Method for preparing high cis-polyisoprene through utilizing gas phase polymerization, and catalyst

A polyisoprene, gas-phase polymerization technology, applied in the field of gas-phase polymerization of high cis-1,4-polyisoprene, can solve problems affecting rubber processing and application performance

Active Publication Date: 2013-06-05
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

Method used

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  • Method for preparing high cis-polyisoprene through utilizing gas phase polymerization, and catalyst
  • Method for preparing high cis-polyisoprene through utilizing gas phase polymerization, and catalyst
  • Method for preparing high cis-polyisoprene through utilizing gas phase polymerization, and catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] (1) Catalyst preparation

[0033] The catalyst consists of Nd(naph) 3 、Al(i-Bu) 3 , AlEtCl 2 , silica with a particle size in the range of 10-250 μm, and nano-particle carbon black with a particle size in the range of 5-300 nm. The solvent used in the catalyst preparation process is n-hexane, of which the first component Nd (naph) 3 The amount is 1.2mmol, the second component Al(i-Bu) 3 The amount is 96mmol, the third component AlEtCl 2 The amount of is 7.2mmol, and the amount of the fourth component silicon dioxide is 1.2g, and the amount of the fifth component carbon black is 2.4g, makes powdery catalyst A 1 10.31g.

[0034] (2) Isoprene gas phase polymerization process

[0035] In the purified stirred reactor, add the powder catalyst A prepared above under the protection of nitrogen 1 10.31 g, evacuated nitrogen, started stirring, introduced isoprene gas, reacted at 70°C for 1 hour under 0.1 MPa pressure, and dried after post-treatment to obtain 2399.2 g...

Embodiment 2

[0043] (1) Catalyst preparation

[0044] The catalyst consists of Nd(OiPr) 3 、Al(i-Bu) 3 、Al 2 Et 3 Cl 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 toluene, wherein the first component Nd(OiPr ) 3 The amount is 1.0mmol, the second component Al(i-Bu) 3 The amount is 30.0mmol, the third component Al 2 Et 3 Cl 3 The amount of is 1.0mmol, the amount of the fourth component magnesium chloride is 50.0g, the amount of the fifth component silicon dioxide is 50.0g, and the powdery catalyst B is prepared 1 107.2g.

[0045] (2) Isoprene gas phase polymerization process

[0046] In the purified stirred reactor, add the powder catalyst B prepared above under the protection of nitrogen 1 107.2g, evacuated nitrogen, started stirring, introduced isoprene gas, under 0.1MPa pressure, reacted at 60°C for 1 hour, after post-treatment and...

Embodiment 3

[0054] (1) Catalyst preparation

[0055] The catalyst consists of Nd(P 204 ) 3 、Al(Me) 2 H, Al 2 Et 3 Cl 3 , Alumina with a particle size range of 10-250 μm

[0056] It consists of five components such as nanoparticle talc powder with a particle size range of 5-300nm. The solvent used in the catalyst preparation process is toluene, wherein the first component Nd(P 204 ) 3 The amount is 1.0mmol, the second component Al(Me) 2 The amount of H is 100.0mmol, the third component Al 2 Et 3 Cl 3 The amount of is 8.0mmol, the amount of the fourth component alumina is 20.5g, the amount of the fifth component talcum powder is 72.4g, and the obtained powdery catalyst C 1 102.3 g.

[0057] (2) Isoprene gas phase polymerization process

[0058] In the purified stirred reactor, add the powder catalyst C prepared above under the protection of nitrogen. 1 102.3g, evacuate nitrogen, start stirring, feed isoprene gas, react at 50°C for 1 hour under 0.1MPa pressure, and dry after ...

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Abstract

The invention discloses a method for preparing high cis-polyisoprene through utilizing gas phase polymerization, and a catalyst. The catalyst is composed of five components comprising a first component, a second component, a third component, a fourth component and a fifth component, wherein the first component is a rare earth compound; the second component is anyone of aluminum alkyl, aluminum alkyl hydroxide and alkyl aluminoxane; the third component is anyone of alkyl chloride or aluminum alkyl chloride; the fourth component is magnesium chloride, silica, carbon black or alumina; the fifth component is anyone or a mixture containing several of nanometer silica, nanometer carbon black, nanometer alumina, nanometer titanium dioxde, nanometer antimonony oxide, nanometer calcium carbonate, nanometer talcum powder and nanometer montmorillonite; and the molar ratio of the first component to the second component is 1:20-100, the molar ratio of the first component to the third component is 1:1-10, the ratio of the mole of the first component to the mass of the fourth component is 1:2000-200000, and the mass ratio of the fifth component to the fourth component is 1:0.125-200. High cis-polyisoprene rubber particles are obtained through the gas phase polymerization of isoprene and the catalyst at 40-70DEG C for above 30min.

Description

technical field [0001] The invention relates to a gas-phase polymerization method of high cis-1,4-polyisoprene and a preparation method of a catalyst thereof. Background technique [0002] Rare earth catalysts are highly efficient catalysts for the synthesis of highly stereoregular rubbers. Isoprene can undergo directional polymerization under the action of rare earth catalysts to synthesize high cis-1,4-polyisoprene. Rare earth catalysts usually consist of a main catalyst rare earth salt (or rare earth alcoholate), a cocatalyst and a third component that can release halogen atoms. Wherein, the cocatalyst can be any one of alkylaluminum, alkylaluminum hydride and alkoxyaluminum. The third component that can release halogen atoms can be any one of halogenated alkanes and alkylaluminum chlorides. The existing domestic and foreign production processes of high cis-1,4-polyisoprene are solution polymerization. The polymer, isoprene and catalyst system in this process are all ...

Claims

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Application Information

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IPC IPC(8): C08F136/08C08F4/58C08F4/54C08F4/52C08F2/34
Inventor 曹堃姚臻倪旭峰付强张景屠宇侠
Owner ZHEJIANG UNIV
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