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Method for rapidly evaluating activity of catalyst for cyclic ester ring opening polymerization in industrial production process

A technology of ring-opening polymerization and catalyst, applied in the field of polyester materials, can solve the problems of cumbersome steps and high cost, and achieve the effects of reliable test data, good reproducibility and high sensitivity

Inactive Publication Date: 2015-04-22
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The technical problem to be solved by the present invention is to provide a new method for evaluating the activity of catalysts to catalyze the ring-opening polymerization of cyclic esters. This method combines test results and theoretical formula calculations to solve the problems of cumbersome steps and high costs in current catalyst activity evaluation methods.

Method used

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  • Method for rapidly evaluating activity of catalyst for cyclic ester ring opening polymerization in industrial production process
  • Method for rapidly evaluating activity of catalyst for cyclic ester ring opening polymerization in industrial production process
  • Method for rapidly evaluating activity of catalyst for cyclic ester ring opening polymerization in industrial production process

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] 5 g of monomer and catalyst were used and mixed under vigorous stirring. After that, an appropriate amount of sample was taken for DSC measurement. DSC experiments were performed on a PerkinElmer 8500DSC instrument equipped with a cooling system. The most typical sample size for DSC measurements is 3-5 mg. The flow rate of nitrogen into the DSC sample cell is 50mL min -1 . The experiments were carried out in sealed aluminum crucibles. The relevant data were analyzed using Pyris V11 Data Analysis software.

[0040] First, the DSC reactants were completely sealed at 5 and 7.5 °C min-1 The heating rate was raised in the temperature range of 30 to 250 ° C, and the kinetic parameters of the polymerization at a uniform temperature were measured. The results are shown in Table 1:

[0041] Table 1: Temperature sweep kinetic parameters of GA homopolymerization at 145°C

[0042]

[0043] Note: catalyst, co-catalyst and initiator dosage ratio (molar ratio) are

[0044] n...

Embodiment 2

[0052] Except that the catalyst was changed to Bi(OAc) 3 Except its composite catalyst, adopt same measuring method as embodiment 1. The operating conditions and results are shown in Tables 3 and 4.

[0053] Table 3: Non-isothermal kinetic parameters of GA homopolymerization at 145 °C

[0054]

[0055] Note: the catalyst, co-catalyst and initiator consumption ratio (molar ratio) of each item in the above table are in line with:

[0056] no GA :n Bi(OAc)3 = 100; n Ph3P :n Bi(OAc)3 = 1; n MeOH :n Bi(OAc)3 =0.5

[0057] Table 4: Isothermal kinetic parameters of GA homopolymerization at 145 °C

[0058]

[0059] Note: the catalyst, co-catalyst and initiator consumption ratio (molar ratio) of each item in the above table are in line with:

[0060] no GA :n Bi(OAc)3 = 100; n Ph3P :n Bi(OAc)3 = 1; n MeOH :n Bi(OAc)3 =0.5

[0061] As can be seen from the data in Table 3 and Table 4, to Bi(OAc) 3 Add Ph to the system 3 After P and MeOH, the activation energy of ...

Embodiment 3

[0063] In addition to changing the catalyst to SnCl 2 2H 2 Except for O and its composite catalyst, the same measuring method as in Example 1 was adopted. The operating conditions and results are shown in Tables 5 and 6.

[0064] Table 5: Non-isothermal kinetic parameters of GA homopolymerization at 145 °C

[0065]

[0066] Note: the catalyst, co-catalyst and initiator consumption ratio (molar ratio) of each item in the above table are in line with:

[0067] no GA :n SnCl2·2H2O = 100; n Ph3P :n SnCl2·2H2O = 1; n MeOH :n SnCl2·2H2O =0.5

[0068] Table 6: Isothermal kinetic parameters of GA homopolymerization at 145 °C

[0069]

[0070] Note: the catalyst, co-catalyst and initiator consumption ratio (molar ratio) of each item in the above table are in line with:

[0071] no GA :n SnCl2·2H2O = 100; n Ph3P :n SnCl2·2H2O = 1; n MeOH :n SnCl2·2H2O =0.5

[0072] in Bi(OAc) 3 In the reaction of catalyzing the ring-opening polymerization of GA, at 145°C, E a 5...

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Abstract

The invention belongs to the technical field of polyester materials, in particular relates to a novel method for evaluating the activity of a catalyst for catalyzing cyclic ester ring opening polymerization, and solves the problem that a conventional cyclic ester ring opening polymerization catalyst activity evaluation method is large in workload and slow in speed. The method comprises the following steps: measuring the heat release process of the catalyst in the process of catalyzing cyclic ester ring opening polymerization by using a differential scanning calorimetry method, and confirming relevant reaction kinetic parameters (such as activation energy Ea, reaction velocity constant kapp and reaction order n). By comparing the activity of a single catalyst, a composite catalyst and acetylacetone catalysts and in the combination with DSC analysis result, the prompting function of various catalysts on cyclic ester ring opening polymerization are relatively accurately evaluated.

Description

technical field [0001] The invention belongs to the technical field of polyester materials, in particular to a new method for evaluating the activity of a catalyst to catalyze ring-opening polymerization of cyclic esters. Background technique [0002] Polyglycolic acid is decomposed and absorbable in the living body, so it is used as a medical polymer material such as sutures and artificial skin. In addition, polyglycolic acid is also excellent in heat resistance and mechanical strength, and is also used in the production of industrial products such as packaging materials, injection molded products, fibers, vapor-deposited films, and fishing lines, and is used in a wide range of technical fields. [0003] Polyglycolic acid is typically manufactured by ring-opening polymerization of glycolide. By this method, the degree of polymerization of polyglycolic acid can be easily controlled, and at the same time, polyglycolic acid with a high degree of polymerization having a weight...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N25/20
Inventor 陈群高建崔爱军陈圣春何明阳尹芳华
Owner CHANGZHOU UNIV
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