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Method for controlling conversion of isotactic polybutylene-1 crystal system two to crystal system one by carbon dioxide

A technology of isotactic polybutene and crystal form, applied in the field of transformation from crystal form II of polybutene-1 to crystal form I, can solve the problems of small processing capacity, high equipment requirements, difficult process control, etc., and achieve the transformation period reduced effect

Inactive Publication Date: 2008-01-30
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Such as literature Armeniades, C., E.Baer, ​​J.macromol.Sci.B1, 309 (1967), Goldbach, G., Angew.Makromol.Chem.29 / 30, 213 (1973), Goldbach, G., Angew .Makromol.Chem.29 / 30, 175(1974), Kwang-bum Hong, Joseph E., J.Appl.Polym.Sci.30, the method disclosed in 3163(1985), these studies mainly focus on isotactic polymerization The transformation of the crystal form of ene-1 under hydraulic and mechanical force has a small processing capacity, and its processed form is limited to the film of isotactic polybutene-1. At the same time, the requirements for equipment are high, and the process is not easy to control

Method used

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  • Method for controlling conversion of isotactic polybutylene-1 crystal system two to crystal system one by carbon dioxide
  • Method for controlling conversion of isotactic polybutylene-1 crystal system two to crystal system one by carbon dioxide
  • Method for controlling conversion of isotactic polybutylene-1 crystal system two to crystal system one by carbon dioxide

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Place the isotactic polybutene-1 membrane with a thickness of 1mm in the crystal form II in a high-pressure container, and then pass through CO 2 , to control the CO in the high-pressure vessel 2 The temperature is 5°C and the pressure is 30 MPa.

[0022] After the temperature and pressure stabilized, the isotactic polybutene-1 in CO 2 Take out after 0.1 hour of medium treatment.

[0023] Through X-ray diffraction analysis (XRD), see Figure 1, it can be drawn from the diffraction pattern that the characteristic diffraction peaks that characterize the crystal form II have all disappeared, indicating that the crystal form II in the treated isotactic polybutene-1 film is All transformed into crystal form I; through differential scanning calorimetry (DSC), see Figure 2, only the melting peak of crystal form I appeared in the DSC curve, and it also showed that crystal form II was completely transformed into crystal form I . That is to say, in CO 2 The density is 28.1152...

Embodiment 2

[0025] Place isotactic polybutene-1 particles with a diameter of 3-5 mm in a high-pressure container, and then pass a certain amount of CO 2 , to control the CO in the high-pressure vessel 2 The temperature is 120° C. and the pressure is 30 MPa.

[0026] After the temperature and pressure stabilized, the isotactic polybutene-1 in CO 2 Take out after 0.15 hours of medium treatment.

[0027] By X-ray diffraction analysis (XRD), see Figure 3, as can be seen from the diffraction pattern, the characteristic diffraction peaks that characterize the crystal form II have all disappeared, indicating that all of the crystal form II in the isotactic polybutene-1 particles after treatment Transformed into Form I; through differential scanning calorimetry (DSC), see Figure 4, only the melting peak of Form I appears in the DSC curve, and it also shows that Form II is completely transformed into Form I. That is to say, in CO 2 The density is 25.7473g / cm 3 After 0.15 hours, the crystal fo...

Embodiment 3

[0029] Put powdery isotactic polybutene-1 particles in a high-pressure container, and then pass a certain amount of CO 2 , to control the CO in the high-pressure vessel 2 The temperature is 5° C. and the pressure is 0.1 MPa. After the temperature and pressure stabilized, the isotactic polybutene-1 in CO 2 Remove after 24 hours of processing. Through X-ray diffraction analysis (XRD), it can be seen from the diffraction pattern that the characteristic diffraction peaks that characterize the crystal form II have all disappeared, indicating that the crystal form II in the treated isotactic polybutene-1 powder has completely transformed into a crystal form I; by differential scanning calorimetry (DSC), only the melting peak of the crystal form I appears in the DSC curve diagram, indicating that the crystal form II is completely transformed into the crystal form I. That is to say, in CO 2 The density is 0.0435g / cm 3 When, after 24 hours, the crystal form II was completely trans...

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Abstract

The invention discloses a method of CO2 regulation and control isotactic polybutene-1 crystalline II changing into crystalline I, comprising the steps: the isotactic polybutene-1 crystalline II is put in CO2 atmosphere for 0.1 to 48 hours before the disposal material is taken out, then the isotactic polybutene-1 crystalline I is produced. Through controlling the CO2 temperature and pressure of isotactic polybutene-1 crystalline II, the invention successfully controls the procedure of isotactic polybutene-1 crystalline II changing into crystalline I as well as makes use of the interaction of CO2 molecule and isotactic polybutene-1 molecule to accelerate the isotactic polybutene-1 crystalline II changing into crystalline I, which reduces the transition periodicity of crystalline II changing into crystalline I. Thus, the stable isotactic polybutene-1 crystalline I gotten from industrial and business is easier, which is very important for widely use of isotactic polybutene-1.

Description

technical field [0001] This patent relates to a method for converting isotactic polybutene-1 crystal form II to crystal form I. Background technique [0002] Isotactic polybutene-1 is a commonly used engineering plastic, which has good elasticity, impact resistance, stress crack resistance, creep resistance, heat resistance and compression resistance, moisture barrier performance, electrical insulation performance, etc. It is widely used in the production of pipelines, the production of film and fiber materials for food packaging bags, and the improvement of other material properties by blends. [0003] Isotactic polybutene-1 has five different crystal forms, Form I, Form II, Form III, Form I' and Form II'. Among the five crystal forms, the most widely studied are the crystal form I and the crystal form II, and the crystal form I is composed of 3 1 The hexagonal unit cell structure of helical chains, the crystal form II is composed of 11 3 The tetragonal unit cell structu...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J3/00C08L23/20
Inventor 赵玲李磊刘涛许志美何峰
Owner EAST CHINA UNIV OF SCI & TECH
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