Gas-phase polymerization method and polymer of polybutene-1

A gas-phase polymerization and butene technology, applied in the field of regular polymers, can solve the problems of difficult mass transfer and heat transfer, unsatisfactory polymer performance, and sticky system.

Inactive Publication Date: 2011-05-04
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Adopting the method of gas phase polymerization after the bulk prepolymerization of the liquid phase, although the isotacticity has been improved to 95%, and the activity reaches 14000g / gcat·4h, but because the ash content of the obtained polymer is relatively high, the isotacticity and polymerization Indicators such as activity are not ideal enough, so the performance of the obtained polymer is also unsatisfactory
[0007] From the technical development of olefin polymers, generally speaking, the performance of copolymer products containing a certain amount of comonomer is better than that of homopolymer products. Due to the limitation of the current catalyst level, it is often difficult to control the polymerization by liquid phase method. , when the polymerization temperature is slightly higher, the polybutene-1 copolymer resin is easy to swell in its monomer or solvent, which makes the system sticky and makes mass and heat transfer difficult, which limits the conversion rate in the polymerization process, so the production Reduced efficiency while increasing the complexity of the production process and production costs

Method used

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  • Gas-phase polymerization method and polymer of polybutene-1
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  • Gas-phase polymerization method and polymer of polybutene-1

Examples

Experimental program
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Effect test

Embodiment 1

[0054] Preparation of solid component (A) in the catalyst system

[0055] In the reactor fully replaced by high-purity nitrogen, magnesium chloride (0.05mol) 4.8g, toluene 75ml, epichlorohydrin (ECP) 7.8ml (0.1mol), tributyl phosphate (TBP) 8.2ml (0.03 mol), heated to 50°C with stirring, and maintained for 2.5 hours. After the solid was completely dissolved, 1.2 g of phthalic anhydride was added and maintained for 1 hour. The solution was cooled to below -25°C, and TiCl was added dropwise within one hour. 4 56ml, slowly heated up to 80°C, and gradually precipitated solids, added 2.7ml of diisobutyl phthalate (DIBP), and maintained at 80°C for 1 hour, after hot filtration, added 100ml of toluene, washed twice, and obtained brown yellow solid. Add 60ml of toluene, TiCl 440ml, treated at 90°C for 2 hours, and repeated treatment once. Add 100 ml of toluene, raise the temperature to 110° C., repeat washing three times for 10 minutes each, then add 100 ml of hexane, and repeat wa...

Embodiment 2

[0058] Bulk Polymerization of Butene-1 in Gas Phase

[0059] The catalyst prepared in Example 1, triisobutylaluminum (TIBA) and diphenyldimethoxysilane (DDS) are 200 according to the Al / Ti molar ratio, and the ratio of Si / Ti molar ratio is 8 at room temperature Mix and add to activation vessel with a small amount of isopentane, residence time is about 10 minutes. The catalytic system was added to the treated gas-phase fluidized bed polymerization reactor, and the operating conditions were as follows: temperature 75°C, pressure 1.5MPa, polymerization reaction time 3 hours, butene-1 gas phase composition 30mol%, nitrogen gas phase composition 69.7 mol%, hydrogen gas phase composition 0.3 mol%.

[0060] Polymer test: polymer melt index MI is 0.38g / 10min, polymer isotactic index (mmmm%) 98.2%, MWD=7.4, polymer is the sub-spherical particle of particle diameter 1-4mm, catalyst efficiency 1.6 kgPB / gcat, the catalyst ash content in the polymer expressed in ppm titanium is 1.8.

Embodiment 3

[0062] Bulk Polymerization of Butene-1 in Gas Phase

[0063] The catalyst prepared in Example 1, triethylaluminum (TIBA) and diisopropyldimethoxysilane (DIPMS) are 100 according to the Al / Ti molar ratio, and the ratio of Si / Ti molar ratio is 4, at room temperature Mix and add to activation vessel with a small amount of isopentane, residence time is about 10 minutes. The catalytic system was added to the treated gas-phase fluidized bed polymerization reactor, and the operating conditions were as follows: temperature 75°C, pressure 1.5MPa, polymerization reaction time 3 hours, butene-1 gas phase composition 30mol%, nitrogen gas phase composition 69.4 mol%, hydrogen gas phase composition 0.6 mol%.

[0064] Polymer test: polymer melt index MI is 0.94g / 10min, polymer isotactic index (mmmm%) 96.7%, MWD=8.3, polymer is the sub-spherical particle of particle diameter 1-4mm, catalyst efficiency 0.9 kgPB / gcat, the catalyst ash content in the polymer, expressed in ppm titanium is 3.5. ...

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Abstract

The invention provides a gas-phase polymerization method of polybutene-1 for preparing high-quality butene-1 polymer, which comprises: performing homopolymerization of butene-1 serving as a monomer and a reaction medium or copolymerization of butene-1 and other alpha-olefins in a gas-phase polymerization reactor at a reaction temperature of 0 to 110 DEG C in the presence of a Ziegler-Natta catalyst with high stereoselectivity, and standing for 1 to 6 hours optimally. The method is simple in process, easy in operation and low in cost. The prepared polybutene-1 product is sphere-like or spherical particles and contains little fine powder, thereby contributing to the long-term operation o devices.

Description

technical field [0001] The invention relates to a gas-phase polymerization method of polybutene-1, and the resulting polymer with high isotacticity. technical background [0002] Isotactic polybutene-1 has good mechanical properties, outstanding creep resistance, low temperature flow resistance and environmental stress cracking resistance, and has wear resistance, flexibility and high filler filling. Compared with other polyolefins, polybutene-1 has the best stress crack resistance and significantly higher creep resistance than polyethylene or polypropylene. Especially under the stress that does not exceed the yield point, its outstanding creep resistance can remain unchanged up to 110 °C. Moreover, isotactic polybutene-1 still shows good mechanical properties under heated conditions, and its heat resistance allows it to be used for a long time at 80-90°C, and the upper limit of the use temperature in hot water is It can reach 110°C, and its wear resistance can be compared...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F10/08C08F2/34C08F4/645C08F4/654
Inventor 王世波周俊领高克京刘东兵吕新平毛炳权邢宝泉王丽莎
Owner CHINA PETROLEUM & CHEM CORP
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