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Industrial production method of high isotactic polybutylene and device for implementing method

A technology of high tactic polybutene and production method, applied in the field of tactic polybutene, can solve the problems of mass transfer, heat transfer difficulty, harm to workers, low monomer concentration and partial pressure, etc.

Active Publication Date: 2014-07-02
SHANDONG ORIENT HONGYE CHEM +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The biggest disadvantage of gas-phase polymerization is: low monomer concentration and partial pressure (inert gas with a boiling point lower than butene monomer often exists in gas-phase polymerization, which is used to reduce and avoid polymer bonding and to be brought by the volatilization of inert low-boiling gas. take the heat of polymerization), the polymerization rate is relatively low; the requirements for the polymerization process, polymerization device and process operation are very high, usually only large-scale enterprises can realize it, and it is not suitable for general small and medium-sized enterprises, especially some small-sized polypropylene devices for transformation. ene polymerization
In solution polymerization, polybutene swells and dissolves in its monomers, which makes the system sticky, resulting in difficulties in mass transfer and heat transfer, which limits the polymerization process to be terminated at low conversion rates or to use reactive extrusion Technology to further increase the conversion rate and remove unreacted monomers
In this way, the production efficiency is reduced, while the complexity of the production process and the production cost increase
Chinese invention patent 200710013587.X prepared polybutene with high identity by bulk precipitation method, which overcomes the shortcomings of solvent recovery and post-treatment in solution method, but this patent only covers the synthesis method of polybutene by bulk precipitation polymerization and the material itself It is protected and does not involve the production method, process flow and implementation equipment of industrial production; in the preparation method disclosed in this patent, the monomers that do not participate in the polymerization reaction are recovered through a flash evaporation, and the monomer recovery is incomplete, resulting in waste; The patent only mentions supported TiCl prepared by milling method 4 The main catalyst; the patent does not mention the post-treatment of the polymer. During the polymer packaging process, if the polymerization system is opened, the residual monomers in the polymer that are not fully recovered will volatilize and leak in the polymerization workshop. If it is higher, there will be a potential explosion hazard, which will not only affect the production and equipment, but also endanger the staff; this patent has not considered the potential risk that the recycled monomer cannot enter the polymerization system in case of emergency failure At the same time, the patent does not mention the purification of recovered monomers. Inert impurities and reactive impurities in recovered monomers are introduced into the polymerization system, which will seriously affect the normal implementation of polymerization production, reduce production efficiency, and reduce product quality.

Method used

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  • Industrial production method of high isotactic polybutylene and device for implementing method
  • Industrial production method of high isotactic polybutylene and device for implementing method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] After the 12 cubic meter polymerization kettle was treated by the vacuum nitrogen system, 3.4 tons of purified butene monomer was introduced into the polymerization kettle through the batching system at one time, and 2.8kg of triethylaluminum was added in sequence, and the external electron donor diphenyl dimethyl Oxysilane 0.3kg, MgCl 2 Loaded TiCl 4 Catalyst (titanium loading: 3.2wt.%) 0.36kg, add hydrogen 5MPa as a molecular weight regulator through the gas distribution system, raise the temperature of the polymerization tank to 50°C through the utility system and react under this condition for 3h. After the reaction is over, the polymerization tank is decompressed, and part of the unreacted monomer is flashed off, and then enters the butene gas holder. Then transfer the polybutene to the flash tank to continue the further flash evaporation of the monomer. After the combustible gas is detected and there is no monomer residue, a certain amount of nitrogen is introduc...

Embodiment 2

[0052] In addition to the cocatalyst being 2.8kg of diethylaluminum chloride, the external electron donor being 0.3kg of methyltriethoxysilane, and the main catalyst being MgCl 2 Load VCl 4 Catalyst (2.5wt.% vanadium load) 0.36kg, polymerization time 4 hours, other parameters and polymerization process steps are the same as in Example 1. The weight of the synthesized polymer is 3.04 tons, and the conversion rate is about 89.4%. The bulk density of polybutene is 367kg / m 3 , The melt flow rate is 0.53g / 10min, the tested polybutene isotacticity is 96.8%, and the ash content is less than 100ppm. After two flashes, 345kg of monomers were recovered, and the monomer loss per ton of polymer was calculated to be only 4.9kg. The polymerization parameters and product physical parameters are shown in Table 1.

Embodiment 3

[0054] After the 12 cubic meter polymerization kettle was treated by the vacuum nitrogen system, 3.4 tons of butene monomer was introduced into the polymerization kettle through the batching system at one time, and after the temperature of the polymerization kettle was raised to 60°C through the public engineering system, triisobutyl Aluminum 2.0kg, external electron donor cyclohexylmethyldimethoxysilane 0.2kg, MgCl 2 Loaded TiCl 4 Catalyst (titanium loading: 3.2wt.%) 0.2kg, add hydrogen 3MPa as a molecular weight regulator through the gas distribution system. React under these conditions for 6h. After the reaction is over, the polymerization tank is decompressed, and part of the unreacted monomer is flashed off, and then enters the butene gas holder. Then transfer the polybutene to the flash tank to continue the further flash evaporation of the monomer. After the combustible gas is detected and there is no monomer residue, a certain amount of nitrogen is replaced in the fla...

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Abstract

The invention discloses an industrial production method of high isotactic polybutylene and a device for implementing the method. The production method comprises the process flows of carrying out bulk polymerization on a liquid-phase butylene-1 monomer in a polymerization kettle at the temperature of 10 DEG C below zero to 70 DEG C above zero to synthesize isotactic polybutylene, and recovering part of unreacted butylene-1 into a butylene gasometer through primary pressure reduction after polymerizing for a certain period of time; then, transferring high isotactic polybutylene from the polymerization kettle to a flash distillation kettle, carrying out reduced-pressure flash distillation, and further recovering the unreacted butylene-1 monomer into the butylene gasometer; sequentially introducing nitrogen gas and air into the flash distillation kettle to replace, discharging a granular high isotactic polybutylene product through an emptying valve at the bottom of the kettle, and packaging. The device comprises a proportioning system, a polymerization system, a gas distribution system, a vacuum nitrogen system, a degassing and flash distillation system and a utility system. Through the industrial production method and the device, the industrial synthesis of the high isotactic polybutylene can be realized, and no organic solvents, waste gases, waste water and waste residues are discharged; in addition, the industrial production method belongs to a green and clean production process.

Description

technical field [0001] The present invention relates to the field of petrochemical industry, in particular to a method for producing high isotactic polybutene, and more specifically to an industrial production method and device for preparing high isotactic polybutene by liquid-phase bulk polymerization. Background technique [0002] High isotactic polybutene is a semi-crystalline polymer obtained by polymerization of butene-1 monomer. Its main physical and mechanical properties are similar to those of current general-purpose polypropylene and polyethylene. Alternative use in ethylene and polypropylene applications. [0003] High isotactic polybutene has outstanding thermal creep resistance (Vicat softening temperature is about 20°C higher than that of polypropylene), excellent impact resistance and lower glass transition temperature, so that it can be used at -20°C~ Use for a long time between 110°C. The use of high isotactic polybutene homopolymers and copolymers is mainl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F10/08C08F110/08C08F2/02C08F6/28C08F4/646C08F4/68C08F2/01
Inventor 贺爱华王峰忠邵华锋高丰宝刘晨光毕新平姜秀波杨海洋姚薇
Owner SHANDONG ORIENT HONGYE CHEM
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