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Preparation method of polymeric material

A polymer material and polymer technology, which is applied in the field of preparing polyurethane or polyacrylate and its composite materials by front-end polymerization, can solve the problems of low efficiency and slow reaction speed.

Inactive Publication Date: 2014-07-23
王超 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the slow speed of the bulk polymerization reaction, continuous external energy supply is required, and the efficiency is low. If the method of front-end polymerization is adopted, the energy consumption in the synthesis process can be greatly reduced, and materials with better performance can be synthesized.

Method used

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  • Preparation method of polymeric material

Examples

Experimental program
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Effect test

Embodiment 1

[0037] Polyacrylate front-end polymerization

[0038] Pour 100g of acrylate monomer into a 10mm diameter test tube, slowly add 0.1% benzoyl peroxide dropwise, immerse a heating rod at 0.5cm below the liquid surface, heat to 60°C for 40s and then evacuate. The pressure is 1 atmosphere. The Fourier transform infrared spectrum shows that the polyacrylate synthesized by the front-end polymerization and the tank reaction has the same characteristic peaks. From the SEM image, it can be seen that the polyacrylate synthesized by the front-end polymerization has good dispersion, which proves that the front-end polymerization has a stable reaction. region, making the synthesized polyacrylate structure stable.

example 2

[0040] Polyurethane front-end polymerization reaction

[0041] The solvent is xylene with a mass fraction of 20%, 2,4-toluene diisocyanate (TDI) with a mass fraction of 14%, 1,4-butanediol (BG) with a mass fraction of 3%, and polypropylene glycol with a molecular weight of 2000 ( The mass fraction of PPG) is 62%, and the mass fraction of dibutyltin dilaurate (DBTDL) is 1%. First, pour BG, PPG, xylene and DBTDL into a 10mm diameter test tube according to the above ratio, shake the test tube slightly to mix them evenly, and finally Slowly add TDI dropwise, immerse the heating rod at 0.5cm below the liquid surface and heat for 40s, then evacuate. The pressure is 1 atmosphere. Fourier transform infrared spectroscopy shows that the polyurethane synthesized by the front-end polymerization and the tank reaction has the same characteristic peaks. From the SEM image, it can be seen that the polyurethane synthesized by the front-end polymerization has good dispersion, which proves that...

example 3

[0043] Polyurethane acrylate front-end polymerization scheme

[0044]First add the polyether diol ([NCO] / [OH]=2 / 1, mol / mol) of the TDI of metering, dehydration, 45% (mass) DMSO (solvent), appropriate amount of DBTDL (catalyst), heat up to 75°C, heat preservation reaction for 4 h, then lower the temperature to 45°C to obtain NCO-terminated prepolymer. At 45°C, a measured amount of HPA ([TDI] / [HPA]=1 / 2, mol / mol) was added dropwise to the above reaction solution. After the dropwise addition is completed (about 1 h), raise the temperature to 55°C, keep the temperature for 10 h, and track the reaction with FTIR. When the NCO absorption peak at 2270-2273 cm-1 disappears, stop the reaction and cool down to room temperature to obtain a terminal alkenyl macromolecule monomer. At room temperature, add metered HPA ([alkenyl-terminated macromer] / [HPA]=1:4, mol / mol), thermal free radical Initiator and 45% (mass) dimethyl sulfoxide (DMSO), fully stirred evenly. Pour an appropriate amoun...

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Abstract

The invention provides a preparation method of polyurethane or polyacrylate and composite materials thereof by use of a frontal polymerization reaction. The method comprises the following steps: A, the following components are evenly mixed, the components are as follows: 70-98% by weight of polymer monomer, 2-4% by weight of an initiator, 0-2% by weight of a catalyst and 0-28% by weight of a solvent; B, the components are mixed into a reactor for a short time of heating in one end of the reactor, then the heating is stopped, and the frontal polymerization reaction can be completed with the help of heat from exothermic reaction. According to the method the energy consumption in the process of synthesis can be greatly reduced, materials with more excellent performances can be synthesized.

Description

technical field [0001] The invention relates to a method for preparing polymer materials, in particular to a method for preparing polyurethane or polyacrylate and composite materials thereof by front-end polymerization. Background technique [0002] Frontal polymerization (frontal polymerization, FP) is a new technology for the preparation and processing of polymers and their composite materials that has developed rapidly in recent years. It is a new polymerization method of converting monomers into polymers by using the heat generated by the self-reaction of monomers to maintain polymerization. The typical reaction process is as follows: first, put the mixture containing monomer and initiator into the tubular reactor, heat at any end of the reactor, the initiator is decomposed by heat, triggers the polymerization reaction of the monomer, and releases heat; the heat of polymerization reaction Diffusion to the low-temperature unreacted area, forming a narrow reaction area in...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F20/06C08F20/28C08F20/04C08F22/14C08F2/06C08G18/76C08G18/66C08F290/06
Inventor 王超殷燕子
Owner 王超