Preparation method of weather-resistant hydrolysis-resistant polyurethane adhesive

A polyurethane adhesive, anti-hydrolysis technology, applied in the direction of polyurea/polyurethane adhesive, adhesive, adhesive type, etc., can solve the problem of easy fracture and pulverization of the adhesive layer, affecting the adhesive performance, etc., to achieve high Effect of Adhesive Properties

Active Publication Date: 2020-12-29
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, al

Method used

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  • Preparation method of weather-resistant hydrolysis-resistant polyurethane adhesive
  • Preparation method of weather-resistant hydrolysis-resistant polyurethane adhesive
  • Preparation method of 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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PUM

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Abstract

The invention discloses a preparation method of a weather-resistant hydrolysis-resistant polyurethane adhesive. The method comprises: weighing a certain amount of a free radical capture cross-linkingagent and an ethanol solution, adding the weighed products into a reaction kettle, carrying out stirring for dissolving, then, adding a polymer glue solution, heating to a temperature of 110-115 DEG Cwhile stirring, carrying out reaction for 2h, adding triethylamine, cooling to 75-80 DEG C, reacting for 6-7 hours, then, carrying out cooling and discharging, carrying out rotary evaporation to obtain a solid substance, adding the solid substance into ethanol, and stirring to prepare the polyurethane adhesive. One end of the prepared free radical capture cross-linking agent is connected with oneside of a carbonyl group of an ester group in -NH-COO-, and the other end of the free radical capture cross-linking agent is connected with one end of a hydroxyl group of the ester group, so that polymer chains are still connected through the free radical capture cross-linking agent when the adhesive is hydrolyzed in high-temperature water, and the adhesive strength of the adhesive is not reduceddue 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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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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