A kind of synthetic method of high regularity polybutene-1

A synthesis method and a high-specificity technology are applied in the field of synthesis of polybutene-1 of regularity, and can solve the problems of long polybutene-1 crystal transformation period, low isotacticity of polybutene-1, and the like. Improve the effect of long crystal transformation period, simple process and easy operation

Active Publication Date: 2019-03-12
PETROCHINA CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The main purpose of the present invention is to provide a synthetic method of polybutene-1 with high isotacticity, which has solved the problem of low isotacticity of polybutene-1 and long crystal transformation period of polybutene-1 in the prior art defect

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  • A kind of synthetic method of high regularity polybutene-1
  • A kind of synthetic method of high regularity polybutene-1

Examples

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Comparison scheme
Effect test

Embodiment 1

[0040] In a 0.25L stainless steel autoclave, after the system was replaced three times with nitrogen, 0.81ml of 1mol / L triethylaluminum solution was added successively under nitrogen protection (the solvent is n-hexane, the same as in the following examples), diphenyl dimethoxy Silane 0.009mmol, methyl n-butyl ether 0.018mmol, TiCl 4 / MgCl 2 .ID / SiO 2 Supported Ziegler-Natta catalyst 5mg (0.0027mmol titanium), liquid phase propylene 70g, pre-polymerized at 50°C for 10min. After the reaction, vacuumize, add butene-1 monomer 95g, hydrogen 0.0035MPa, polymerize at a constant temperature at 35°C for 5h, and flash evaporate to remove unreacted monomer to obtain polybutene-1 powder with a particle size of 0.01-3mm. The molar ratio of the aluminum in the cocatalyst to the titanium in the main catalyst is 300, the molar ratio of the aluminum in the cocatalyst to the silicon in the composite external electron donor is 90, diphenyldimethoxysilane and methyl n-butyl ether The molar ra...

Embodiment 2

[0042] Compared with Example 1, except that the molar ratio of diphenyldimethoxysilane and methyl n-butyl ether in the composite external electron donor was changed to 1:7, the rest of the operation and reaction conditions remained unchanged, and the obtained particle size was 1348μm×1635μm polybutene-1 powder (such as figure 1 and figure 2 ). Catalyst activity is 6101g polybutene-1 / g main Cat, and isotactic polymer content (heptane soluble matter accounts for the percentage of heptane soluble matter and ether soluble matter summation) is 97.6%, molecular weight distribution is 6.3, poly The propylene content is 5.0%, the semi-crystallization time t of polybutene-1 powder crystallization at room temperature 1 / 2 =4.4h (the half-crystallization time t of the polybutene-1 homopolymer of measurement 1 / 2 = 25.4h). The crystal melting peak temperatures of the polymers measured by differential scanning calorimetry (DSC) were 124.2°C and 162.9°C, respectively.

Embodiment 3

[0044] Compared with Example 1, except that the molar ratio of diphenyldimethoxysilane to methyl n-butyl ether in the composite external electron donor was changed to 1:8, the rest of the operation and reaction conditions remained unchanged. Catalyst activity is 6131g polybutene-1 / g main Cat, and isotactic polymer content (heptane soluble matter accounts for the percentage of heptane soluble matter and ether soluble matter summation) is 98.1%, molecular weight distribution is 5.9, poly The propylene content is 4.8%, the semi-crystallization time t of polybutene-1 powder crystallization at room temperature 1 / 2 =4.5h (the half-crystallization time t of the polybutene-1 homopolymer of measurement 1 / 2 = 25.4h). The crystal melting peak temperatures of the polymers measured by differential scanning calorimetry (DSC) were 123.9°C and 162.6°C, respectively.

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Abstract

The invention discloses a high-isotacticity polybutene-1 synthesis method. According to the method, the stereo-tacticity of polybutene-1 is regulated by means of alkoxy silane and ether compound external electron donors. The method comprises the following specific steps: (1) sequentially adding an alpha-olefin prepolymerization monomer, a cocatalyst, a Ti loaded main catalyst and the alkoxy silane and ether compound external electron donors into a tank reactor, and polymerizing at 5-95 DEG C for 10-100 minutes; and (2) depressurizing to remove the unreacted alpha-olefin prepolymerization monomer in the system, then introducing a butylene-1 monomer and a molecular weight regulator, polymerizing at 0-95 DEG C for 1-20 hours, and performing flash evaporation on the unpolymerized monomer to obtain powdery polybutene-1. The high-isotacticity polybutene-1 synthesis method provided by the invention is simple in process and easy to operate; the product is high in isotacticity and high in crystallization melting point; and meanwhile, the crystal form transition cycle of polybutene-1 can be also shortened.

Description

technical field [0001] The invention relates to the field of petrochemical industry, in particular to a method for synthesizing high isotactic polybutene-1. Background technique [0002] Polybutene-1 is a semi-crystalline thermoplastic resin with polymorphism. Polybutene-1 material has outstanding creep resistance, impact resistance and environmental stress cracking resistance, especially its excellent impact resistance. It can be used in automobile bumper materials. In addition, polybutene-1 can be used for a long time at 80-90 ° C, and the upper limit of the service temperature can reach 110 ° C. It is an excellent hot water pipe material. The performance of polybutene-1 material has a certain relationship with its isotacticity and crystal transformation. Polybutene-1 with high isotacticity shows high yield strength and high modulus mechanical properties. In addition, polybutene-1 Moderately thermodynamically unstable crystal form II transforms into stable crystal form I,...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F210/08C08F210/06C08F4/649C08F4/646
CPCC08F210/08C08F2500/15C08F4/6498C08F4/6494C08F4/6465C08F210/06
Inventor 任合刚付义宋磊王斯晗高宇新赵成才王登飞刘宾元高晶杰杨敏董晓芳
Owner PETROCHINA CO LTD
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