Method for preparing linear macromolecules with controllable molecular weight by solution polycondensation reaction

A technology of solution polycondensation and molecular weight, which is applied to linear polymer devices and the field of linear polymer preparation, can solve problems such as judging the degree of reaction and difficult reaction time

Active Publication Date: 2016-04-27
中科嘉鸿(佛山市)新能源科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Therefore, it is difficult to judge the degree of reaction by reaction time

Method used

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  • Method for preparing linear macromolecules with controllable molecular weight by solution polycondensation reaction
  • Method for preparing linear macromolecules with controllable molecular weight by solution polycondensation reaction
  • Method for preparing linear macromolecules with controllable molecular weight by solution polycondensation reaction

Examples

Experimental program
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Effect test

Embodiment 1

[0033] Weigh 500.0g polyphosphoric acid, 29.9gP 2 o 5 (0.211mol) and 33.8g3,3`-diaminobenzidine (0.158mol), add 500mL successively, into the four-necked flask equipped with nitrogen inlet, mechanical stirring, condensing reflux tube and thermometer, and use electric heating mantle to gradually heat up to 210°C. Control the temperature to 210° C., the rotation speed to 390-410 rpm, and add 26.2 g of isophthalic acid (0.158 mol). When the temperature is kept at about 210°C and the rotational speed is maintained at 400 rap / min, when the current reaches 2.50 A, 15 mL of deionized water is quickly added to the solution, and the solution is quickly poured into deionized water. After standing overnight, take it out, dry it, crush it, and rinse it repeatedly with deionized water until the solution becomes neutral. Dry the solid to obtain powdered mPBI. The intrinsic viscosity measured by the Ubbelohde viscometer is 0.82dL / g, and the calculated molecular weight is the viscosity ave...

Embodiment 2

[0035] Weigh 500.0g polyphosphoric acid, 29.9gP 2 o 5 (0.211mol) and 33.8g3,3`-diaminobenzidine (0.158mol), add 500mL successively, into the four-necked flask equipped with nitrogen inlet, mechanical stirring, condensing reflux tube and thermometer, and use electric heating mantle to gradually heat up to 210°C. Control the temperature to 210° C., the rotation speed to 390-410 rpm, and add 26.2 g of isophthalic acid (0.158 mol). When the temperature is kept at about 210°C and the rotation speed is maintained at 400 rap / min, when the current reaches 2.66A, 15 mL of deionized water is quickly added to the solution, and the solution is quickly poured into deionized water. After standing overnight, take it out, dry it, crush it, and rinse it repeatedly with deionized water until the solution becomes neutral. Dry the solid to obtain powdered mPBI. The intrinsic viscosity measured by Ubbelohde viscometer is 0.90dL / g, and the calculated viscosity-average molecular weight is 41352....

Embodiment 3

[0037] Weigh 500.0g polyphosphoric acid, 29.9gP 2 o 5(0.211mol) and 33.8g3,3`-diaminobenzidine (0.158mol), add 500mL successively, into the four-necked flask equipped with nitrogen inlet, mechanical stirring, condensing reflux tube and thermometer, and use electric heating mantle to gradually heat up to 210°C. Control the temperature to 210° C., the rotation speed to 390-410 rpm, and add 26.2 g of isophthalic acid (0.158 mol). When the temperature is kept at about 210°C and the rotational speed is maintained at 400 rap / min, when the current reaches 3.01 A, 15 mL of deionized water is quickly added to the solution, and the solution is quickly poured into deionized water. After standing overnight, take it out, dry it, crush it, and rinse it repeatedly with deionized water until the solution becomes neutral. Dry the solid to obtain powdered mPBI. The intrinsic viscosity measured by the Ubbelohde viscometer is 1.04dL / g, and the calculated viscosity-average molecular weight is ...

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Abstract

The invention relates to a method for preparing linear macromolecules with controllable molecular weight by a solution polycondensation reaction. The method comprises five steps, i.e., preparing a reaction solution, controlling the reaction, computing product molecular weight, establishing a mathematical relation between reaction terminating current and the product molecular weight, and controlling the product molecular weight. Compared with the prior art, the method disclosed by the invention has the advantages that the viscosity of a solution polymerization system can be determined through the size of electric stirring device output current, and then, the molecular weight of a polymer is effectively controlled in a preparation process. The method has universality to solution polymerization reactions and is applicable to the preparation of various kinds of polymers such as polybenzimidazole, polyketone, polysulfone, polyether and polyamide. According to the method, the control on the molecular weight of the linear macromolecules to be prepared is accurate, and meanwhile, only a current measuring and displaying device (e.g., an ammeter) in series connection with an electric stirring device is additionally arranged outside a reaction device, so that the reaction device is simple, and the operation is easy. The method is of great significance for the preparation of the linear macromolecules with controllable molecular weight.

Description

technical field [0001] The invention relates to the field of polymer material preparation, in particular to a method for preparing a linear polymer with a controllable molecular weight; the invention also relates to a device for preparing a linear polymer with a controllable molecular weight by the method. Background technique [0002] Solution polycondensation is a method of polycondensation of monomers in an inert solvent. It can polycondense infusible or easily decomposable monomers to obtain heat-resistant aromatic heterocyclic polymers, such as polyimide, polysulfone, polyarylamide, polyarylate, etc. [0003] The characteristics of the solution polycondensation method are: the polycondensation reaction is carried out in a solvent, the reaction system is uniform, the viscosity is small, and it will not be extremely difficult to stir due to the increase of the degree of polymerization like the melt polycondensation. In addition, the solvent absorbs the heat of reaction, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/18C08G73/10C08G65/40C08G65/44C08G75/02
Inventor 孙公权马文佳王素力
Owner 中科嘉鸿(佛山市)新能源科技有限公司
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