Preparation method of hydrogenated xylylene diisocynate

A technology for hydrogenating xylylene diisocyanate and cyclohexyldimethylamine, which is applied in the preparation of isocyanic acid derivatives, organic compounds, chemical instruments and methods, etc., can solve the problems of unindustrialization, severe amine coating, Solvent problems such as large amount, to achieve stable quality, improved dispersion and fluidity, and high product quality

Active Publication Date: 2017-05-17
HUNAN HAILI CHEM IND
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This patent has the disadvantages of severe amine coating and many by-products.
[0010] Similar to the British patent GB1086782, a method for forming a salt of xylylenediamine in an inert organic solvent is disclosed. This patent has the disadvantages of large amount of solvent and low conversion rate.
[0011] Similar to the British patent GB1146664A also discloses a method for forming a salt of xylylenediamine, the method provided by this patent has the disadvantage of being unindustrializable

Method used

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  • Preparation method of hydrogenated xylylene diisocynate

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Embodiment 1

[0036] A preparation method of hydrogenated xylylene diisocyanate of the present invention, comprises the following steps:

[0037] (1) Salt-forming reaction: At room temperature, first add 250 grams of toluene, 250 grams of concentrated hydrochloric acid with a concentration of 36%, and 30 grams of water into a 1L reactor, start the reactor to stir, and start to drop 1,3-cyclo Hexamethylene dimethylamine, keep the reaction temperature at 20°C, after 142 grams of 1,3-cyclohexanedimethylamine is added dropwise, keep it warm for 0.5h, then raise the temperature, reflux for dehydration, after dehydration is complete, the reaction solution enters the filter device and filters , to obtain the amine salt, the mother liquor is used mechanically, the amine salt is transferred to a vacuum drying device, and dried to obtain a solid product of the amine salt;

[0038] (2) Photochemical reaction: transport the amine salt obtained above to a 2L reactor, add 1300 grams of xylene and 0.5 gra...

Embodiment 2

[0041] A preparation method of hydrogenated xylylene diisocyanate of the present invention, comprises the following steps:

[0042] (1) Salt-forming reaction: At room temperature, first add 250 grams of toluene, 250 grams of concentrated hydrochloric acid with a concentration of 36%, and 30 grams of water into a 1L reactor, start the reactor to stir, and start to drop 1,3-cyclo Hexamethylene dimethylamine, keep the reaction temperature at 20°C, wait until 142 grams of 1,3-cyclohexanedimethylamine is added dropwise, keep the temperature for 0.5h, then raise the temperature, reflux for dehydration, after the dehydration is complete, the reaction liquid enters the filter device, filters, The amine salt is obtained, the mother liquor is used mechanically, the amine salt is transferred to a vacuum drying device, and dried to obtain a solid product of the amine salt;

[0043] (2) Photochemical reaction: transport the amine salt obtained above to a 2L reactor, add 1300 g of chloroben...

Embodiment 3

[0046] A preparation method of hydrogenated xylylene diisocyanate of the present invention, comprises the following steps:

[0047] (1) Salt-forming reaction: At room temperature, first add 250 grams of toluene, 250 grams of concentrated hydrochloric acid with a concentration of 36%, and 30 grams of water into a 1L reactor, start the reactor to stir, and start to drop 1,3-cyclo Hexamethylene dimethylamine, keep the reaction temperature at 20°C, wait until 142 grams of 1,3-cyclohexanedimethylamine is added dropwise, keep the temperature for 0.5h, then raise the temperature, reflux for dehydration, after the dehydration is complete, the reaction liquid enters the filter device, filters, The amine salt is obtained, the mother liquor is used mechanically, the amine salt is transferred to a vacuum drying device, and dried to obtain a solid product of the amine salt;

[0048] (2) Photochemical reaction: transport the amine salt obtained above to a 2L reactor, add 1300 g of trichloro...

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Abstract

The invention discloses a preparation method of hydrogenated xylylene diisocynate. The preparation method of the hydrogenated xylylene diisocynate comprises the following steps: (1) performing salt forming reaction on 1,3-cyclohexanol dimethylamine and concentrated hydrochloric acid in a two-phase reaction solvent to obtain amine salt, wherein the two-phase reaction solvent consists of water and an inert organic solvent insoluble in water ; (2) performing photochemical reaction on the ammonium salt obtained in the step (1) and phosgene in an inert solvent by taking N,N-dimethylformamide or N,N-dimethylacetamide as a catalyst to obtain reaction liquid, and performing aftertreatment on the reaction liquid to obtain the hydrogenated xylylene diisocynate. The preparation method of the hydrogenated xylylene diisocynate has the advantages of complete ammonium salt formation, small grain size of the ammonium salt, low viscosity of the ammonium salt, high space-time conversion rate of photochemical reaction, simple process, low cost and the like.

Description

technical field [0001] The invention belongs to the technical field of isocyanate preparation, in particular to a method for preparing hydrogenated xylylene diisocyanate. Background technique [0002] Hydrogenated xylylene diisocyanate (H 6 XDI), the chemical structural formula is: [0003] [0004] Relative molecular weight 194.23, H at room temperature 6 XDI (mixture of isomers) is a colorless transparent liquid with a pungent odor, a boiling point of 294.4°C (760mm Hg), a density of 1.101g / mL (25°C), a flash point of 159°C, and a refractive index of 1.485. [0005] The polyurethane prepared by hydrogenated xylylene diisocyanate has the same yellowing resistance as that produced by HDI and IPDI. Hydrogenated xylylene diisocyanate and HDI are equally reactive. Due to its ring structure, its properties during curing, such as fast surface drying and hardness of cured products, are basically similar to IPDI, with excellent weather resistance and color stability. Polyme...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C263/10C07C263/20C07C265/14
CPCC07C263/10C07C263/20C07C265/14
Inventor 刘国文罗先福周锦萍王燕周亮臧阳陵
Owner HUNAN HAILI CHEM IND
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