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Preparation method of theic

A technology of Cyclic and cyanuric acid, applied in the direction of organic chemistry, can solve the problems of difficult purification, complicated process, long reaction cycle, etc., and achieve the effect of reducing the difficulty of purification, ensuring the purity of the product, and ensuring the recovery rate

Active Publication Date: 2021-02-02
山东键邦新材料股份有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to solve the problems of complex process, long reaction cycle, inconvenient recovery of excessive chlorohydrin and difficult purification when using chlorohydrin as raw material

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] A kind of preparation method of Sai Ke

[0043] S1: Mix cyanuric acid (129g, 1mol), TEA (5mol) and NaI (0.15mol) in DMF (900mL) evenly, heat to 80°C, add chloroethanol (3.15mol) dropwise into the reaction system, control During the dropwise addition, the system temperature was <85°C. After the dropwise addition was completed, the temperature was kept at 80°C for reaction. After the reaction was completed, the temperature was lowered, and the solvent was removed under reduced pressure to obtain the crude product of Sacchar.

[0044] S2: Add the crude product of Saike to methanol (520mL) with a water content of 20%, heat to reflux, keep for 20min, cool down to 25°C naturally, cool to 0°C in an ice bath, crystallize for 6h, and filter to obtain a water content of 5 % methanol, and dried to obtain 240.3 g of Saike fine product, with a purity of 98.3%.

Embodiment 2

[0046] A kind of preparation method of Sai Ke

[0047] S1: Mix cyanuric acid (129g, 1mol), Py (3.5mol) and KI (0.2mol) in DMSO (750mL) evenly, heat to 70°C, add chloroethanol (3mol) dropwise into the reaction system, control During the dropwise addition, the system temperature was <85°C. After the dropwise addition was completed, the temperature was maintained at 70°C for reaction. After the reaction was completed, the temperature was lowered, and the solvent was removed under reduced pressure to obtain the crude product of Sacchar.

[0048] S2: Add the crude Cyke product to ethanol (600mL) with a water content of 10%, heat to reflux, keep for 15min, cool down to 30°C naturally, cool down to 5°C in an ice bath, crystallize for 5h, and filter to obtain a water content of 5 % ethanol, and dried to obtain 248.2 g of Saike fine product, with a purity of 99.2%.

Embodiment 3

[0050] A kind of preparation method of Sai Ke

[0051] S1: Mix cyanuric acid (129g, 1mol), DBU (4mol) and KI (0.3mol) in DMA (650mL) evenly, heat to 60°C, add chloroethanol (3.1mol) dropwise into the reaction system, control During the dropwise addition, the system temperature was <85°C. After the dropwise addition was completed, the temperature was kept at 60°C for reaction. After the reaction was completed, the temperature was lowered, and the solvent was removed under reduced pressure to obtain the crude product of SEC.

[0052] S2: Add the crude Saike product into ethanol (770mL) with a water content of 30%, heat to reflux, keep for 10min, cool down to 25°C naturally, cool down to 5°C in an ice bath, crystallize for 4h, and then filter, the water content is 10 % ethanol, and dried to obtain 245.5 g of Saike fine product, with a purity of 98.7%.

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PUM

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Abstract

The invention relates to the field of organic chemical industry, in particular to a preparation method of tris (2-hydroxyethyl) isocyanurate. According to the method, a chloroethanol route is used, iodide ions are used as a catalyst, a proper feeding mode and a purification method are adopted, and the defects that the method is complex in process, long in reaction period and inconvenient in excessive recovery of chloroethanol are overcome. Iodine ions are used as a catalyst so that the temperature during the reaction of chloroethanol and cyanuric acid is reduced. Meanwhile, the equivalent chloroethanol is added in a dropwise adding manner so that the self reaction of the chloroethanol and the generation of impurities generated by the reaction of the theic and the chloroethanol are reduced,the operation is simple, the purification is convenient, and the industrial prospect is better.

Description

technical field [0001] The invention relates to the field of organic chemical industry, in particular to a preparation method of tris(2-hydroxyethyl)isocyanurate. Background technique [0002] Three (2-hydroxyethyl) isocyanurate is called Tri-(2-hydroxyethyl) isocyanurate in English, referred to as THEIC, commonly known as Sike. Saike is a nitrogen-containing aromatic heterocyclic polyol. The appearance of the product is white powder crystal, which is easily soluble in water, dimethylformamide (DMF), dimethylacetamide (DMA) and methylpyrrolidone Polar solvents, insoluble in ethanol, acetone and fatty solvents. Due to the presence of a stable triazine ring in the product structure of Saike, it has excellent chemical stability and thermal stability. The three hydroxyethyl groups have strong derivatization potential, basically the same properties as fatty alcohol hydroxyl groups, and are easy to react with other organic functional groups to form new compounds or polycondensat...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D251/34
CPCC07D251/34
Inventor 林永祥朱剑波
Owner 山东键邦新材料股份有限公司
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