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Method and catalyst for preparing high cis-polybutadiene by gas-phase polymerization

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

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 cis-polybutadiene by gas-phase polymerization
  • Method and catalyst for preparing high cis-polybutadiene by gas-phase polymerization
  • Method and catalyst for preparing high cis-polybutadiene by gas-phase polymerization

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] (1) Catalyst preparation

[0031] 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 4.8g, and the amount of the fifth component carbon black is 2.9g, makes powdery catalyst A 1 16.81g.

[0032] (2) Butadiene gas phase polymerization process

[0033] In the purified stirred reactor, add the powder catalyst A prepared above under the protection of nitrogen 1 16.81g, 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 2879.1g of polymer p...

Embodiment 2

[0041] (1) Catalyst preparation

[0042] 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 1 107.2 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 1 107.2g, evacuate nitrogen, start stirring, feed butadiene gas, under 0.1MPa pressure, react at 60°C for 1 hour, and dry after post-treatment to...

Embodiment 3

[0052] (1) Catalyst preparation

[0053] 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

[0054] 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 1 102.3g.

[0055] (2) Butadiene gas phase polymerization process

[0056] 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 butadiene gas, under 0.1MPa pressure, react at 50°C for 1 hour, and dry afte...

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Abstract

The invention discloses a method and catalyst for preparing high cis-polybutadiene by gas-phase polymerization. The catalyst is mixed by five components, wherein the first component is a rare-earth compound; the second component is alkyl aluminum, alkyl aluminium hydride or alkylaluminoxane; the third component is alkyl chloride or alkyl aluminum chloride; the fourth component is magnesium chloride, silicon dioxide, carbon black or aluminum oxide; the fifth component is any one or combination of more of nano silicon dioxide, nano carbon black, nano aluminum oxide, nano titanium dioxide, nano antimony trioxide, nano calcium carbonate, nano talcum powder and nano montmorillonite; and the mol ratio of the first component to the second component is 1:(20-100), the mol ratio of the first component to the third component is 1:(1-10), the ratio of the molar weight 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 is 1:(0.125-200). Butadiene and a catalyst are subjected to gas-phase polymerization reaction at 40-70 DEG C for more than 30 minutes to obtain the high cis-1,4-polybutadiene rubber particles.

Description

technical field [0001] The invention relates to a gas phase polymerization method of high cis-1,4-polybutadiene 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. Butadiene can undergo directional polymerization under the action of rare earth catalysts to synthesize high cis-1,4-polybutadiene. 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-polybutadiene are solution polymerization. The polymer, butadiene and catalyst system in this process are...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F236/06C08F4/58C08F4/54
Inventor 姚臻倪旭峰曹堃屠宇侠张景
Owner ZHEJIANG UNIV
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