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Preparation method of boron modified phenolic resin adhesive

A technology of phenolic resin glue and phenolic resin, applied in the direction of adhesives, aldehyde/ketone condensation polymer adhesives, adhesive types, etc., can solve problems such as high corrosion, achieve strong impact toughness, good adhesion, The effect of improving the curing speed

Inactive Publication Date: 2017-05-17
JIANGSU GUOJIAO CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Some studies have introduced hydroquinone structure into polyborosiloxane to obtain polyborosiloxane. At present, the following technical route is mainly used to prepare boron-modified phenolic resin: In a nitrogen atmosphere, the bulk reaction is performed by dihalosilane and boric acid , then add hydroquinone solution to continue the reaction, then add hydroquinone solution to continue the reaction to obtain boron-modified phenolic resin, but the reaction between halosilane and boric acid generates HCL gas with a pungent smell, which is highly corrosive

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] The invention discloses a method for preparing a boron-modified phenolic resin adhesive. The preparation method is specifically as follows:

[0016] (1) Add organosiloxane and boric acid to styrene solvent, then place the entire reaction vessel in a closed container filled with nitrogen, and at the same time ensure that the temperature in the closed container rises from 100°C to 210°C, and react for 1~ 5h;

[0017] (2) Add polyhydric phenol into the reaction vessel and react for 4-10 hours to obtain polyborosiloxane;

[0018] (3) Add the prepared polyborosiloxane, toughening modifier, catalyst and formaldehyde into the reactor at a ratio of 10:10:1:1, and react at 80-100°C for 1-5 hours , then add sodium hydroxide solution to adjust the pH to 6.5-7.5, and then obtain the modified phenolic resin by distillation under reduced pressure;

[0019] (4) Mix polyborosiloxane and modified phenolic resin in a ratio of 1:5 to 2:5 to obtain a boron-modified phenolic resin adhesiv...

Embodiment 2

[0022] The invention discloses a method for preparing a boron-modified phenolic resin adhesive. The preparation method is specifically as follows:

[0023] (1) Add organosiloxane and boric acid to styrene solvent, then place the entire reaction vessel in a closed container filled with nitrogen, and at the same time ensure that the temperature in the closed container rises from 100°C to 210°C, and react for 1~ 5h;

[0024] (2) Add polyhydric phenol into the reaction vessel and react for 4-10 hours to obtain polyborosiloxane;

[0025] (3) Add the prepared polyborosiloxane, toughening modifier, catalyst and formaldehyde into the reactor at a ratio of 40:40:3:3, and react at 80-100°C for 1-5 hours , then add sodium hydroxide solution to adjust the pH to 6.5-7.5, and then obtain the modified phenolic resin by distillation under reduced pressure;

[0026] (4) Mix polyborosiloxane and modified phenolic resin in a ratio of 2:5 to 3:5 to obtain a boron-modified phenolic resin adhesiv...

Embodiment 3

[0029] The invention discloses a method for preparing a boron-modified phenolic resin adhesive. The preparation method is specifically as follows:

[0030] (1) Add organosiloxane and boric acid to styrene solvent, then place the entire reaction vessel in a closed container filled with nitrogen, and at the same time ensure that the temperature in the closed container rises from 100°C to 210°C, and react for 1~ 5h;

[0031] (2) Add polyhydric phenol into the reaction vessel and react for 4-10 hours to obtain polyborosiloxane;

[0032] (3) Add the prepared polyborosiloxane, toughening modifier, catalyst and formaldehyde in the ratio of 8:8:1:1 to the reactor, and react at 80-100°C for 1-5 hours , then add sodium hydroxide solution to adjust the pH to 6.5-7.5, and then obtain the modified phenolic resin by distillation under reduced pressure;

[0033] (4) Mix polyborosiloxane and modified phenolic resin in a ratio of 3:5 to 4:5 to obtain a boron-modified phenolic resin adhesive....

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Abstract

The invention relates to a preparation method of a boron modified phenolic resin adhesive. The method comprises the following steps: adding organosiloxane and boric acid to a styrene solvent, placing a whole reaction container in a closed container full of nitrogen, guaranteeing that the temperature in the closed container rises to 210 DEG C from 100 DEG C, and carrying out a reaction for 1-5 h; adding polyphenol to the reaction container, and carrying out a reaction to prepare polyborosiloxane; adding the prepared polyborosiloxane, a toughening modifier, a catalyst and formaldehyde to the reactor, and carrying out reduced pressure distillation to obtain modified phenolic resin; and uniformly mixing the polyborosiloxane with the modified phenolic resin to obtain the boron modified phenolic resin adhesive. The polyborosiloxane containing a large amount of terminal hydroxyl groups and having excellent heat stability is synthesized through polycondensation of organosiloxane, boric acid and polyphenol, and the modified phenolic resin has enough high impact toughness, cementability, heat resistance and flame resistance, so the solidification speed in the preparation process is improved.

Description

technical field [0001] The invention relates to a preparation method of an adhesive, in particular to a preparation method of a boron-modified phenolic resin adhesive. Background technique [0002] Polyborosiloxane has excellent heat resistance. Some studies have used boric acid and silicone prepolymers to prepare polyborosiloxane and used it to modify phenolic resins. The carbon residue rate of the modified resins has been greatly improved, but the modified phenolic resin adhesives The adhesion strength was not significantly improved. Some studies have introduced hydroquinone structure into polyborosiloxane to obtain polyborosiloxane. At present, the following technical route is mainly used to prepare boron-modified phenolic resin: In a nitrogen atmosphere, the bulk reaction is performed by dihalosilane and boric acid , then add hydroquinone solution to continue the reaction, then add hydroquinone solution to continue the reaction to obtain boron-modified phenolic resin, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09J161/14C09J183/14C08G8/28C08G77/56
Inventor 张孝俤
Owner JIANGSU GUOJIAO CHEM TECH
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