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Stably-stored blocked isocyanate composition, and preparation method and application thereof

A technology of blocked isocyanate and storage stability, applied in polyurea/polyurethane adhesives, adhesive types, polyurea/polyurethane coatings, etc., can solve problems such as color instability, and achieve stable color number and chromaticity low effect

Active Publication Date: 2020-02-18
WANHUA CHEM GRP CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The object of the present invention is to provide a storage-stable blocked isocyanate composition and a preparation method thereof, aiming at the problem of color instability of existing blocked isocyanates during storage, by controlling the phenolic compounds in blocked isocyanate products The content can effectively improve the storage stability of blocked isocyanate products blocked by oxime compounds, and ensure the low chroma of the products

Method used

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  • Stably-stored blocked isocyanate composition, and preparation method and application thereof
  • Stably-stored blocked isocyanate composition, and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0054] (1) Add 200g of polyisocyanate Desmodur N3300, 0.15g of methyl p-toluenesulfonate, and 97.5g of Mobil S100 solvent oil into a four-necked flask, stir evenly under nitrogen protection, heat up to 90°C for 2 hours, and obtain alkylation treatment The final polyisocyanate is then cooled to 60°C;

[0055] (2) Add 92 g of butanone oxime to a four-necked flask, control the reaction temperature to 60-70° C., stir the reaction until the characteristic absorption peak of NCO is not detected in the infrared spectrum, and obtain the blocked isocyanate composition product; after testing, the product The chromaticity is 14 Hazen; the content of phenolic compounds in the product tested by HPLC analysis is 11ppm.

[0056] The obtained blocked isocyanate composition product was stored at 50° C. for 3 months, and the measured chromaticity value of the product is shown in Table 2.

Embodiment 2

[0058] (1) Add 200g of polyisocyanate Desmodur N3300, 0.20g of methyl p-toluenesulfonate, and 97.5g of Mobil S100 solvent oil into a four-neck flask, stir evenly under nitrogen protection, heat up to 90°C for 2 hours, and obtain alkylation treatment The final polyisocyanate is then cooled to 60°C;

[0059] (2) Add 92 g of butanone oxime to a four-necked flask, control the reaction temperature to 60-70° C., stir the reaction until the characteristic absorption peak of NCO is not detected in the infrared spectrum, and obtain the blocked isocyanate composition product; after testing, the product The chromaticity is 14 Hazen; the content of phenolic compounds in the product tested by HPLC analysis is 9ppm.

[0060] The obtained blocked isocyanate composition product was stored at 50° C. for 3 months, and the measured chromaticity value of the product is shown in Table 2.

Embodiment 3

[0062] (1) Add 200g of polyisocyanate Desmodur N3300, 0.02g of methyl p-toluenesulfonate, and 97.5g of Mobil S100 solvent oil into a four-neck flask, stir evenly under nitrogen protection, heat up to 90°C for 2 hours, and obtain alkylation treatment The final polyisocyanate is then cooled to 60°C;

[0063] (2) Add 92 g of butanone oxime to a four-necked flask, control the reaction temperature to 60-70° C., stir the reaction until the characteristic absorption peak of NCO is not detected in the infrared spectrum, and obtain the blocked isocyanate composition product; after testing, the product The chromaticity is 14 Hazen; the content of phenolic compounds in the product tested by HPLC analysis is 43ppm.

[0064] The obtained blocked isocyanate composition product was stored at 50° C. for 3 months, and the measured chromaticity value of the product is shown in Table 2.

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Abstract

The invention belongs to the technical field of isocyanate preparation, and particularly relates to a stably-stored blocked isocyanate composition, and a preparation method and an application thereof.The preparation method comprises the following steps: (1) mixing and heating polyisocyanate and an alkylation reagent to obtain alkylated polyisocyanate; and (2) contacting and reacting the alkylatedpolyisocyanate with a blocking agent to obtain the blocked isocyanate composition, wherein the blocking agent comprises at least one oxime compound. The preparation method can effectively improve thestorage stability of the isocyanate product blocked with the oxime compound and ensure the low chroma of the product.

Description

technical field [0001] The invention belongs to the technical field of isocyanate preparation, and in particular relates to a storage-stable blocked isocyanate composition and a preparation method and application thereof. Background technique [0002] Blocked isocyanate is produced by the reaction between isocyanate and blocking agent. The chemical bond formed between blocking agent and NCO is relatively weak, and it can unblock and release free NCO under certain conditions. Therefore, blocked isocyanates are widely used in one-component polyurethane coatings and adhesives, especially for automotive coatings and coil coatings. There are many types of blocking agents that can be used for isocyanate groups. Currently, commonly used blocking agents include phenolic compounds, alcohol compounds, oxime compounds, β-dicarbonyl compounds, pyrazole compounds, and amide compounds. [0003] Oxime compounds are widely used as isocyanate blocking agents because of their low unblocking ...

Claims

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Application Information

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IPC IPC(8): C08G18/28C08G18/80C09D175/04C09J175/04
CPCC08G18/286C08G18/8077C09D175/04C09J175/04
Inventor 李海军尚永华石滨刘照李金明朱智诚王暖程张晓鹏路富有黎源
Owner WANHUA CHEM GRP CO LTD
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