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Asymmetric latent polyurethane curing agent and preparation method thereof

A polyurethane curing agent and latent technology, which is applied in the field of asymmetric latent polyurethane curing agent and its preparation, can solve problems such as differences in operation and use performance, and achieve the effects of no catalyst residue, environmental protection, and excellent vulcanization performance

Active Publication Date: 2017-08-15
江苏湘园化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] However, there are differences between the two in terms of operation and performance.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Embodiment 1: A kind of asymmetric latent polyurethane curing agent and its preparation method

[0028] Add 82.5g of ethyl p-aminobenzoate (also known as benzocaine, white crystalline powder, industrial product with a purity ≥99%) into a three-necked flask equipped with stirring, reflux, oil-water separator, and thermometer, and add 250g of di Toluene (15.4%, 21.4%, and 63.2% between adjacent and paired), stir to fully dissolve it, then add 120.1g of acetophenone (light yellow transparent liquid, purity ≥ 99.5%), stir for 15 to 20 minutes and then add 52.5g of diethanolamine (industrial product with a purity ≥ 99%), then add 20g of supported titanate catalyst, raise the temperature to 50°C, heat to reflux to separate water, maintain the reflux reaction for 2 hours, then raise the temperature to 130°C, and observe Obvious water separation, continue to react at this temperature for 2 hours, when no water is separated, turn on the vacuum, and gradually increase the tempera...

Embodiment 2

[0030] Embodiment two; A kind of asymmetric latent polyurethane curing agent and preparation method thereof

[0031]Add 75.6g of methyl p-aminobenzoate (white crystalline powder, an industrial product with a purity ≥99%) into a three-necked flask equipped with a stirring, reflux device, oil-water separator, and thermometer, add 250g of toluene, and stir to fully dissolve it. Then add acetophenone (oily colorless liquid, purity ≥99.5%), stir for 15-20 minutes, then add diethanolamine (industrial product with purity ≥99%), then add 20g of supported titanate catalyst, heat up to 80°C, Heat to reflux to separate the water, maintain the reflux reaction for 2 hours, then raise the temperature to 120°C, observe that there is obvious water separation, continue to react at this temperature for 2 hours, when no water is separated, turn on the vacuum, and gradually increase the temperature , when no liquid flows out, the temperature rises to 140°C, the vacuum is 10 torr, the heating is s...

Embodiment 3

[0032] Embodiment three; A kind of asymmetric latent polyurethane curing agent and preparation method thereof

[0033] Add 82.5g of ethyl p-aminobenzoate (also known as benzocaine, white crystalline powder, industrial product with purity ≥99%) into a three-necked flask equipped with stirring, reflux, oil-water separator, and thermometer, and add 250g of toluene , stir to make it fully dissolved, then add 106.2g of benzaldehyde (also known as benzoin aldehyde, light yellow transparent liquid, industrial product with purity ≥99%), stir for 15-20 minutes and then add 52.5g of diethanolamine (purity ≥99% industrial product), then add 20g of loaded titanate catalyst, raise the temperature to 75°C, heat to reflux to separate water, maintain the reflux reaction for 2 hours, then raise the temperature to 130°C, and observe that water is separated again. Continue to react for 2 hours. When no water is separated, turn on the vacuum and gradually increase the temperature. When no liquid ...

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Abstract

The invention discloses an asymmetric latent polyurethane curing agent and a preparation method thereof. A molecular structure of the asymmetric latent polyurethane curing agent has an oxazolidine group and an imine group, and has oxazolidine and imine dual function groups effect, and the asymmetric latent polyurethane curing agent has the characteristics of low viscosity, convenient operation, moderate reaction speed, and no odor after being released. The synthesis is characterized in that in a reaction vessel, ethanolamine cyclization, primary amino aldehyde (ketone) amination, and carboxyl and hydroxy esterification reaction are completed, process such as purification separating of an intermediate is not required, the process condition is mild, discharge of exhaust gas and waste residue is not generated, and a catalyst can be reused. The main raw materials are para amino benzoic acid (or ester), diethanolamine and aldehyde or ketone with 1-13 carbons. The reaction temperature is 40-150 DEG C, and the product can be used as the latent curing agent of a polyurethane material and as an active diluent.

Description

technical field [0001] The invention relates to an asymmetric latent polyurethane curing agent and a preparation method thereof, belonging to the fields of functional special chemicals and fine chemicals. Background technique [0002] The latent curing agent is an important component in the preparation of one-component polyurethane materials (SPU). It can be quickly unblocked when exposed to water vapor at room temperature to expose hydroxyl groups, primary amino groups and / or secondary amino groups that can react with isocyanate groups (-NCO). Preferential reaction with water over NCO is the key to this class of curing agents. Since the 1980s, many patents at home and abroad have disclosed a series of varieties of this type of curing agent, which are used in polyurethane CASE materials, such as US patent US5749627, German patent DE4021659, Japanese patent EP0965604 in the European Union, Grace Corporation EP2858965A1 (CN104364225A), EP2948485A1 (CN104903371A) of Swiss SIKA...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G18/32C07D263/04C07C249/02C07C251/16
CPCC07C249/02C07D263/04C08G18/3253C08G18/3296C07C251/16
Inventor 周建
Owner 江苏湘园化工有限公司
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