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High-adhesiveness phenol aldehyde composite adhesive and preparation method thereof

A composite adhesive and high-adhesive technology, applied in the direction of polymer adhesive additives, adhesives, adhesive types, etc., to achieve low curing temperature, good gloss, and reduced release of free aldehydes

Inactive Publication Date: 2014-02-05
SHENYANG POLYTECHNIC UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] Imidazole-type polyether ionic liquids have terminal hydroxyl groups and flexible polyether long chains, and the modification of phenolic resin adhesives with imidazole-type polyether ionic liquids has not been reported at home and abroad.

Method used

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  • High-adhesiveness phenol aldehyde composite adhesive and preparation method thereof
  • High-adhesiveness phenol aldehyde composite adhesive and preparation method thereof
  • High-adhesiveness phenol aldehyde composite adhesive and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] Mix 0.5 mol of phenol, 0.25 mol of sodium hydroxide and 0.025 mol of aqueous solution into a round bottom flask, apply machine stirring and raise the temperature to 42°C, keep for 10 minutes, then add 80% formaldehyde solution (0.8 mol), within 15 minutes Raise the temperature to 70°C, add the remaining 20% ​​formaldehyde to obtain a phenolic resin prepolymer; add chloromethylimidazole-polyether ionic liquid after 10 minutes, keep the temperature for 20 minutes, then slowly raise the temperature to 93°C, and keep the system for 60 minutes. Cool down to 70°C, dehydrate under reduced pressure, add ethanol to adjust the viscosity, the measured viscosity is 390mPa·s, immediately cool to 40°C, and discharge to obtain a phenolic composite adhesive.

[0035] Wherein the chloromethylimidazole-polyether ionic liquid accounts for 10% by mass of the phenolic resin prepolymer.

[0036] Chloromethylimidazole-polyether ionic liquid, the structural formula is as follows:

[0037] ...

Embodiment 2

[0040] Mix 0.5 mol of phenol, 0.25 mol of sodium hydroxide and 0.025 mol of aqueous solution into a round-bottomed flask, apply mechanical stirring and raise the temperature to 45°C, keep for 10 minutes, then add 80% formaldehyde solution (0.8 mol), within 15 minutes The temperature was raised to 70°C, and the remaining 20% ​​formaldehyde was added to obtain a phenolic resin prepolymer; after 10 minutes, chloroethylimidazole-polyether ionic liquid was added. After keeping for 20 minutes, slowly raise the temperature to about 95°C, and after keeping for 60 minutes, cool the system down to 70°C, dehydrate under reduced pressure, add ethanol to adjust the viscosity, the measured viscosity is 410mPa·s, immediately cool to 40°C, and discharge to obtain phenolic formaldehyde Composite adhesive.

[0041] The specific steps of the lapped spline prepared in this example are the same as in Example 1, wherein the chloroethylimidazole-polyether ionic liquid accounts for 15% by mass of the...

Embodiment 3

[0045] The preparation method of this example is the same as Example 2, except that the ethylimidazole-polyether ionic liquid accounts for 20% by mass of the phenolic resin system, and the imidazole-type polyether ionic liquid used is anion BF 4 — imidazole polyether ionic liquid.

[0046] The resulting anion is Cl — Dissolve the chloroethylimidazole-polyether ionic liquid in dimethyl sulfoxide, stir evenly, add sodium tetrafluoroborate, react at 50°C for 24 hours, and perform anion exchange: after the ion exchange reaction, let stand and filter out chlorine Sodium chloride, then distilled under reduced pressure at 90°C and 0.1MPa to obtain the anion as BF 4 — The imidazole type polyether ionic liquid, structural formula is as follows:

[0047]

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Abstract

The invention belongs to the field of preparation of high-performance high polymer materials, and relates to a preparation method of a novel composite adhesive product, particularly a method for preparing a phenol aldehyde composite adhesive from an ionic liquid and a phenol aldehyde resin prepolymer by in-situ blending. The preparation method comprises the following steps: firstly synthesizing a phenol aldehyde resin prepolymer from raw materials phenol and formaldehyde in the presence of an alkali catalyst; by using an imidazole polyether ionic liquid with characteristic group as a modifier, heating, stirring under reflux, carrying out stage heating and temperature control, dehydrating under reduced pressure and the like to obtain the phenol aldehyde composite adhesive containing the imidazole polyether ionic liquid structure; and adding ethanol to regulate the viscosity of the composite adhesive to obtain the alcohol-soluble phenol aldehyde composite adhesive with acceptable viscosity. The method can further enhance the binding property and curing property of the phenol aldehyde adhesive, lower the free aldehyde content, and effectively solve the problems of low heat stability, deep color, high cracking tendency and the like in the phenol aldehyde adhesive.

Description

technical field [0001] The invention relates to a high-performance phenolic composite adhesive and a preparation method thereof, in particular to a high-performance environment-friendly phenolic composite adhesive formed by blending an imidazole-type polyether ionic liquid and a phenolic resin prepolymer and a preparation method thereof. Background technique [0002] Phenolic resin (PF) is widely used in many fields such as automobiles, electronics, electrical, transportation, and military because of its good cold resistance, electrical insulation, dimensional stability, molding processability, and flame retardancy. However, pure phenolic resin adhesives have disadvantages such as brittleness, high toxicity, high curing temperature, slow speed, dark color after curing, and easy cracking, resulting in low production efficiency, high energy and equipment consumption, and the phenolic hydroxyl groups of pure phenolic resin. The methylene is easily oxidized, which affects the he...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09J161/06C09J11/08
Inventor 郭立颖白世阳黄鹏程朱雪梅程送林刘金麟张彬马秀云
Owner SHENYANG POLYTECHNIC UNIV
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