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Bulk polymerization method with constant-rate dropwise adding of monomer

A bulk polymerization and drop-adding technology, which is applied in the field of bulk polymerization, can solve problems such as the difficulty of heat dissipation in bulk polymerization, and achieve the effects of wide application range, improved strength, and uniform materials

Active Publication Date: 2015-09-02
GUANGZHOU HKUST FOK YING TUNG RES INST
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] In order to solve the above technical problems, the present invention provides a bulk polymerization method in which monomers are added dropwise at a constant rate. This method is not limited to the size of the prepared product, and can well solve the problem of heat dissipation and "burst polymerization" in bulk polymerization. , the prepared material avoids the introduction of new impurities and has excellent dielectric properties

Method used

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  • Bulk polymerization method with constant-rate dropwise adding of monomer
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  • Bulk polymerization method with constant-rate dropwise adding of monomer

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0061] (1) Fully mix 2.88mol styrene and 0.12mol divinylbenzene, add 4.233g benzoyl peroxide (BPO) (its molar concentration in the total reactant is 0.05mol / L) as initiator and fully Stir, and fill with argon for 30 minutes after it is completely dissolved to fully remove the dissolved oxygen in the monomer. All reactants were stored in syringes mounted on micropropellers and kept at low temperatures.

[0062] (2) Using DSC (Dynamic Differential Scanning Calorimetry) to test the reaction rate curves of the reactants at the heating rates of 1° C. / min, 2° C. / min and 5° C. / min respectively. Moreover, the polymerization reaction enthalpy ΔH was also measured by DSC to be 600 J / g.

[0063] (3) Combine the curves obtained in step (2) in one graph, and use the Kamal-Sourour model:

[0064] dα dt = ( A 1 exp ( - ...

Embodiment 2

[0080] Fully mix 2.94mol styrene and 0.06mol divinylbenzene, add 4.209g BPO (the molar concentration in the total reactant is 0.05mol / L) as an initiator and stir well, and fill with argon after it is completely dissolved 30 minutes to fully remove the dissolved oxygen in the monomer. All reactants were stored in syringes mounted on micropropellers and kept at low temperatures.

[0081] DSC (Dynamic Differential Scanning Calorimetry) was used to test the polymerization enthalpy of the reactants, and the reaction rate curves at different heating rates of 1 °C / min, 2 °C / min and 5 °C / min.

[0082] The Kamal-Sourour model was used to optimize the fitting of the rate curve, and the obtained parameters and ΔH were substituted into the exothermic model, and combined with the Fourier heat transfer model, the dropping rate at 70°C was determined to be 5.5ml / h , the corresponding growth rate in the thickness direction is 0.171cm / h (reactor with a diameter of 6.4cm).

[0083]Vacuumize a...

Embodiment 3

[0086] Mix 2.97mol of styrene and 0.03mol of divinylbenzene, add 4.197g of BPO (the molar concentration in the total reactant is 0.05mol / L) as an initiator and stir well, and fill with argon after it is completely dissolved 30 minutes to fully remove the dissolved oxygen in the monomer. All reactants were stored in syringes mounted on micropropellers and kept at low temperatures.

[0087] DSC (Dynamic Differential Scanning Calorimetry) was used to test the polymerization enthalpy of the reactants, and the reaction rate curves at different heating rates of 1 °C / min, 2 °C / min and 5 °C / min.

[0088] The rate curve was optimally fitted using the Kamal-Sourour model, and the obtained parameters and ΔH were substituted into the exothermic model, and combined with the Fourier heat transfer model to determine that the dropping rate at 70°C was 7ml / h. The corresponding growth rate in the thickness direction is 0.218cm / h (reactor with a diameter of 6.4cm).

[0089] Vacuumize the react...

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Abstract

The invention provides a bulk polymerization method with constant-rate dropwise adding of a monomer. The method comprises the following steps: stirring a reactant uniformly, and dropwise adding the reactant into a reactor at a constant rate to perform polymerization reaction, wherein the maximum rate fmax of the constant rate is selected by the steps of testing the polymerization enthalpy and reaction rate curve of the reactant by using a dynamic differential scanning calorimetry; performing optimization fitting on the obtained reaction rate curve by adopting a Kamal-Sourour dynamic model to obtain a parameter value of the model; substituting the parameter value and the polymerization enthalpy into a heat release model, and performing common calculation by combining a Fourier heat transfer model to obtain a change chart of the monomer conversion rate of a reaction system along with time at specified temperatures and different dropwise adding rates; and when the dropwise adding rate is more than fmax, showing explosive polymerization of the reaction system by the change chart. The method provided by the invention is not limited by the product size, and can be used for well solving the problems of difficult heat dissipation and 'explosive polymerization' during bulk polymerization; and the prepared material is uniform, can avoid introduction of new impurities, and is excellent in dielectric property.

Description

technical field [0001] The present invention relates to a bulk polymerization method, in particular, the present invention relates to a bulk polymerization method in which monomers are added dropwise at a constant rate. Background technique [0002] In recent years, frequencies involved in electronic equipment and communications have reached the GHz band, and this trend is intensifying. However, as the frequency increases, the temperature rise of the device caused by the dielectric loss of the material will become more serious, which will affect the life of the device and even its normal operation. At the same time, the frequencies involved in communication equipment such as communication satellites and radar are not limited to a single frequency band. Due to dielectric loss, when the signal passes through the dielectric material, it will be attenuated or distorted. Therefore, it is necessary to prepare a structural material that still has a low dielectric constant and diel...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F2/02C08F212/08
Inventor 陈元武朱业俊吴景深
Owner GUANGZHOU HKUST FOK YING TUNG RES INST
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