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A kind of isocyanate stabilizer and preparation method thereof

A technology of isocyanate and stabilizer, applied in the field of isocyanate, can solve the problems of difficult to achieve stable storage of XDI, turbidity, poor stability effect, etc., and achieve the effects of improving long-term storage stability, preventing turbidity and increasing stability

Active Publication Date: 2022-07-12
WANHUA CHEM GRP CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] However, the above-mentioned stabilizers such as acid stabilizer perchloric acid, trifluoromethanesulfonic acid, carbon dioxide or acyl chloride have poor stabilizing effects on m-xylylene diisocyanate (XDI). It is known that XDI is due to self-polymerization Nylon-1 type polymers are formed and tend to become cloudy, and the currently used isocyanate stabilizers and the stabilizers disclosed in the above patents are difficult to achieve stable storage of XDI at room temperature for more than 1 month

Method used

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  • A kind of isocyanate stabilizer and preparation method thereof
  • A kind of isocyanate stabilizer and preparation method thereof
  • A kind of isocyanate stabilizer and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] The preparation method of isocyanate stabilizer, the steps are:

[0054] 20g of pure MDI was added to the reaction flask, dissolved in 400g of chlorobenzene, 29.2g of hydrogen chloride gas (MDI to hydrogen chloride molar ratio 1:10) was introduced at a rate of 10L / h, and the reaction temperature was controlled below 30°C. After the reaction was completed , the white solid in the reaction solution was separated by 0.3Mpa nitrogen pressure filtration, washed with fresh chlorobenzene and dried to obtain 25.5g of white solid material, namely the isocyanate stabilizer represented by formula (Ia), with a yield of 99.0%.

[0055] NMR data are 1 H NMR (400MHz, DMSO) δ9.15 (b, 1.2H), 7.59-7.50 (m, 4H), 7.25-7.20 (m, 4H), 3.96 (s, 2H); 13 C NMR (100MHz, DMSO): δ133.5, 133.4, 129.9, 127.6, 122.1, 41.3.

[0056]

Embodiment 2

[0058] The preparation method of isocyanate stabilizer, the steps are:

[0059] 20g of pure MDI was added to the reaction flask, dissolved in 400g of chlorobenzene, 7.30g of hydrogen chloride gas was introduced at a rate of 10L / h (molar ratio of MDI to hydrogen chloride 1:2.5), and the reaction temperature was controlled to <30°C. After the reaction was completed, IIIIV The white solid in the reaction solution was separated by 0.3Mpa nitrogen pressure filtration, washed with fresh chlorobenzene and dried to obtain 12.8g of white solid substance, namely the isocyanate stabilizer represented by formula (Ia), with a yield of 50.0%.

Embodiment 3

[0061] The preparation method of isocyanate stabilizer, the steps are:

[0062] 20g of pure MDI was added to the reaction flask, dissolved in 400g of chlorobenzene, 64.7g of hydrogen bromide gas (MDI to hydrogen bromide molar ratio 1:10) was introduced at a rate of 10L / h, and the reaction temperature was controlled to <30°C, After the reaction was completed, the white solid in the reaction solution was separated by 0.3Mpa nitrogen pressure filtration, washed with fresh chlorobenzene, and dried to obtain 32.3g of white solid matter, namely the isocyanate stabilizer represented by formula (Ib), with a yield of 98.0%.

[0063] NMR data are 1 H NMR (400MHz, DMSO) δ9.17 (b, 1.2H), 7.59-7.51 (m, 4H), 7.26-7.20 (m, 4H), 3.94 (s, 2H); 13 C NMR (100MHz, DMSO): δ133.4, 129.9, 127.6, 125.5, 122.1, 41.3.

[0064]

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Abstract

The present invention relates to an isocyanate stabilizer and a preparation method thereof. The structure of the isocyanate stabilizer is shown in the general formula (I). The stabilizer of the present invention is synthesized through a one-step reaction, and can be obtained after separation and purification. The preparation method is simple, and is suitable for improving the storage stability of isocyanates, especially XDI, and prolonging the storage time of isocyanates. , the isocyanates with this kind of stabilizer can be used in the synthesis of optical resins.

Description

technical field [0001] The invention belongs to the technical field of isocyanates, and relates to an isocyanate stabilizer and a preparation method thereof. Background technique [0002] Among isocyanate compounds, due to the high reactivity of isocyanate groups, they tend to turn yellow or self-polymerize during storage, which affects downstream applications, so adding stabilizers to inhibit isocyanate yellowing and self-polymerization is essential. [0003] At present, the representative of isocyanate compound stabilizers is hindered phenolic compounds. For example, US Patent No. US3715381 discloses 2,6-di-tert-butyl-4-methylphenol (BHT) as an isocyanate stabilizer, and the Japanese publication number is JP33438 / 1970. The patent reports phosphites such as triphenyl phosphite antioxidants, both of which have good effects and are still widely used. [0004] In addition, many other stabilizers are also known, such as Japanese Patent JPS5036546 discloses substituted urea as ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C263/18C07C265/14C07C265/12C07C265/04C07C265/08C07C269/00C07C271/04C08G18/80C08G18/71
CPCC07C263/18C07C265/14C07C265/12C07C265/04C07C265/08C07C269/00C07C271/04C08G18/8087C08G18/712C07C2601/14
Inventor 朱付林李建峰尚永华陈浩刘照郑兵吴谦宋国毅黎源
Owner WANHUA CHEM GRP CO LTD