Looking for breakthrough ideas for innovation challenges? Try Patsnap Eureka!

Method for purifying triglycidyl isocyanurate

A technology of glycidyl ester and triglycidyl isocyanurate, which is applied in the field of purification of triglycidyl isocyanurate, can solve the problem of TGIC yield decline, high chlorine content of TGIC products, and the inability to completely avoid the residual sodium chloride salt in the by-product and other issues to achieve good water solubility

Pending Publication Date: 2022-04-12
湖南云科化工有限公司
View PDF4 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although this patented method can effectively avoid containing methanol in the product, the following problems still exist in this patented method: (1) due to the poor solubility of ethanol to sodium chloride salt, the chloride ion content in the TGIC product must be higher than the traditional method; (2) Since TGIC has a higher solubility in ethanol, if ethanol is used as a crystallization solvent, the yield of TGIC will inevitably decrease; (3) 48-630ppm of ECH residues still exist in the TGIC product obtained by the patented method
Although this patent method avoids the use of methanol, so that the methanol content in the product is 0, there are still the following problems: (1) directly using ECH as the crystallization solvent will inevitably increase the residual amount of ECH in the product; (2) ECH has a relatively strong dissolving ability for TGIC , part of the TGIC must be dissolved in the crystallization mother liquor, so that the yield decreases; (3) although organic bases are used as catalysts, it is impossible to completely avoid the residue of by-product sodium chloride salt
However, this method does not effectively remove methanol, and the addition of entrainer will inevitably introduce entrainer residue
In addition, the chlorine content of the TGIC product obtained by this method is still relatively high, ranging from 0.11% to 0.18%. not particularly high

Method used

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
View more

Image

Smart Image Click on the blue labels to locate them in the text.
Viewing Examples
Smart Image
  • Method for purifying triglycidyl isocyanurate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0034] The purification method of triglycidyl isocyanurate TGIC of the present embodiment comprises the following steps: a) Take 100.66 grams of commercially available TGIC product No. Heating speed to 95°C, keep warm for 30min; b) Add 70g of water at 25°C to the flask with distillation recovery solvent system, heat to boiling, distill 10g of water, triglycidyl isocyanurate TGIC crude product is dissolved in water to form a homogeneous mixed solution; c) cool the homogeneous mixed solution to 30°C at a cooling rate of 4°C / min, and crystals are precipitated; d) filter the crystals, and then wash them with 10 grams of deionized water to obtain washed crystals e) The cleaned crystals were heated and dried under vacuum at -0.05MPa and 80°C to obtain 99.16 grams of purified TGIC product with a yield of 98.5%. The product quality analysis and characterization results are shown in Table 1.

Embodiment 2

[0036] The purification method of triglycidyl isocyanurate TGIC of the present embodiment comprises the following steps: a) Take 180.89 grams of commercially available TGIC product No. Heating speed to 100°C, and keeping it warm for 40min; b) Add 200 grams of water at 85°C to a flask with a distillation recovery solvent system, heat to boiling, distill 20 grams of water, and dissolve the crude triglycidyl isocyanurate TGIC Form a homogeneous mixed solution in water; c) cool the homogeneous mixed solution to 20° C. at a cooling rate of 3° C. / min, and crystals are precipitated; d) filter the crystals, and then wash them with 30 grams of deionized water to obtain the washed Crystals; e) The cleaned crystals were heated and dried under vacuum at -0.08MPa and 70°C to obtain 176.45 grams of purified TGIC product with a yield of 97.5%. The product quality analysis and characterization results are shown in Table 1.

Embodiment 3

[0038] The purification method of triglycidyl isocyanurate TGIC of the present embodiment comprises the following steps: a) take commercially available TGIC product No. 2056.8 grams, join in the reactor with distillation recovery solvent system, with 4 DEG C / min Heat up to 95°C at a heating rate and keep it warm for 60 minutes; b) Add 3,500 grams of water at 95°C to a reaction kettle with a distillation recovery solvent system, heat to boiling, and steam 400 grams of water, triglycidyl isocyanurate TGIC The crude product is dissolved in water to form a homogeneous mixed solution; c) the homogeneous mixed solution is cooled to 10°C at a cooling rate of 2°C / min, and crystals are precipitated; d) the crystals are filtered, and then washed with 500 grams of deionized water to obtain a clean The cleaned crystals; e) The cleaned crystals were heated and dried under vacuum at -0.095MPa and 50°C to obtain 1974.5 grams of purified TGIC product with a yield of 96.0%. The product quality ...

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

PUM

No PUM Login to View More

Abstract

The invention relates to a method for purifying triglycidyl isocyanurate. The purification method comprises the following steps: adding a triglycidyl isocyanurate TGIC crude product into a reaction device with a distillation solvent recovery system, heating to 95-100 DEG C, and preserving heat; the method comprises the following steps: adding water into a reaction device with a solvent distillation and recovery system, heating until boiling, distilling off part of water, and dissolving a triglycidyl isocyanurate TGIC crude product in water to form a homogeneous mixed solution; cooling and separating out crystals; filtering and cleaning to obtain cleaned crystals; and drying to obtain the product. According to the purification method, the effective recovery rate of TGIC exceeds 95%; the TGIC quality is high, the epoxy equivalent is 99.5-100.6 g / mol, ECH residues, ethanol residues and methanol residues are all lower than 10 ppm, and the chlorine content is lower than 0.06%. The purification method greatly improves the antianaphylaxis and environmental protection property of the TGIC product.

Description

technical field [0001] The invention belongs to the field of chemical industry, in particular to a method for purifying triglycidyl isocyanurate. Background technique [0002] Triglycidyl isocyanurate (TGIC) is a heterocyclic polyepoxy compound with excellent heat resistance, weather resistance, light resistance, corrosion resistance, chemical resistance and mechanical properties, mainly used for carboxyl-containing The curing agent for polyester and carboxylic acrylic resin powder coatings can also be used in the manufacture of electrical insulating material laminates, printed circuits, various tools, adhesives, plastic stabilizers, etc. [0003] At present, the mainstream process for the industrial production of TGIC is a process route in which isocyanuric acid, epichlorohydrin (ECH) and caustic soda are used as raw materials. TGIC synthesized by the traditional process, considering that the product is obtained by cooling and crystallizing from methanol solvent, the resid...

Claims

the structure of the environmentally friendly knitted fabric provided by the present invention; figure 2 Flow chart of the yarn wrapping machine for environmentally friendly knitted fabrics and storage devices; image 3 Is the parameter map of the yarn covering machine
Login to View More

Application Information

Patent Timeline
no application Login to View More
IPC IPC(8): C07D405/14
Inventor 刘郁东刘良会钱文胜秦艳龙肖云飞
Owner 湖南云科化工有限公司
Who we serve
  • R&D Engineer
  • R&D Manager
  • IP Professional
Why Patsnap Eureka
  • Industry Leading Data Capabilities
  • Powerful AI technology
  • Patent DNA Extraction
Social media
Patsnap Eureka Blog
Learn More
PatSnap group products