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Method for preparing electronic grade triglycidyl isocyanurate

A technology of triglycidyl isocyanurate, applied in the direction of organic chemistry, can solve problems such as endangering the physical and mental health of workers, affecting product yield and quality, and complicated distillation steps, so as to avoid a large number of direct contact and recycling Simple and easy, high yield effect

Active Publication Date: 2016-10-12
HUANGSHAN HUAHUI TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the operation of the distillation step in this process is too complicated, and errors in the operation will also lead to a slightly higher residual amount of ECH
[0007] It can be seen that in the existing process for preparing TGIC products, due to the large amount of solvent epichlorohydrin (ECH), the yield and quality of the product are seriously affected, and the residual solvent volatilizes into the air, pollutes the environment, and endangers the physical and mental health of operators. , while wasting the solvent, leading to an increase in production costs

Method used

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  • Method for preparing electronic grade triglycidyl isocyanurate
  • Method for preparing electronic grade triglycidyl isocyanurate

Examples

Experimental program
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Embodiment 1

[0028] The method for preparing described TGIC product in the present embodiment comprises the steps:

[0029] (1) Add 200Kg of cyanuric acid, 1003Kg of epichlorohydrin, 20Kg of benzyltriethylammonium chloride, and 20Kg of methanol into the reaction kettle and mix well, and heat the mixture system to 110°C, and Carry out the reaction for about 5 hours until the mixed solution gradually becomes clear and transparent, and then carry out vacuum distillation to remove unreacted ECH according to the conventional method in the prior art;

[0030] (2) Transfer the synthesis solution after the reaction in step (1) to the cyclization kettle, add 1000Kg of methanol solvent and mix evenly, and add 200Kg of caustic soda in 4 times, control the reaction temperature at 20°C for 110min; cyclization After the reaction is over, centrifuge and perform solid-liquid separation to obtain a solid mixture of TGIC products and salts and methanol mother liquor;

[0031] (3) Collect the solid mixture ...

Embodiment 2

[0033] The method for preparing described TGIC product in the present embodiment comprises the steps:

[0034] (1) Add 200Kg of cyanuric acid, 574Kg of epichlorohydrin, 16Kg of benzyltriethylammonium chloride, and 10Kg of methanol into the reaction kettle and mix well, and heat the mixture system to 90°C, and Carry out the reaction for about 3 hours until the mixed solution gradually becomes clear and transparent, and then carry out vacuum distillation to remove unreacted ECH;

[0035](2) Transfer the synthesis solution after the reaction in step (1) to the cyclization kettle, add 1600Kg of methanol solvent and mix evenly, and add 217Kg of caustic soda in 3 times, control the reaction temperature at 25°C for 120min; cyclization After the reaction is over, centrifuge and perform solid-liquid separation to obtain a solid mixture of TGIC products and salts and methanol mother liquor;

[0036] (3) Collect the solid mixture after solid-liquid separation, add 2070Kg of water to was...

Embodiment 3

[0038] The method for preparing described TGIC product in the present embodiment comprises the steps:

[0039] (1) Add 200Kg of cyanuric acid, 717Kg of epichlorohydrin, 8Kg of benzyltriethylammonium chloride, and 10Kg of methanol into the reaction kettle and mix well, and heat the mixture system to 100°C, and Carry out the reaction for about 4 hours until the mixed solution gradually becomes clear and transparent, and then carry out vacuum distillation to remove unreacted ECH;

[0040] (2) Transfer the synthetic solution after the reaction in step (1) to the cyclization kettle, add 1000Kg of methanol solvent and mix well, and add 186Kg of caustic soda in 4 times, control the reaction temperature at 15°C for 90min; cyclization After the reaction is over, centrifuge and perform solid-liquid separation to obtain a solid mixture of TGIC products and salts and methanol mother liquor;

[0041] (3) Collect the solid mixture after solid-liquid separation, add 1655Kg of water to wash ...

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Abstract

The invention belongs to the technical field of preparation of chemical preparations and in particular relates to a novel method for preparing electronic grade triglycidyl isocyanurate. The method for preparing electronic grade triglycidyl isocyanurate provided by the invention uses a conventional two-step method in the prior art for preparation; commonly used cyanuric acid and epichlorohydrin are selected as reaction raw materials; methanol as a co-solvent is creatively added to the synthesis reaction steps, to promote the heterogeneous reaction between a solid phase cyanuric acid and a liquid phase ECH; methanol is added in a cyclization reaction step to effectively reduce the dosage of ECH, thereby greatly improving the ECH recovery efficiency and reducing the unit consumption and production energy consumption of ECH.

Description

technical field [0001] The invention belongs to the technical field of preparation of chemical preparations, and in particular relates to a new method for preparing electronic-grade triglycidyl isocyanurate. Background technique [0002] Triglycidyl isocyanurate (TGIC), chemically known as tris(2,3-epoxypropyl)-s-triazine-2,4,6-(1H-3H-5H)-trione, is A heterocyclic compound, because it contains three epoxy groups and a triazine ring structure, and has high functionality, reactivity, and excellent chemical and thermal stability, it is used as an excellent curing agent Widely used in all walks of life, especially in printed circuit boards (PCB), it is an irreplaceable curing agent. Due to the stable triazine ring structure in the TGIC molecule, the TGIC powder coating has good heat resistance and weather resistance; at the same time, the amide group in the triazine ring makes it easy to crystallize into crystals, suitable for large-scale industrial applications Production. I...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D405/14
CPCC07D405/14
Inventor 汤增荣杨志萍方向宏何领王永垒商永嘉
Owner HUANGSHAN HUAHUI TECH
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