77-93-0Relevant articles and documents
Citrate plasticizer
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Paragraph 0066-0068, (2021/05/15)
The invention discloses a citrate plasticizer and a preparation method thereof, and the preparation method of citrate comprises the following steps: firstly, citric acid and alcohol react to prepare citric acid triester, and then dianhydride acylation is carried out to prepare carboxyl-containing citric acid triester. After chlorination, the carboxyl-containing citric acid triester and the tris(2-ethoxyl) isocyanurate are subjected to esterification reaction to prepare triester citrate containing the isocyanurate. According to the present invention, the preparation method has characteristics of simple operation, wide raw material source and mild reaction condition, and meets the industrial production, the prepared triester citrate containing isocyanurate has a good plasticizing effect and excellent thermal stability, low-temperature flexibility, solvent extraction resistance, migration resistance and flame retardance, and can be widely applied to plastic rubber plasticizers.
The preparation method of the triethyl citrate
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Paragraph 0037-0050, (2019/07/04)
The invention relates to a method for preparing triethyl citrate, and belongs to the technical field of pharmacy. The method includes that steps that citric acid and ethyl alcohol conduct an esterification reaction so as to obtain a reaction mixture; an impurity removing reaction is carried out on the reaction mixture at the temperature ranging from 60 DEG C to 100 DEG C under the alkali effect; and then the triethyl citrate is obtained. By means of the method, the triethyl citrate which has the low genotoxicity impurity content and meets the medical quality requirement can be efficiently obtained.
METHOD FOR THE PRODUCTION OF METHYLSUCCINIC ACID AND THE ANHYDRIDE THEREOF FROM CITRIC ACID
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Page/Page column 16, (2018/04/21)
A process for the preparation of methylsuccinic acid in any form, including its salts, its mono- and diester derivatives and the anhydride thereof, which comprises reacting citric acid or a derivative thereof in decarboxylation conditions, said process comprising (i) reacting citric acid or mono- and diester derivatives thereof in a non- aqueous solvent, specifically excluding alcohols, on a metallic catalyst at a temperature between 50 to 400°C and under a partial hydrogen pressure from 0.1 to 50 bar or (ii) reacting citric acid or any salt thereof or mono-, di- and triester derivatives thereof on a metallic catalyst in solvents comprising at least 5% water, at a temperature of from 50 to 400°C under a hydrogen partial pressure from 0.1 to 400 bar
Synthetic method for auxiliary for 3D printing flexible material
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Paragraph 0022; 0023, (2017/02/17)
The invention designs a synthetic method for a tribenzyl citrate auxiliary for a 3D printing flexible material. The preparing method includes the steps that monohydric alcohol, benzyl alcohol and citric acid are used as main raw materials, a catalyst and a water carrying agent are used, and the product tribenzyl citrate is prepared through two steps of reaction including acid alcohol esterification and ester exchange, neutralizing, washing, reduced pressure distillation and purification. the product is the auxiliary for the 3D printing flexible material.
Method for preparing triethyl citrate through mesoporous silica-supported N,N-dicyclohexyl carbodiimide
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Paragraph 0022, (2016/10/17)
The invention discloses a method for preparing triethyl citrate through mesoporous silica-supported N,N-dicyclohexyl carbodiimide. The method comprises the specific step that citric acid and absolute ethyl alcohol are subjected to an esterification reaction to synthesize triethyl citrate through the mesoporous silica-supported N,N-dicyclohexyl carbodiimide. Mesoporous silica is adopted for supporting an esterification reaction condensing agent, no obvious corrosivity exists, the esterification reaction efficiency and yield are improved, the purity is good, the reaction period is greatly shortened, the aftertreatment technology is simplified, the esterification reaction condition is mild, the technology is simple, and the method is suitable for industrial production.
Preparation method of high-purity triethyl citrate
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Paragraph 0010, (2017/06/19)
The invention discloses a preparation method of high-purity triethyl citrate .The preparation method comprises the steps that citric acid monohydrate or anhydrous citric acid and ethyl alcohol are adopted as raw materials, catalytic esterification, ethyl alcohol azeotropy water entraining, activated carbon decoloration, distillation ethyl alcohol removal, filtering, filtrate washing/water distribution and oil layer drying are performed to obtain the high-purity triethyl citrate .Crude triethyl citrate with the small content of impurities can be obtained through a proper catalyst and the addition amount of the catalyst, the reaction balance can be broken through the specific technology, the high yield can be obtained, and the reaction time can be shortened .Meanwhile, an inventor further finds that the reaction charge rate and the reaction temperature can affect the reaction rate and the product quality .
Preparation method of citrate
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Paragraph 0010, (2016/10/07)
The invention discloses a method for preparing citrate by taking citric acid and fatty alcohol as main raw materials and using carbodiimide as a catalyst. The method is characterized in that in the synthetic process of citrate, carbodiimide is used as a catalyst, which not only can achieve a catalytic action but also can be used as a water retaining agent to absorb water generated in the process of esterification reaction so as to ensure that the reaction is carried out in a direction of generating ester. After reaction, a citrate compound is synthesized by virtue of purification processes of filtration, neutralization, water washing, decolorization, reduced pressure distillation and the like, and the preparation method belongs to the technical field of organic chemical synthesis. The preparation method disclosed by the invention has the advantages that the yield is high and reaches 95-98%; the catalyst is low in price and less in dosage which accounts for 0.2-1.25% of the total weight of the reaction raw material namely citric acid; the reaction condition is mild, the reaction can be carried out at normal temperature, the reaction speed is high, and the reaction time is short; the catalyst can be used repeatedly; and the catalyst is also a water retaining agent, reduces the addition of organic solvents of methyl benzene and the like, and is safe and environmentally friendly.
A continuous triethyl citrate production system and method for production thereof (by machine translation)
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Paragraph 0022;0023, (2016/10/08)
A continuous triethyl citrate production system and method for producing the same, comprises the following steps: anhydrous citric acid, ethanol, strong acid catalyst, according to a certain ratio (anhydrous citric acid and ethanol can be 95% according to the quality than the 1 [...] 1.8-2.3 into the dissolving the kettle, stirring is dissolved, the temperature is controlled at 60 °C -70 ° C; the mixture after dissolving by the metering pump into the primary esterification reactors esterification, temperature control in the 128 °C -130 ° C; after the initial esterification by the metering pumped into the moderate esterification reactors, esterification temperature control in the 130 °C -135 ° C; moderate by esterification, by the metering pumped into the depth esterification reactors esterification, the temperature is controlled at 135 °C -145 °C, a three-step reaction for the esterification, including primary esterification, moderate esterification, depth esterification. Final use anhydrous ethanol to increase the esterification of citric acid. Experiment proves that, using this method is suitable for large-scale continuous production, reduce the production cost, ≥ 99% esterification rate citrate, triethyl citrate can be achieved the final yield of ≥ 95%. (by machine translation)
Method for preparing triethyl citrate through using nanometer intercalated hydrotalcite catalyst
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Paragraph 0021, (2016/12/01)
The invention discloses a method for preparing triethyl citrate through using a nanometer intercalated hydrotalcite catalyst. The method comprises the following steps: 1, charging: adding the nanometer intercalated hydrotalcite catalyst, citric acid and excess ethanol to a container, and stirring the added materials until uniformity; 2, carrying out an esterification reaction: carrying out oil bath heating, continuously adding ethanol in the heating process until ethanol is excess, and carrying out condensation refluxing and evaporated ethanol collection, wherein the esterification reaction is carried out for 16-20h; and 3, purifying: filtering out the nanometer intercalated hydrotalcite catalyst after the esterification reaction ends, dealcoholizing, neutralizing the dealcoholized material, washing the neutralized material with water, decolorizing the washed material, and purifying the decolorized material to obtain the finished triethyl citrate. The method for preparing triethyl citrate by using the nanometer intercalated hydrotalcite catalyst allows the citric acid conversion rate to be not lower than 99%, the product prepared in the invention is highly pure, the whole catalysis reaction is easy to operate, the temperature is easy to control, and the catalyst can be repeatedly used after being filtered.
Sulfonated graphene as highly efficient and reusable acid carbocatalyst for the synthesis of ester plasticizers
Garg, Bhaskar,Bisht, Tanuja,Ling, Yong-Chien
, p. 57297 - 57307 (2015/02/02)
Plasticizers are well known for their effectiveness in producing flexible plastics. The automotive, plastic and pharmaceutical industries, essential to a healthy economy, rely heavily on plasticizers to produce everything from construction materials to medical devices, cosmetics, children toys, food wraps, adhesives, paints, and 'wonder drugs'. Although H2SO4 is commonly used as commodity catalyst for plasticizer synthesis it is energy-inefficient, non-recyclable, and requires tedious separation from the homogeneous reaction mixture resulting in abundant non-recyclable acid waste. In this study, for the first time, we report an efficient synthesis of ester plasticizers (>90% yields) using sulfonated graphene (GSO3H) as an energy-efficient, water tolerant, reusable and highly active solid acid carbocatalyst. The hydrothermal sulfonation of reduced graphene oxide with fuming H2SO4 at 120°C for 3 days afforded GSO3H with remarkable acid activity as demonstrated by 31P magic-angle spinning (MAS) NMR spectroscopy. The superior catalytic performance of GSO3H over traditional homogeneous acids, Amberlyst-15, and acidic ionic liquids has been attributed to the presence of highly acidic and stable sulfonic acid groups within the two dimensional graphene domain, which synergistically work for high mass transfer in the reaction. Furthermore, the preliminary experimental results indicate that GSO3H is quite effective as a catalyst in the esterification of oleic and salicylic acid and thus may pave the way for its broad industrial applications in the near future.
