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Industrial preparation method of acrylate grafted polyisoprene

A technology of polyisoprene and acrylate, applied in the field of industrialized preparation of modified polyisoprene, which can solve the problems of inability to effectively dissolve polar polymerization inhibitors, unspecified purification methods of reactants, and polarity of solvent xylene Low-level problems, to achieve the effect of easy automatic management, low energy consumption for solvent recovery, and high reproducibility

Inactive Publication Date: 2018-05-18
濮阳林氏化学新材料股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Sodium methoxide, potassium hydroxide, and sodium hydroxide are all inorganic and solid. In industrial production, this type of catalyst has three shortcomings: the first is that the solubility of inorganic substances in organic reaction solvents is low, and they cannot be evenly distributed in the reaction system.
This type of polymerization inhibitor is solid, and the solvent xylene has a low polarity, which cannot effectively dissolve the polar polymerization inhibitor containing phenolic hydroxyl groups. For the reactor in the workshop, when feeding multiple times, the solid polymerization inhibitor is not conducive to automatic feeding. It needs to be manually operated many times, and the efficiency is low. Since the density of the solid polymerization inhibitor is higher than that of the solvent xylene, and it cannot be dissolved in xylene, it is easy to deposit near the discharge valve at the bottom of the reactor, and cannot be completely dissolved during the subsequent heating reaction, resulting in The waste of polymerization inhibitor and the error of feeding amount will affect the post-treatment of glue
In addition, the patent does not describe the purification method of reactants

Method used

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  • Industrial preparation method of acrylate grafted polyisoprene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] S1, introducing the solvent tetrahydrofuran into the A storage tank 1;

[0044] S2. Add 5 kg of maleic anhydride-modified polyisoprene into the first preparation tank 2, and introduce 11.2 L of solvent tetrahydrofuran into the first preparation tank 2, and stir at 30° C. to make the maleic anhydride-modified polyisoprene Isoprene is fully dissolved in the solvent;

[0045] S3. Add 0.05 kg of methyl tert-butyl ether into the second preparation tank 3, and introduce 0.06 L of solvent tetrahydrofuran into the second preparation tank 3, and stir at 20° C. to fully dissolve the polymerization inhibitor in the solvent;

[0046] S4, importing 1L of triethylamine into the B storage tank 4;

[0047] S5, importing 0.7L of hydroxyethyl methacrylate into C storage tank 5;

[0048] S6, 11.2 L of the maleic anhydride-modified polyisoprene solution prepared in step S2, 1 L of triethylamine in step S4, 0.7 L of hydroxyethyl methacrylate in step S5, and tertiary methyl methacrylate pr...

Embodiment 2

[0051] S1, introducing the solvent tetrahydrofuran into the A storage tank 1;

[0052] S2. Add 5 kg of maleic anhydride-modified polyisoprene into the first preparation tank 2, and introduce 5.6 L of solvent tetrahydrofuran into the first preparation tank 2, and stir at 40° C. to make the maleic anhydride-modified polyisoprene Isoprene is fully dissolved in the solvent;

[0053] S3. Add 0.05 kg of methyl tert-butyl ether into the second preparation tank 3, and introduce 0.03 L of solvent tetrahydrofuran into the second preparation tank 3, and stir at 30° C. to fully dissolve the polymerization inhibitor in the solvent;

[0054] S4, importing 1L of triethylamine into the B storage tank 4;

[0055] S5, importing 0.7L of hydroxyethyl methacrylate into C storage tank 5;

[0056] S6, 5.6 L of maleic anhydride-modified polyisoprene solution prepared in step S2, 1 L of triethylamine in step S4, 0.7 L of hydroxyethyl methacrylate in step S5, and tertiary methyl methacrylate prepared...

Embodiment 3

[0059] S1, introducing the solvent tetrahydrofuran into the A storage tank 1;

[0060] S2. Add 5 kg of maleic anhydride-modified polyisoprene into the first preparation tank 2, and introduce 11.2 L of solvent tetrahydrofuran into the first preparation tank 2, and stir at 30° C. to make the maleic anhydride-modified polyisoprene Isoprene is fully dissolved in the solvent;

[0061] S3. Add 0.1 kg of methyl tert-butyl ether into the second preparation tank 3, and introduce 0.11 L of solvent tetrahydrofuran into the second preparation tank 3, and stir at 20° C. to fully dissolve the polymerization inhibitor in the solvent;

[0062] S4, importing 1L of triethylamine into the B storage tank 4;

[0063] S5, importing 0.9L of hydroxyethyl methacrylate into the C storage tank 5;

[0064] S6, 11.2 L of the maleic anhydride-modified polyisoprene solution prepared in step S2, 1 L of triethylamine in step S4, 0.9 L of hydroxyethyl methacrylate in step S5, and tertiary methyl methacrylate...

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Abstract

The invention relates to an industrial preparation method of acrylate grafted polyisoprene. The preparation method comprises the following steps: adding modified polyisoprene and a polymerization inhibitor into corresponding preparation tanks; guiding solvents into the preparation tanks, and stirring for dissolution to obtain a modified polyisoprene solution and a polymerization inhibitor solution; sequentially guiding the modified polyisoprene solution, a liquid catalyst, a liquid grafting raw material and the polymerization inhibitor solution into a reaction kettle, and stirring for reacting; after the reacting, guiding the obtained reaction liquid into a washing kettle; adding acetone into the washing kettle, and stirring and washing; after the washing, standing for layering; drawing out the upper-layer mixed liquid; performing reduced-pressure heating and distillation of the lower-layer glue liquid to obtain the acrylate grafted polyisoprene; measuring the esterification rate by chemical titration. According to the industrial preparation method provided by the invention, the adopted solvents serve as dissolution liquid as well as reaction liquid; the raw materials, catalyst andadditives are in a liquid or solution state, which is convenient for pipeline conveying and feeding in production; moreover, the operation is simple, and the reaction conditions are mild.

Description

technical field [0001] The invention relates to an industrialized preparation method of modified polyisoprene, in particular to an industrialized preparation method of acrylate grafted polyisoprene. Background technique [0002] Semiconductor devices need to be packaged with adhesives during preparation to achieve the effects of preventing oxidation, waterproofing and shockproofing. Adhesives commonly used in these devices are light-curable adhesives. When the liquid chemical formula material is under the action of high-intensity energy of ultraviolet light or electron beam, it quickly transforms into a solid state to achieve the encapsulation effect. [0003] The main material in UV-curable coatings is a prepolymer, which has groups that can undergo photocuring reactions, such as carbon-carbon double bonds, acryloyloxy groups, methacryloyloxy groups, etc., among which acrylate and methacrylate groups Groups are most common. Common prepolymers in UV curing systems include...

Claims

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Application Information

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IPC IPC(8): C08F285/00C08F220/20C08F279/02C08F222/06
Inventor 张欣亮张广恩贺留洋王世浩林洪凯张文君
Owner 濮阳林氏化学新材料股份有限公司
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