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Bulk depositing synthesis process of isotactic polybutylene-1

A technology of isotactic polybutene and bulk precipitation, which is applied in the innovative field of bulk precipitation synthesis method, can solve the problems of mass transfer, heat transfer difficulty, system stickiness, production efficiency reduction, etc., and achieves wide popularization and application, simple process, low cost effect

Active Publication Date: 2009-05-20
SHANDONG ORIENT HONGYE CHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, when the polymerization temperature is higher than 30°C, polybutene-1 will swell in its monomer, which will make the system sticky and cause difficulties in mass transfer and heat transfer, which limits the polymerization process to low conversion rates. Terminate or use reactive extrusion technology to further increase conversion and remove unreacted monomers
In this way, the production efficiency is reduced, while the complexity of the production process and the production cost increase
[0007] At present, there are many domestic reports on butene-1 polymers, but they are all limited to scientific research, and there are no reports on real industrialization.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Example 1. A bulk precipitation synthesis method of highly isotactic polybutene-1.

[0026] 3L fully enclosed magnetic stirring stainless steel pressure polymerization kettle (double-helical stirring paddle), pumping for 2 to 3 hours, during which it was replaced several times with high-purity nitrogen. 560g of monomer Bt was added to the reactor, with Ti / Bt=8×10 -6 (molar ratio, the same below), Al / Ti=400 (molar ratio, the same below), DDS / Ti=0 (molar ratio, the same below), under stirring, add triisobutylaluminum (Al), externally The electron body and the supported titanium catalyst (Ti) were polymerized at 50° C. for 3 hours, and after the drying was terminated, 425 g of powdered polymer polybutene was directly obtained, the monomer conversion rate was 76%, and the catalytic efficiency was 147,569 g polymer / g Ti. The content of insoluble matter obtained by extraction with diethyl ether was 80%, that is, the content of isotactic polybutene-1 was 80%.

Embodiment 2

[0027]Example 2. A bulk precipitation synthesis method of highly isotactic polybutene-1.

[0028] The experimental procedure is the same as in Example 1. Take DDS / Ti=0.3 (molar ratio, the same below), add triisobutylaluminum (Al), external electron donor and supported titanium catalyst (Ti) sequentially under stirring, polymerize at 50°C for 3 hours, and stop drying 400 g of powdery polymer polybutene was obtained directly, the monomer conversion rate was 71%, and the catalytic efficiency was 138800 g polymer / gTi. The content of insoluble matter obtained by extraction with diethyl ether was 96%, that is, the content of isotactic polybutene-1 was 96%.

Embodiment 3

[0029] Example 3. A bulk precipitation synthesis method of highly isotactic polybutene-1.

[0030] The experimental procedure is the same as in Example 2. Under stirring, triisobutylaluminum (Al), external electron donor and supported titanium catalyst (Ti) were successively metered in, and polymerized at 50° C. for 3 hr. During the reaction, the hydrogen partial pressure was maintained at 0.1 MPa. After the drying was terminated, 520 g of powdery polymer polybutene was directly obtained, the monomer conversion rate was 93%, and the catalytic efficiency was 180440 g polymer / gTi. The content of insoluble matter obtained by extraction with diethyl ether was 95%, that is, the content of isotactic polybutene-1 was 95%.

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Abstract

The invention discloses a bulk precipitation synthesis method of high isotactic polybutene-1, which belongs to high molecular polymer technology. It uses butene-1 as monomer and reaction medium, under the condition of reaction temperature of 0-70 ℃, adopts supported titanium catalyst to catalyze butene-1, and synthesizes powdery polybutene-1 polymerization by bulk precipitation polymerization The unpolymerized monomers are removed and re-polymerized by flash evaporation to obtain a powdery granular product of high isotactic polybutene-1. It can adopt organometallic aluminum AlR 3 As a cocatalyst, an external electron donor compound can be added to the catalyst system, and hydrogen can also be added as a molecular mass regulator. The polymerization process is carried out in a polymerization tank with ribbon stirring. It has simple process, high efficiency and low cost. The prepared high stereoregular polybutene-1 polymer with an isotactic content of more than 98% has a crystallinity of more than 60% and a melting point of 127.5°C, which is completely close to similar foreign products. Can be widely promoted and applied.

Description

technical field [0001] The invention belongs to the technical field of high molecular polymers, and more specifically relates to the innovation of the bulk precipitation synthesis method of high isotactic polybutene-1. Background technique [0002] Stereoregular polybutene polymer is a semi-crystalline polymer composed of butene-1 as a monomer, which naturally has physical properties similar to polyethylene and polypropylene polymers. [0003] The properties of stereoregular polybutene-1 include high flexibility, high crystallinity, outstanding creep resistance and tensile strength at high temperature. Its applicable temperature ranges from -20°C to 105°C, and it can be used for hot and cold water pipes, packaging films, and film films. [0004] The traditional preparation methods of stereoregular polybutene-1 include gas-phase and liquid-phase methods. The gas phase method is usually carried out using a gas phase ebullating bed process. U.S. Patents 4,503,203, 5,241,024,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F110/08C08F2/02C08F4/642
Inventor 黄宝琛郑保永姚薇马少勇邵华锋崔颜英赵永仙王国华
Owner SHANDONG ORIENT HONGYE CHEM
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