Linear controllable ultra-high molecular weight polyalkyl methacrylate and synthesis method

A polyalkyl methacrylate, ultra-high molecular weight technology, applied in the polymer field, can solve problems such as difficulty in realizing large-scale industrial production and limited molecular growth with the increase of solid content, so as to improve the molecular weight of polymers, Good heat dissipation effect, ensure the effect of heat dissipation effect

Active Publication Date: 2022-04-01
长春市兆兴新材料技术有限责任公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Solution polymerization is feasible, but it must be completed in the presence of a large excess of solvent. After the polymerization is completed, the solvent will be coated in the polymer and it is difficult to remove
Bulk polymerization is easy to explode, and the growth of molecules is limited with the increase of solid content in the later stage of the reaction
Therefore, the method of preparing polyalkylmethacrylate with controllable activity is still in scientific research, and it is extremely rare in production, and it is even more difficult to realize large-scale industrial production.

Method used

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  • Linear controllable ultra-high molecular weight polyalkyl methacrylate and synthesis method

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Experimental program
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Effect test

Embodiment 1

[0045] This embodiment provides a kind of synthetic method of ultra-high molecular weight polymethyl methacrylate, and concrete steps are as follows:

[0046] (1) Preparation of high-molecular-weight polymethyl methacrylate seeds: first take 100 g of methyl methacrylate that has been processed by vacuum distillation, and pass nitrogen to remove oxygen for later use. In a 1000 ml three-necked reaction flask, add 500 g of ethyl acetate, and pass nitrogen Stir, add 0.05g ethyl 2-bromoisobutyrate, 0.03g copper powder, 0.03g cuprous bromide, 0.05g pentamethyldiethylenetriamine, 0.005g disodium edetate, and mix well , raise the temperature to 50°C, add 10g of methyl methacrylate at one time until the system becomes slightly viscous, then adjust the temperature to 78°C, ethyl acetate refluxes in the condenser, slowly add the remaining 90g of methacrylic acid dropwise Methyl ester, the rate of addition is based on the reflux state. After the addition is completed, react at a constant ...

Embodiment 2

[0049] This embodiment provides a kind of synthetic method of ultra-high molecular weight polymethyl methacrylate, and concrete steps are as follows:

[0050] (1) preparation of high molecular weight polymethyl methacrylate seed: with embodiment 1 step (1);

[0051] (2) Synthesis of ultra-high molecular weight polymethyl methacrylate: Methyl methacrylate is processed through vacuum distillation, feed nitrogen deoxygenation for subsequent use, get the high molecular weight polymethyl methacrylate prepared by 120g step (1) Seed solution, wherein the high molecular weight polymethyl methacrylate seed content is 20g, under the protection of nitrogen, transfer to a 2L reaction kettle with a double planetary mixer, stir with nitrogen, raise the temperature to 78 ° C, and wait for the condensation tube reflux in the medium, slowly add 750g of spare methyl methacrylate monomer dropwise, the rate of addition should be stable with the reflux in the condenser tube, after the 750g methyl ...

Embodiment 3

[0053] This embodiment provides a kind of synthetic method of ultra-high molecular weight polymethyl methacrylate, and concrete steps are as follows:

[0054] (1) preparation of high molecular weight polymethyl methacrylate seed: with embodiment 1 step (1);

[0055] (2) Synthesis of ultra-high molecular weight polymethyl methacrylate: Methyl methacrylate is processed through vacuum distillation, feed nitrogen deoxygenation for subsequent use, get the high molecular weight polymethyl methacrylate prepared by 120g step (1) Seed solution, wherein the high molecular weight polymethyl methacrylate seed content is 20g, under the protection of nitrogen, transfer to a 2L reaction kettle with a double planetary mixer, stir with nitrogen, raise the temperature to 85 ° C, wait for the condensation tube Backflow occurs in the middle, slowly add 1500g methyl methacrylate monomer dropwise, the rate of addition should be stable with the reflux in the condenser tube, after the 750g methyl met...

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Abstract

The invention relates to linear controllable ultra-high molecular weight poly (alkyl methacrylate) and a synthesis method, and the synthesis method comprises the following steps: firstly, preparing a high molecular weight poly (alkyl methacrylate) seed, and preparing ultra-high molecular weight poly (alkyl methacrylate) by using the high molecular weight poly (alkyl methacrylate) seed. A mode of combining solution polymerization and bulk polymerization is adopted, a solvent in a seed solution is replaced by excessive reaction monomers in the process of preparing the ultra-high molecular weight polyalkyl methacrylate, and the monomers are used for replacing the solvent to achieve a dilution effect, so that curing is avoided, a good heat dissipation effect is ensured, and molecular growth is not limited; by controlling the temperature in each reaction process, implosion caused by a gel effect can be avoided, redundant monomers are distilled out after the reaction is finished, the overall polymer performance is not influenced, the water consumption is not increased in the whole production process, wastewater is not generated, and the method is suitable for large-scale industrial production.

Description

technical field [0001] The invention belongs to the technical field of macromolecules, and in particular relates to a linear controllable ultrahigh molecular weight polyalkylmethacrylate and a synthesis method. Background technique [0002] As an important organic material, especially as a transparent material, alkyl methacrylate is an irreplaceable organic polymer with strong weather resistance and transparency, and its light transmittance reaches 92%. Inorganic glass is good, and its strength is far greater than ten times that of inorganic glass. Since its invention in World War II, it has been used until today. Widely used in aircraft, automobiles, trains, ships, human bones, bridges, buildings, culverts, optical instruments and other fields. [0003] The main synthesis method of polyalkyl methacrylate is to use free radicals to initiate polymerization. At present, the methods of free radicals to initiate polymerization include suspension polymerization, solution polymer...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08F120/14C08F120/18C08F130/08C08F120/24C08F2/06C08F2/02
Inventor 韩兆让
Owner 长春市兆兴新材料技术有限责任公司
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