- Study of methods of preparation of 1,4-diglycidyltetrazolone. New synthesis of triglycidylisocyanurate
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1,4-Diglycidyltetrazolone was synthesized for the first time by the reaction of tetrazolone and epichlorohydrin with subsequent treatment of the products of addition with a base. The basic directions of the reaction of carbamoyl azide with epichlorohydrin, which yields triglycidylisocyanurate and diglycidylcarbamoyl azide, were investigated. The features of the synthesis and properties of the substances obtained were described. 1996 Plenum Publishing Corporation.
- Korotkikh,Korotkikh
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- Synthesis method of high-purity tris (glycidyl) isocyanurate
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The invention discloses a synthesis method of high-purity tris (glycidyl) isocyanurate. The method comprises the following steps: (1) adding cyanuric acid, a catalyst and a polar solvent into a reactor, and uniformly mixing; (2) dropwise adding epoxy chloropropane to react with cyanuric acid, and separating to obtain an intermediate; (3) reacting the intermediate and calcium oxide in an organic medium; and (4) separating while the product is hot, removing solids, cooling and crystallizing the liquid, and separating to obtain the product TGIC. According to the method, the hydrolysis side reaction of the product and an intermediate product is effectively controlled, so that the product yield reaches 96% or above, and the purity reaches 99%.
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Paragraph 0027-0059
(2021/07/14)
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- Low-chlorine electronic-grade TGIC and preparation method thereof
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The invention belongs to the technical field of curing agents, and particularly relates to a method for preparing low-chlorine electronic-grade TGIC and a high-purity byproduct sodium chloride at low cost. According to the method for preparing the low-chlorine electronic-grade TGIC at low cost, sodium cyanate and epoxy chloropropane are used as reaction raw materials, catalysis is carried out at a high temperature by using a transfer catalyst, and a substitution reaction of the sodium cyanate and the epoxy chloropropane and a trimerization cyclization reaction of a reaction intermediate are sequentially carried out, so that the required TGIC product is prepared. In the whole reaction, the epichlorohydrin is used as a reaction raw material and a reaction solvent at the same time, other solvents or water do not need to be additionally introduced, the reaction can be carried out at high temperature, the reaction efficiency is improved, the condition of ring opening of epoxy groups of the product caused by a large amount of water in the system is avoided, few by-products are generated in the whole reaction, the yield of the target product is high, and the purity of the prepared TGIC product is high.
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Paragraph 0023-0046
(2021/08/21)
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- Preparation method of triglycidyl isocyanurate
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The invention relates to a preparation method of triglycidyl isocyanurate. The preparation method comprises the steps that cyanuric acid and dichloropropanol are subjected to a heating reaction in thepresence of alkali and a solvent, the molar ratio of cyanuric acid to dichloropropanol is 1: 2 to 8, and the molar ratio of the addition amount of alkali to the addition amount of dichloropropanol is2: 1. The raw material conversion rate of the triglycidyl isocyanurate prepared by the method is high and reaches 95% or above, the product selectivity is good and reaches 95% or above, and the product yield is high and reaches 90% or above and is far higher than the yield of about 80% in the prior art.
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Paragraph 0038-0051
(2021/02/06)
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- Method for synthesizing TGIC and coproducing ECH from dichloropropanol
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The invention provides a method for synthesizing TGIC and coproducing ECH from dichloropropanol. The method comprises the following steps: (1) proportionally adding cyanuric acid, dichloropropanol, aquaternary ammonium salt phase transfer catalyst and water, heating and stirring the mixture and carrying out temperature control reaction in stages, heating and stirring the mixture to a certain temperature, carrying out heat preservation reaction for a period of time, heating the mixture, carrying out heat preservation reaction for a period of time, and cooling a reaction product; (2) in the reaction system in the step (1), adjusting the vacuum degree, dropwise adding liquid caustic soda while carrying out steam stripping with water within a certain period of time, carrying out heat preservation reaction for a period of time after dropwise adding is finished, and then removing solid salt through plate-and-frame filter pressing; (3) carrying out reduced pressure distillation on the filtrate obtained in the step (2) to remove ECH, and collecting a crude product TGIC from the kettle liquid; (4) recrystallizing the crude product TGIC in an organic solvent for a period of time under a low-temperature condition, and then centrifugally separating, washing and drying the product to obtain a TGIC product. According to the treatment method disclosed by the invention, the cost of TGIC can be effectively reduced, an important organic chemical raw material ECH is co-produced, and the method is low-carbon and environment-friendly.
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Paragraph 0033; 0035-0037; 0039-0041; 0043-0045; 0047-0049
(2020/11/23)
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- Method for preparing triglycidyl isocyanurate (TGIC)
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The invention relates to a method for preparing triglycidyl isocyanurate (TGIC). The method is characterized in that the TGIC is prepared from sodium cyanate, which serves as a raw material, through substitution and condensation reactions. The method specifically comprises the following steps of proportionally mixing sodium cyanate, epichlorohydrin, a benzyl bromide organic catalyst, 30% hydrogen peroxide and a polar solvent in a reactor in one time, carrying out stirring for 10 minutes at room temperature, then, carrying out heating, controlling the temperature to 70 DEG C to 90 DEG C, carrying out a reflux reaction for 3 to 5 hours, and then, carrying out aftertreatment, thereby obtaining the TGIC. According to the method, a one-pot method preparation process is adopted, so that process flows are simple and quick; the raw materials are readily available and easily stored, and the reactions are carried out at normal pressure, so that when industrialization is achieved, the equipment investment and labor can be reduced, and the production cost is reduced; and the TGIC prepared by the method is high in yield and high in purity.
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Paragraph 0012
(2017/08/28)
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- Preparation isocyanuric acid and three-glycidyl ester of the new method (by machine translation)
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The invention discloses a method for preparing isocyanuric acid and three-glycidyl ester method, comprises the following steps: (1) isocyanuric acid with sodium hydroxide solution under low temperature conditions the reaction, pH value of the reaction system is maintained at 4 - 6 between, and by reduced pressure distillation and continuously evaporated water content in the reaction system, to obtain the isocyanuric acid and three sodium salt; (2) isocyanuric acid trisodium salt after fully dried, in the presence of a phase transfer catalyst in reaction with the excess epichlorohydrin, glycidyl ester crude product obtained three polyisocyanurates; (3) by reduced pressure distillation and excess of epichlorohydrin, the methanol solvent is cooled and crystallized, get the isocyanuric acid and three glycidyl ester pure product. The method of the invention more effectively solves the problem of chlorine-containing waste water sewage treatment problem, while at the same time guarantee the product yield, and reducing the production cost; and the product can meet the National standard. The method of the invention simple process, equipment investment is not large, and is suitable for universal use. (by machine translation)
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Paragraph 0013-0016
(2017/07/23)
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- Electronic grade of a kind of preparation method of three isocyanuric acid glycidyl (by machine translation)
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The invention belongs to the technical field of chemical preparation, in particular relates to a preparation of electronic grade isocyanuric acid new method for three-glycidyl ester. The invention relates to a method of preparation of electronic grade TGIC, by the prior art conventional in the preparation is carried out by the two-step, cyanuric acid is a commonly used as the raw materials of reaction with epichlorohydrin, and creativity in the synthetic reaction step, by adding methanol as a cosolvent, ECH solid phase cyanogen uric acid and liquid phase in order to promote a non-homogeneous reactions are carried out, and because the cyclization reaction step of the addition of the methanol, effectively reduces the amount of the feeding ECH, thereby greatly improving the efficiency of recovery ECH, and reduce the energy consumption of the unit consumption of ECH. (by machine translation)
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Paragraph 0026; 0040; 0041
(2017/01/17)
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- A method for producing three isocyanuric acid glycidyl
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The invention relates to a triglycidyl isocyanurate production method comprising the steps of synthesizing, distillation, crystallization, centrifugation, and drying. Especially, in the distillation process, a solvent which has a boiling point lower than 110 DEG C, which can be subjected to binary azeotrope with epoxy chloropropane, and which cannot be subjected to a reaction with components of the reaction system is slowly added, wherein an addition amount is 5-10% of that of a triglycidyl isocyanurate crude product. The materials are stirred for 20min; through reduced-pressure distillation under a vacuum degree of -0.090MPa to -0.0999MPa, solvent and epoxy chloropropane are removed by azeotrope, wherein a temperature is controlled under 95 DEG C. With the method, preparation process conditions are mild, all ECH solvent can be recovered, working environment can be improved, production cost can be reduced, and the process is stable and safety. Various performance indexes of the product are excellent. With the triglycidyl isocyanurate production method, no epoxy chloropropane residue is caused.
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Paragraph 0018-0027; 0058
(2017/02/23)
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- HIGHLY SOLUBLE TRIS-(2,3-EPOXYPROPYL)-ISOCYANURATE AND METHOD FOR PRODUCING SAME
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There is provided an epoxy composition which has difficulty in precipitating a crystal during storage, is homogeneous and can be stored for a long period; and a cured product of the composition having excellent transparency, heat resistance, and light resistance can be obtained on curing. An α-type tris-(2,3-epoxypropyl)-isocyanurate crystal comprising β-type tris-(2,3-epoxypropyl)-isocyanurate in the crystal in a ratio of 2% by mass to 15% by mass. A method for producing the α-type tris-(2,3-epoxypropyl)-isocyanurate crystal comprising step (i) separating β-type tris-(2,3-epoxypropyl)-isocyanurate contained in a tris-(2,3-epoxypropyl)-isocyanurate solution from the solution as a solid to obtain a crystal with an increased content ratio of α-type tris-(2,3-epoxypropyl)-isocyanurate.
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Paragraph 0084-0086
(2015/12/04)
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- METHOD FOR PRODUCING EPOXY COMPOUND
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There is provided a method for producing an epoxy compound having an epoxy ring bonded to a triazinetrione ring via a long chain alkylene group, an olefin compound having a specific structure is used to efficiently obtain an epoxy compound of which an olefin moiety is epoxidized in high yield. A method for producing an epoxy compound of Formula (2): comprising reacting a triolefin compound of the following Formula (1): (In the above-mentioned Formulae, R1 to R9 are each independently a hydrogen atom or a methyl group; and n1 to n3 are each independently an integer of 1 to 4) with hydrogen peroxide, a nitrile compound, and an alkaline substance in a solvent. The nitrile compound is an aliphatic nitrile compound or an aromatic nitrile compound. The alkaline substance is phosphate, carbonate, or an alkaline metal hydroxide.
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Paragraph 0073; 0074
(2015/09/23)
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- PROCESS FOR PREPARATION OF TRIGLYCIDYL ISOCYANURATE (TGIC)
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The present invention relates to an improved process for the preparation of 1,3,5-triazine-2,4,6(1H,3H,5H)-trione (“Triglycidylisocyanurate (TGIC) or the compound of formula I”) comprising reacting cyanuric acid (the compound of formula III) with 3 to 7 molar equivalents of epichlorohydrin in an autoclave at a temperature of 80-100° C. for 1 hour to give the mixture of intermediates A, B and C and reacting intermediates A, B and C with an alkali to obtain the compound of formula I.
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Paragraph 0044
(2015/09/22)
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- Optically active epoxy compound
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Optically active β-type tris-(2,3-epoxypropyl)-isocyanurate is obtained by a method of reacting isocyanuric acid with an optically active epihalohydrin, or a method of optically resolving a racemic modification of tris-(2,3-epoxypropyl)-isocyanurate by using an amylose or cellulose derivative. It is a method for producing a high melting point type tris-(2,3-epoxypropyl)-isocyanurate obtained by mixing two enantiomers of optically active β-type tris-(2,3-epoxypropyl)-isocyanurate.
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- Method for reducing an organic solvent remaining in beta-form tris- (2,3,-epoxypropyl) - isocyanurate crystals
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A process for producing β-form tris-(2,3-epoxypropyl)-isocyanurate crystals containing from 2 to 15 wt % of a-form tris-(2,3-epoxypropyl)-isocyanurate in the interior of the crystals, which comprises the following steps (A), (B), (C) and (D): (A) a step of reacting cyanuric acid with epichlorohydrin to form an addition product of cyanuric acid and epichlorohydrin, followed by dehydrochlorination to obtain a reaction solution containing tris-(2,3-epoxypropyl)-isocyanurate, (B) a step of removing epichlorohydrin from the reaction solution containing tris-(2,3-epoxypropyl)isocyanurate obtained in step (A), and dissolving the obtained tris-(2,3-epoxypropyl)-isocyanurate in a solvent, (C) a step of gradually cooling the liquid obtained in step (B) at a cooling rate within 20° C./hr for crystallization, followed by filtration to obtain crystals, and (D) a step of washing and drying the crystals obtained in step (C).
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- beta -form tris-(2, 3-epoxypropyl)-isocyanurate crystals and process for their production
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beta -form tris-(2,3-epoxypropyl)-isocyanurate crystals containing from 2 to 15 wt % of alpha -form tris-(2,3-epoxypropyl)-isocyanurate in the interior of the crystals.
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- Isocyanuric acid derivatives, method of preparation, therapeutic compositions with a cytostatic action and therapeutic method
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N-substituted-diglycidyl-isocyanurates having the formula: STR1 wherein R represents a hydrocarbon-containing radical selected from the group consisting of alkyl, aryl, aralkyl, alkaryl and cycloalkyl, optionally containing: (a) heterocycles except epoxides, and unsaturation, and (b) substituents selected from the group consisting of halogen, hydroxyl, amino, N-substituted amino, mercapto, alkylmercapto, arylmercapto, alkylsulfoxy, arylsulfoxy, alkoxy, aryloxy and acyloxy, and R1 represents a member selected from the group consisting of hydrogen and alkyl having from 1 to 4 carbon atoms, as well as the method for preparing said N-substituted-diglycidyl-isocyanurates, therapeutic compositions with cytostatic action comprising said N-substituted-diglycidyl-isocyanurates, and a method of treatment of malignant neoplasias in warm-blooded animals by administering a therapeutically effective amount of said N-substituted-diglycidyl-isocyanurate.
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- Isomers of Triglycidylisocyanurates - 1.
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Results of an experimental study are presented in which triglycidylisocyanurate was prepared from cyanuric acid and epichlorhydrin, crystallized, and purified by recrystallization. Polymer obtained consisted of two isomers, alpha and beta, which have been separated by utilizing their different solubility parameters in various solvents. Physical and thermal properties of individual isomers have been determined and NMR spectra for both forms were compared with results obtaining by DTA methods.
- Joel,Becker
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p. 237 - 239
(2007/10/09)
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