Preparation method of low-crystallinity high trans-1,4-polyisoprene

A technology of polyisoprene and low crystallinity, applied in the field of polyisoprene synthesis, can solve the problems of rising crystallinity, high butadiene content, great difference in reactivity ratio, etc. The effect of good particle shape and high trans content

Active Publication Date: 2015-04-08
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

[0004] However, the butadiene content in the above-mentioned method is relatively high, and because the reactivity ratio of butadiene and isoprene is very different, a long trans-polybutadiene segment will be generated in the copolymer, and its crystallization ability is higher than that of the reverse polybutadiene. The crystallization ability of formula polyisoprene is still strong, which will easily lead to an increase in crystallinity, which will affect its use as an elastomer

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  • Preparation method of low-crystallinity high trans-1,4-polyisoprene
  • Preparation method of low-crystallinity high trans-1,4-polyisoprene
  • Preparation method of low-crystallinity high trans-1,4-polyisoprene

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[0028] The application provides a preparation method of low crystallinity and high trans-1,4-polyisoprene, comprising the following steps:

[0029] After mixing isoprene, co-catalyst, main catalyst and comonomer in sequence, prepolymerization and polymerization are carried out respectively to obtain trans-1,4-polyisoprene with low crystallinity and high degree;

[0030] The main catalyst includes: a spherical carrier and an active component loaded on the spherical carrier and a phosphate compound; the spherical carrier is magnesium chloride alcoholate or spherical silica; the active component One or more of halides of titanium, halides of vanadium, oxyhalides of titanium and oxyhalides of vanadium;

[0031] The comonomer is butadiene, piperylene or 2,3-dimethyl-1,3-butadiene; the molar ratio of the comonomer to isoprene in the polymerization reaction is 2% to 30%.

[0032] This application uses a catalyst with high activity, so that the obtained polymer has good shape, good ...

Embodiment 1

[0077] (1) carrier preparation

[0078] In a 250mL glass reactor equipped with a reflux condenser, a mechanical stirrer and a thermometer, and fully replaced with nitrogen, add 36.5mL of absolute ethanol and 21.3g of anhydrous magnesium chloride (ratio of magnesium alcohol to 2.8:1), and stir After the magnesium chloride is completely dissolved, add 75mL of white oil and 75mL of silicone oil, stir and mix, and maintain at 120°C for 1 hour to obtain a uniformly dispersed emulsion;

[0079] Through the emulsifier, under the condition of pressure of 0.3MPa and emulsifier speed of 3000r / min, the obtained emulsion is sprayed into another stirred reactor containing 1600mL of hexane and cooled to -25°C in advance , keep the temperature of hexane not higher than -10°C, stir for 30 minutes, filter, wash with dry hexane, wash away the silicone oil and white oil, vacuum dry and sieve, and obtain a spherical carrier of 30 μm to 50 μm, its composition MgCl 2 2.38C 2 h 6 O.

[0080] (2...

Embodiment 2～11

[0086] Using the main catalyst prepared in Example 1, according to the operation of synthesizing polyisoprene in Example 1, using the main preparation conditions listed in Table 1, the polyisoprene product is prepared, which is a non-bonding spherical polymerization matter particles. See also Table 1 for the trans content, crystallinity, melting temperature, etc. of the polyisoprene product. It can be seen from Table 1 that the polyisoprene product prepared by the present application has high trans content and low crystallinity. The melting temperature of the polyisoprene that embodiment 2~5 prepares is as follows figure 2 shown.

[0087] Table 1 Main preparation conditions and test results of polyisoprene provided in Examples 1-11 of this application

[0088]

[0089]

[0090] Note: "Catalyst concentration" is the molar ratio of active component to isoprene; "monomer ratio" is the molar ratio of comonomer to isoprene; "aluminum phenate" is 2,6-di-tert-butyl Diisobu...

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Abstract

The invention provides a preparation method of low-crystallinity high trans-1,4-polyisoprene. The method comprises the following steps: sequentially mixing isoprene, a cocatalyst, a main catalyst and a comonomer; and respectively carrying out pre-polymerization reaction and polymerization reaction, so as to obtain the low-crystallinity high trans-1,4-polyisoprene, wherein the main catalyst contains a spherical support and an active component and a phosphate compound; the active component and the phosphate compound are loaded on the spherical support; the spherical support is a magnesium chloride alcohol compound or a spherical silicon dioxide; the comonomer is butadiene, pentadiene or 2,3-dimethyl-1,3-butadiene; and the molar ratio of the comonomer to the isoprene in the polymerization reaction is 2%-30%. The invention provides a method for preparing low-crystallinity high trans-1,4-polyisoprene. The problems of polymer morphology control, polymer liquidity and the like in a bulk precipitation polymerization process are effectively solved.

Description

technical field [0001] The invention belongs to the technical field of polyisoprene synthesis, in particular to a preparation method of low crystallinity and high trans-1,4-polyisoprene. Background technique [0002] High trans-1,4-polydiene, its monomers are more regularly arranged in the structure of trans-1,4- in the molecular chain of the material, which is easy to crystallize. This structure endows polydiene with many unique and excellent properties, making it widely used. For example, high trans-1,4-polyisoprene (TPI) can be used as shape memory functional materials, medical materials, plastics and modified rubber materials, etc. Chinese patent documents with application numbers 95110352.0, 200610043556.4 and 201310206156.0 respectively disclose the preparation methods of TPI. The TPI prepared by the methods disclosed in these documents is easy to crystallize or has high crystallinity. The crystallinity is above 30%, and it is a crystalline plastic at room temperature...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F236/08C08F4/02C08F4/649
Inventor 张春雨张学全胡雁鸣白晨羲张贺新毕吉福代全权于琦周那丽华
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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