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A preparation method of a weather-resistant hydrolysis-resistant polyurethane adhesive

A polyurethane adhesive, hydrolysis-resistant technology, applied in the direction of polyurea/polyurethane adhesives, adhesives, adhesive types, etc. The effect of adhesive properties

Active Publication Date: 2021-04-13
浙江圣腾胶业股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At the same time, the polyurethane adhesive will break the carbon-nitrogen bond and carbon-oxygen bond under the action of ultraviolet rays, which will produce amino radicals, alkyl radicals, carbamoyl radicals and alkoxy radicals. The breakage of the molecular chain makes the adhesive layer easy to Fracture pulverization, which affects the adhesion performance

Method used

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  • A preparation method of a weather-resistant hydrolysis-resistant polyurethane adhesive
  • A preparation method of a weather-resistant hydrolysis-resistant polyurethane adhesive
  • A preparation method of a weather-resistant hydrolysis-resistant polyurethane adhesive

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] The specific preparation process of free radical capture crosslinking agent is as follows:

[0033] Step 1: Add 1mol pentamethylpiperidinol, 1.25mol chloroacetic acid and 1400mL acetone into the reaction kettle at the same time, heat to reflux, then add 33g concentrated sulfuric acid dropwise to it while keeping the temperature constant, control the dropwise addition within 30min, add After reflux reaction for 4 hours, recover 1 / 2 acetone, then add ice and water to precipitate crystals, cool to 3-5°C for filtration, add water to the filter cake and neutralize with sodium carbonate to pH = 8, filter to obtain pentamethyl Piperidine-4-chloro-2-acetate, the reaction structural formula is as follows, the product is carried out infrared analysis and can be known, at 794cm -1 At the C-Cl infrared absorption peak, at the same time at 3200cm -1 The broad and scattered absorption peaks at the left and right disappear;

[0034]

[0035] Step 2: Add a mixed solvent of 200mL e...

Embodiment 2

[0042] The specific preparation process of free radical capture crosslinking agent is as follows:

[0043] Step 1: Add 1mol pentamethylpiperidinol, 1.25mol chloroacetic acid and 1400mL acetone into the reaction kettle at the same time, heat to reflux, then add 33g concentrated sulfuric acid dropwise to it while keeping the temperature constant, control the dropwise addition within 30min, add After reflux reaction for 4 hours, recover 1 / 2 acetone, then add ice and water to precipitate crystals, cool to 3-5°C for filtration, add water to the filter cake and neutralize with sodium carbonate to pH = 8, filter to obtain pentamethyl Piperidine-4-chloro-2-acetate, the reaction structure is as follows;

[0044]

[0045] Step 2: Add a mixed solvent of 200mL ethanol and 100mL water, 42g paraformaldehyde and 110g N-isopropylacrylamide into the reaction tank, stir and dissolve, then raise the temperature to 70°C, then add 108g 2,5-dihydroxytoluene, and stir the reaction After 7 hours,...

Embodiment 3

[0050] The concrete preparation process of linking agent is as follows:

[0051] Add 200mL of ethanol and 100mL of mixed solvent of water, 80g of paraformaldehyde and 113g (1mol) g of N-isopropylacrylamide into the reaction tank, stir and dissolve, heat up to 65°C, and then add 396g (2.1mol) of p-nitrophenol , stirred and reacted for 7h, crystals were precipitated after the solvent was distilled off, and the obtained crystals were recrystallized with ethanol to obtain acrylamidonitrophenol; -1 The infrared absorption peak of conjugated olefin appeared at 3350cm -1 There is no infrared absorption peak of the phenolic hydroxyl group, and the carbon atoms in the ortho-position of the phenolic hydroxyl group and the meta-position of the nitro group contain active hydrogen, which can carry out aminomethylation reaction. By controlling the amount of N-isopropylacrylamide, the One of the ortho-position reactions of the hydroxyl group in nitrophenol;

[0052]

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Abstract

The invention discloses a method for preparing a weather-resistant hydrolysis-resistant polyurethane adhesive. The specific preparation process is as follows: a certain amount of free radical capture crosslinking agent and ethanol solution are weighed and added to a reaction kettle, stirred and dissolved, and then polymer glue is added. , raise the temperature to 110-115°C for 2 hours while stirring, then add triethylamine to it, cool down to 75-80°C and react for 6-7h, then cool and discharge the material, spin evaporate to obtain a solid substance, and then add the solid substance to ethanol , stir to form a polyurethane glue. One end of the free radical capture crosslinking agent prepared in the present invention is connected to the carbonyl side of the ester group in -NH-COO-, and the other end is connected to the hydroxyl end of the ester group in it, so that when the adhesive is hydrolyzed in high temperature water, the polymer The chains are still connected by the free radical capture crosslinking agent, so that the adhesive will not reduce its adhesive strength due to high temperature hydrolysis.

Description

technical field [0001] The invention belongs to the field of adhesive preparation and relates to a method for preparing a weather-resistant hydrolysis-resistant polyurethane adhesive. Background technique [0002] Polyurethane adhesives have excellent shear strength and impact resistance properties, are suitable for various structural bonding fields, and have excellent flexibility properties, and are widely used in bonding between various substrates. In the field of preparation, polyurethane adhesives are also used for bonding. In high-temperature and high-humidity environments, water vapor acting on the adhesive will cause the hydrolysis of the ester group in the adhesive, which will cause huge stress inside the adhesive. When the stress When the value accumulates to the critical value of the bonding strength between the adhesive and the base film, the adhesive will easily peel off from the base film. [0003] At the same time, the polyurethane adhesive will break the carb...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C09J175/08C08G65/336C08G65/333C08G18/66C08G18/50C08G18/76C08G18/10C08G18/32C08G18/83
CPCC08G18/10C08G18/5096C08G18/7621C08G18/833C08G65/33396C08G65/336C09J175/08C08G18/3206
Inventor 钟雨玲
Owner 浙江圣腾胶业股份有限公司
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