Toluene diisocyanate trimer preparation method

A technology of toluene diisocyanate and toluene diisocyanate containing toluene diisocyanate is applied in the field of preparing toluene diisocyanate trimer, can solve the problems of strong corrosiveness of phenolic compounds, high production condition requirements, increase production cost and the like, and achieves narrow molecular mass distribution, The effect of improving quality and yield, and easy separation

Inactive Publication Date: 2008-07-02
GUANGZHOU INST OF GEOCHEMISTRY - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the strong corrosiveness and toxicity of the phenolic compounds involved, high production conditions are required in the production process, thereby increasing the production cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Weigh 10g of sodium montmorillonite whose particle size is controlled to be less than 60 microns and 210g of distilled water to make a suspension, and 5g of cetyltrimethylammonium bromide to make a 10% aqueous solution with a mass fraction of distilled water. Add the aqueous solution of cetyltrimethylammonium bromide to the suspension of montmorillonite and stir at 70°C for 3 hours, filter and wash with distilled water repeatedly until the filtrate is washed with 0.1mol / L AgNO 3 Test without Br - . The obtained organic montmorillonite was vacuum-dried in a vacuum oven at 60° C. for 24 hours, ground by a ball mill, and sieved to control the particle size to be less than 60 microns.

[0019] Add 25g of toluene diisocyanate into a three-necked flask containing 75g of anhydrous butyl acetate, stir at 50°C for 15min, and measure the -NCO content by sampling with di-n-butylamine titration. Add 1g of organic montmorillonite, stir, control the temperature at about 50°C, react...

Embodiment 2

[0021] The preparation method of organomontmorillonite is the same as in Example 1.

[0022] Add 5 g of toluene diisocyanate into a three-neck flask containing 95 g of toluene, stir at 20°C for about 1 min, and measure its -NCO content by di-n-butylamine titration. Add 0.5g of organic montmorillonite, stir, control the temperature at about 30°C, react for 8 hours to terminate the reaction, centrifuge and take the supernatant to obtain the product. -1 、1420cm -1 、760cm -1 There is a characteristic absorption peak of isocyanurate, 13 The peak of C-NMR spectrum δ148.6-δ149.1 belongs to the carbonyl peak in trimeric isocyanurate, indicating that the product is toluene diisocyanate trimer. Product yield 7.2%.

Embodiment 3

[0024] Organomontmorillonite with the brand name HFGEL-140 was purchased from Zhejiang Fenghong Clay Chemical Co., Ltd.

[0025] Add 50g of toluene diisocyanate into a three-necked flask containing 50g of anhydrous butyl acetate, stir at 100°C for about 60min, and measure its -NCO content by di-n-butylamine titration. Add 10 g of organic montmorillonite, stir, control the temperature at about 100° C., react for 1 hour to terminate the reaction, and centrifuge to obtain the supernatant to obtain the product. at 1709cm -1 、1420cm -1 、760cm -1 There is a characteristic absorption peak of isocyanurate, 13 The peak of C-NMR spectrum δ148.6-δ149.1 belongs to the carbonyl peak in trimeric isocyanurate, indicating that the product is toluene diisocyanate trimer. Product yield 39%.

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Abstract

The invention relates to preparation method of TDI trimer, which comprises: adding organic montmorillonite as catalyst into the TDI liquid with mass as 0.5~10% of the liquid; at 20~100Deg, taking polymerisation to obtain the product solution; or distilling and removing solvent to obtain the pure product. This invention uses the catalyst with a little toxicity and causticity, reduces cost, and hias high quality and yield.

Description

technical field [0001] The invention relates to a preparation method of toluene diisocyanate trimer, in particular to a method for preparing toluene diisocyanate trimer by using organic montmorillonite as a catalyst. Background technique [0002] The toluene diisocyanate trimer (isocyanurate) prepared by the trimerization of toluene diisocyanate (TDI) has high heat resistance, and at the same time greatly reduces the volatility of toluene diisocyanate and hexamethylene diisocyanate (HDI). Toxicity of monomers. At present, toluene diisocyanate trimer has been widely used in quick-drying and high-decorative wood lacquers. The coatings using it as curing agent have the characteristics of quick-drying, high temperature resistance and good weather resistance. [0003] Catalysts commonly used in the preparation of toluene diisocyanate trimer are organometallic compounds such as organic basic compound, alkali metal salt, organophosphorus, organotin, organotitanium at present, docu...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D251/34
Inventor 庞浩廖兵曹悠黄文勇胡美龙
Owner GUANGZHOU INST OF GEOCHEMISTRY - CHINESE ACAD OF SCI
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