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A kind of preparation method of polybutene-1 of narrow molecular weight distribution

A narrow molecular weight distribution, polybutene technology, applied in the field of preparation of polybutene-1, can solve the problems of conflicting research results, influence promotion, and inability to give influence rules.

Active Publication Date: 2021-01-08
CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although people have carried out a lot of research on the factors affecting its crystallization behavior and crystal transformation (J.Macromol.Sci.Part B,2005,44:377-396), it is difficult to obtain fractions with narrow molecular weight distribution in the research , causing some research results to be contradictory, unable to give a systematic and exact influence law, which seriously affects the promotion of its practical application

Method used

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  • A kind of preparation method of polybutene-1 of narrow molecular weight distribution
  • A kind of preparation method of polybutene-1 of narrow molecular weight distribution
  • A kind of preparation method of polybutene-1 of narrow molecular weight distribution

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preparation example Construction

[0019] The invention provides a kind of preparation method of the polybutene-1 of narrow molecular weight distribution, comprises the following steps:

[0020] Dissolve the polybutene-1 sample in a mixed solvent at 120-150° C. to obtain a sample solution with a concentration of 0.5-1.5 wt %; the mixed solvent includes a good solvent and a poor solvent with a volume ratio of 70-95:5-30 Solvent; the good solvent is selected from one or more of 1,2,4-trimethylbenzene, 1,3,5-trimethylbenzene, 1,2,4-trichlorobenzene, dichlorobenzene and xylene; The poor solvent is selected from ethyl cellosolve and / or butyl cellosolve;

[0021] Lower the temperature of the sample solution to 10-30°C, load the sample on the filler, and completely replace the above-mentioned mixed solvent with a poor solvent after equilibrium, raise the temperature to 100-130°C, and then increase the volume percentage of the good solvent in order to balance After rinsing, polybutene-1 with a narrow molecular weight ...

Embodiment 1

[0037] Solvent gradient fractionation PB-1 specific steps:

[0038] 1) Dissolve the sample: use 1,2,4-trimethylbenzene (TMB) as a good solvent and butyl cellosolve (BCS) as a poor solvent, and dissolve the resin in a mixed solvent of TMB:BCS=70:30 at a high temperature of 140°C For the sample, the solution concentration is 1.5wt%, and the dissolution time is 6h.

[0039] 2) Load the sample: transfer the sample solution to the fractionation column (filler is glass beads of 60-80 mesh), stabilize at 140°C for 60min, then cool down to room temperature at a constant cooling rate of 1.5°C / h, so that the polymer is separated from the mixed solvent The medium precipitate was loaded onto the glass beads packed in the column.

[0040] 3) Rinse the sample: After the cooling program is finished, after equilibrating at room temperature for 24 hours, replace the mixed solvent in the fractionating column with 100% poor solvent BCS, and elute out the room temperature fraction dissolved in t...

Embodiment 2

[0050] 1) Dissolving samples: 1,3,5-Trimethylbenzene (TMB) is used as a good solvent, and butyl cellosolve (BCS) is used as a poor solvent. Dissolve in a mixed solvent of TMB:BCS=80:20 at a high temperature of 140°C For the resin sample, the solution concentration is 1.0wt%, and the dissolution time is 4h.

[0051] 2) Loading the sample: transfer the sample solution to a grading column (filler is 60-80 mesh quartz sand), stabilize at 140°C for 30min, then cool down to room temperature at a cooling rate of 1°C / h, so that the polymer is removed from the mixed solvent The precipitate is loaded onto the silica sand packed in the column.

[0052] 3) Rinse the sample: After the cooling program ends, after equilibrating at room temperature for 24 hours, replace the mixed solvent in the fractionating column with 100% inferior solvent BCS, and simultaneously elute out the room temperature fraction (2-1 # grades). Then the fractionation temperature rises to 120°C, and by successively ...

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Abstract

The invention provides a preparation method of polybutene-1 with a narrow molecular weight distribution, comprising: dissolving a polybutene-1 sample in a mixed solvent at 120-150° C. to obtain a sample solution with a concentration of 0.5-1.5 wt % ; Mixed solvents include good solvents and poor solvents with a volume ratio of 70~95:5~30; good solvents are selected from 1,2,4-trimethylbenzene, 1,3,5-trimethylbenzene, 1,2,4-trimethylbenzene One or more of chlorobenzene, dichlorobenzene and xylene; the poor solvent is selected from ethyl cellosolve and / or butyl cellosolve; the sample solution is cooled to 10-30°C, and the sample is loaded on the filler, After equilibrating, use poor solvent to completely replace the above mixed solvent, raise the temperature to 100-130°C, increase the volume percentage of good solvent in turn, rinse after equilibrating, and obtain polybutene with narrow molecular weight distribution from low to high respectively -1.

Description

technical field [0001] The invention belongs to the technical field of solvent gradient fractionation, and in particular relates to a preparation method of polybutene-1 with narrow molecular weight distribution. Background technique [0002] Polybutene-1 (PB-1) is made of monomer 1-butene by slurry method, bulk method or gas phase method in the presence of a catalyst. structure, especially isotactic polybutene-1 (iPB-1) (with an isotactic content higher than 96%) has outstanding thermal creep resistance, environmental stress cracking resistance, good toughness and wear resistance, and Chemical properties, etc., have the reputation of "plastic gold", and are widely used in various fields such as pipes and films (Prog. Polym. Sci. 1988, 13 (1): 37-62). At high temperature, PB-1 has better creep resistance and stress crack resistance than polyethylene and polypropylene, and is more suitable for hot water pipes; at low temperature, PB-1 also has better low temperature impact re...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08F6/04C08F110/08
CPCC08F6/04C08F110/08C08L23/22C08F2500/03
Inventor 薛彦虎姬相玲薄淑琴
Owner CHANGCHUN INST OF APPLIED CHEMISTRY - CHINESE ACAD OF SCI
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