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Method and catalyst for preparing high trans-polyisoprene by adopting gaseous phase polymerization

A technology of polyisoprene and gas phase polymerization, which is applied in the field of gas phase polymerization and its catalyst preparation, and 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

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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 and catalyst for preparing high trans-polyisoprene by adopting gaseous phase polymerization
  • Method and catalyst for preparing high trans-polyisoprene by adopting gaseous phase polymerization

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 is 3.6mmol, the mass of the third component silicon dioxide is 2.4g, and the mass of the fourth component carbon black is 2.4g. After stirring evenly, the solvent is removed, and finally 5.4g of powdered catalyst A is obtained 1 .

[0032] (2) Isoprene gas phase polymerization process

[0033] In the purified stirred reactor, add the 5.4g powder catalyst A prepared above under nitrogen protection 1 , evacuate nitrogen, start stirring, feed isoprene gas, react under 0.1MPa pressure, 70°C for 1 hour, and dry after post-treatment to obtain 2400g of polymer product. C...

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 20.7g.

[0043] (2) Isoprene 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, evacuated nitrogen, started stirring, introduced isoprene gas, reacted at 70°C for 1 hour under 0.1MPa pressure, and dried after post-treatment to obtain 1501.3g of polymer prod...

Embodiment 3

[0052] (1) Preparation of catalyst

[0053] The catalyst consists of TiCl 4 , AlEt 3 , magnesium chloride with a particle size range of 10-250 μm, and nano-particle silicon dioxide with a particle size range of 5-300 nm. The solvent used in the catalyst preparation process is n-heptane, the first component TiCl 4 The amount is 1.0mmol, the second component AlEt 3 The amount of 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) Isoprene 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, evacuated nitrogen, started stirring, introduced isoprene gas, reacted at 60°C for 1 hour under 0.1MPa pressure, and dried after post-treatment to obtain 1251...

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Abstract

The invention discloses a method and a catalyst for preparing high trans-polyisoprene by adopting gaseous phase polymerization. The catalyst comprises the following components: a first component, namely a compound of transition metal vanadium or titanium, a second component, namely a catalyst promoter, a third component, namely a carrier, and a fourth component, namely nano inorganic particles. In the catalyst, the mole ratio of the first component to the second component is 1:2-10, ratio of the molar weight of the first component to the mass of the third component is 1mol:2000-200000g, and the mass ratio of the fourth component to the third component is 1:0.125-200. The catalyst has high catalytic activity, the catalyst and gaseous phase polymerization are adopted for preparing polyisoprene, an inorganic-organic alloy containing the third component and the fourth component is generated in situ in a reactor, an anti-sticking effect which can not be realized by the existing method is still achieved under the condition that content of nano inorganic particles is as low as 0.1wt%, adhesion of rubber is effectively prevented, and perfect rubber particles are obtained.

Description

technical field [0001] The invention relates to a gas phase polymerization of high trans-1,4-polyisoprene 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. Isoprene can undergo directional polymerization under the action of vanadium and titanium catalysts to synthesize high trans-1,4-polyisoprene. 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-polyisoprene 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 is h...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F136/08C08F2/34C08F4/68C08F4/685C08F4/646
Inventor 倪旭峰姚臻曹堃张景屠宇侠付强
Owner ZHEJIANG UNIV
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