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TGIC (Triglycidyl Isocyanurate) production method based on fused steel belt granulation

A production method and product technology, applied in the field of TGIC production and processing, can solve the problems of reduced yield, intensified side reactions, and easy volatilization of methanol, and achieve high recovery and utilization, improved quality and yield, and uniform feeding speed Effect

Active Publication Date: 2018-07-20
HUANGSHAN JINFENG INDAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] First of all, in the current production process, the addition of solid alkali to the cyclization kettle is basically manual operation. When feeding, the epichlorohydrin in the reaction kettle is volatilized, and the pungent smell is heavy, which is extremely harmful to the health of workers.
In addition, manual feeding has a large amount of solid raw materials in a single feeding. In a short period of time, the stirring is uneven, and "explosion polymerization" is prone to occur, the side reactions are intensified, and the yield is reduced. Moreover, the control of the reaction temperature is all manual operation, and the temperature fluctuation range is large, which affects the product. quality and yield
During the cyclization reaction, most of the water exists in the product in the form of crystal water, which will also adversely affect the yield and purity of the subsequent TGIC
[0005] At the same time, after the solid-liquid separation of the TGIC produced in the cyclization kettle, the granulation process is generally manual. The granulation time is long and methanol is volatile, which not only causes waste, but also pollutes the environment and affects the health of workers.
In addition, the granulated TGIC products are generally dried by microwave vacuum, which is relatively fluffy and has a lot of powder, which may easily cause skin contact allergies of users.

Method used

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  • TGIC (Triglycidyl Isocyanurate) production method based on fused steel belt granulation
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  • TGIC (Triglycidyl Isocyanurate) production method based on fused steel belt granulation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] Example 1: Determination of the effect of cyclization kettle device B

[0051] 1. Production of TGIC (test group)

[0052] (1) Synthesis reaction: Add ECH, CA and tetramethylammonium chloride into synthesis kettle device A at a mass ratio of 7:1:0.03. The jacket A1 of the synthesis kettle was heated to 80°C with steam, and the synthesis reaction was carried out under normal pressure. The reaction was carried out for 5 hours until the mixed solution became clear and transparent, and the intermediate product: 1,3,5-tris(1'-chloro-2 '-hydroxy-propyl) isocyanurate.

[0053] (2) Cyclization reaction: add the above-mentioned intermediate product into the cyclization kettle device B, add solid alkali (99% NaOH), take the weight of the above added CA as 1, and add the weight of solid alkali as 1. The cyclization reaction is carried out under the condition of 30±5° C., and the reaction time is 1.5 h. For the specific cyclization operation, refer to the above step 2, cyclizati...

Embodiment 2

[0069] 1. Production of TGIC particles

[0070] (1) Synthesis reaction: Add ECH, CA and tetramethylammonium chloride into synthesis kettle device A at a mass ratio of 4:1:0.01. The jacket A1 of the synthesis kettle was heated to 80°C with steam, and the synthesis reaction was carried out under normal pressure. The reaction was carried out for 5 hours until the mixed solution became clear and transparent, and the intermediate product: 1,3,5-tris(1'-chloro-2 '-hydroxy-propyl) isocyanurate.

[0071] (2) Cyclization reaction: Add the above-mentioned intermediate product into the cyclization kettle device B, add solid alkali (99% NaOH), take the weight of the above added CA as 1, and add the weight of solid alkali to be 0.9. The cyclization reaction is carried out under the condition of 30±5° C., and the reaction time is 1.5 h.

[0072] (3) Primary separation: the TGIC mixture produced in step 2 is passed into the pressure filter device C for filtration, and the liquid phase obta...

Embodiment 3

[0085] 1. Production of TGIC particles

[0086] (1) Synthesis reaction: Add ECH, CA and tetramethylammonium chloride into synthesis kettle device A at a mass ratio of 7:1:0.03. The jacket A1 of the synthesis kettle was heated to 80°C with steam, and the synthesis reaction was carried out under normal pressure. The reaction was carried out for 5 hours until the mixed solution became clear and transparent, and the intermediate product: 1,3,5-tris(1'-chloro-2 '-hydroxy-propyl) isocyanurate.

[0087] (2) Cyclization reaction: add the above-mentioned intermediate product into the cyclization kettle device B, add solid alkali (99% NaOH), take the weight of the above added CA as 1, and add the weight of solid alkali as 1. The cyclization reaction is carried out under the condition of 30±5° C., and the reaction time is 1.5 h.

[0088] (3) Primary separation: the TGIC mixture produced in step 2 is passed into the pressure filter device C for filtration, and the liquid phase obtained ...

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Abstract

The invention belongs to the field of production and processing of TGIC, and in particular relates to a TGIC (Triglycidyl Isocyanurate) production method based on fused steel belt granulation. The TGIC production method comprises the specific steps: adding epichlorohydrin, cyanuric acid and a tetramethylammonium chloride catalyst into a reaction container; heating and carrying out synthetic reaction under normal pressure obtain an intermediate product; then adding solid alkali and carrying out cyclization reaction; filtering, standing and layering a cyclization reaction product; heating an organic phase of a lower layer and carrying out depressurization and distillation; crystallizing and centrifuging a distilled material to obtain a TGIC crystal containing volatile organic compounds; putting the TGIC crystal containing the volatile organic compounds into a vacuum environment and heating to obtain fused-state TGIC; dropping the fused-state TGIC on a pre-cooled steel belt granulation machine, and rapidly cooling the TGIC to from TGIC grains which have a firm texture and does not easily generate dust. The method provided by the invention is simple, and achieves a high byproduct repeated utilization rate and a high recycling rate; the prepared TGIC grains have the firm texture and a smooth surface, and are convenient to use.

Description

technical field [0001] The invention belongs to the field of TGIC production and processing, and in particular relates to a TGIC production method based on molten steel strip granulation. Background technique [0002] TGIC (triglycidyl isocyanurate, or: triglycidyl isocyanurate) is a curing agent used in powder coatings, due to its good thermal stability, good weather resistance, yellowing resistance Excellent, excellent mechanical properties and widely used. In the 1990s, the developed region of the Yangtze River Delta introduced TGIC water washing production technology from abroad. After ten years of development, the production and application of epoxy resin series products TGIC in my country have developed rapidly. However, with the development of the epoxy resin industry, in recent years, a large number of "three wastes" have been discharged in the production of TGIC, which has caused serious environmental pollution and brought enormous pressure to occupational health a...

Claims

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Application Information

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IPC IPC(8): C07D405/14
CPCC07D405/14
Inventor 洪昭雷吴锡成王建坤
Owner HUANGSHAN JINFENG INDAL
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