prepared above under the protection of nitrogen. 1 76.3g, evacuate nitrogen, start stirring, feed butadiene gas, react at 60°C for 1 hour under 0.1MPa pressure, and dry after post-treatment to obtain 1501.4g of polym...

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Abstract

The invention discloses a method for preparing high transpolybutadiene by utilizing gas-phase polymerization and a catalyst used in the method. The catalyst comprises the following components: a first component which is a compound of transition metal vanadium or titanium, a second component which is a catalyst promoter, a third component which is a carrier and a fourth component which is nanometer inorganic particle. In the catalyst, the molar ratio of the first component to the second component is 1:(2-10); the ratio of the molar weight of the first component to the weight of the third component is 1mol:(2000g-200000g); the weight ratio of the fourth component to the third component is 1:(0.125-200). The catalyst disclosed by the invention is high in catalytic activity. The catalyst is used for preparing polybutadiene by adopting gas-phase polymerization, and an inorganic-organic alloy containing the third component and the fourth component in a reactor is generated in situ by using polybutadiene, so that an anti-sticking effect which cannot be realized by the existing method can be still realized when the content of inorganic nanometer particles is lower than 0.1wt%, and therefore, the sticking of rubber is effectively prevented and ideal rubber particles are obtained.

Description

technical field [0001] The invention relates to a gas phase polymerization of high trans-1,4-polybutadiene and a preparation method of a catalyst thereof. Background technique [0002] Vanadium or titanium catalysts are efficient catalysts for the synthesis of highly stereoregular rubber. Butadiene can undergo directional polymerization under the action of vanadium and titanium catalysts to synthesize high trans-1,4-polybutadiene. Vanadium and titanium catalysts are usually composed of the compound of transition metal vanadium or titanium as the main catalyst and the co-catalyst. The co-catalyst can be an aluminum alkyl, and its main function is to reduce the main catalyst to a polymerization active state. [0003] Most of the existing domestic and foreign production processes for high trans-1,4-polybutadiene are solution polymerization. In this process, the polymer, monomer and catalyst system are all dissolved in solvents such as n-hexane, etc., and the reaction system ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F136/06C08F4/68C08F4/646C08F2/34
Inventor 姚臻倪旭峰曹堃屠宇侠张景
Owner ZHEJIANG UNIV
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