- Citrate plasticizer
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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.
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Paragraph 0066-0068
(2021/05/15)
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- The preparation method of the triethyl citrate
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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.
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Paragraph 0037-0050
(2019/07/04)
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- METHOD FOR THE PRODUCTION OF METHYLSUCCINIC ACID AND THE ANHYDRIDE THEREOF FROM CITRIC ACID
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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
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Page/Page column 16
(2018/04/21)
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- Synthetic method for auxiliary for 3D printing flexible material
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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.
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Paragraph 0022; 0023
(2017/02/17)
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- Method for preparing triethyl citrate through mesoporous silica-supported N,N-dicyclohexyl carbodiimide
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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.
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Paragraph 0022
(2016/10/17)
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- Preparation method of high-purity triethyl citrate
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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 .
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Paragraph 0010
(2017/06/19)
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- Preparation method of citrate
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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.
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Paragraph 0010
(2016/10/07)
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- A continuous triethyl citrate production system and method for production thereof (by machine translation)
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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)
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Paragraph 0022;0023
(2016/10/08)
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- Method for preparing triethyl citrate through using nanometer intercalated hydrotalcite catalyst
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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.
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Paragraph 0021
(2016/12/01)
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- Sulfonated graphene as highly efficient and reusable acid carbocatalyst for the synthesis of ester plasticizers
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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.
- Garg, Bhaskar,Bisht, Tanuja,Ling, Yong-Chien
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p. 57297 - 57307
(2015/02/02)
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- ALCOHOL-MEDIATED ESTERIFICATION OF CARBOXYLIC ACIDS WITH CARBONATES
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A process for making esters from organic acids by means of reacting a carboxylic acid with dialkylcarbonate in an alcohol-containing solvent without any extrinsic acid or base catalyst is described. A benefit of the preparation process is that it can make the separation and extraction of ester products simpler and more facile vis-a-vis conventional isolation techniques.
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Page/Page column 10
(2014/05/24)
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- Synthesis and antiischemic activity of dicarboxylic nitroxyalkylamides and nitroxyalkylimides
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A number of dicarboxylic N-(2-nitroxyalkyl)amides and N-(2-nitroxyalkyl)imides were synthesized and their antiischemic activity was studied. The ratio of the areas of necrotic and ischemic zones was used as a criterion for evaluation of antiischemic activity. The maximum values were close to antiischemic activity of Nicorandil, with acute toxicity of compounds synthesized being considerably lower.
- Fedorov,Bogdanov,Fadeev,Lagodzinskaya
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p. 1119 - 1125
(2015/04/14)
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- Lubricant compositions containing hydroxy carboxylic acid and hydroxy polycarboxylic acid esters
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Disclosed herein is a composition comprising: (A) a lubricant or a hydrocarbon fuel;(B) at least one hydroxy carboxylic acid ester or hydroxy polycarboxylic acid ester having the generic formula defined herein; and(C) at least one phosphorus-containing additive.
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- SKIN EXTERNAL PREPARATIONS AND COSMETICS
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An object of the present invention is to provide skin external preparations and cosmetics which contain a branched acyl carnitine and have excellent formulation stability. A skin external preparation of the present invention includes a carnitine derivative represented by the following Formula (1) and/or a carnitine derivative salt represented by the following Formula (2), and an amphoteric surfactant. In Formula (1), R1 and R2 are each independently a C1-18 optionally branched, saturated or unsaturated aliphatic hydrocarbon group. In Formula (2), R1 and R2 are the same as in Formula (1), X? is a specific anion and Y+ is a specific cation.
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- HYDRATE INHIBITORS
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The present invention relates to compounds for controlling gas hydrate formation of the formula (I) and (II) and plugging of gas hydrate forming fluids wherein R1 is selected from the group consisting of H, acetyl and carbonyl derivative; R2 is H, -OR3 or -NR4R5, where: R3 is H, C1-6-alkyl or carbonyl derivative, R4, R5 are selected from the group consisting of H, C1-18-alkyl, alkanol, alkoxy, cyclic/aromatic or alkylene. The invention further comprises compositions and method of producing the compounds of formula (I) and (II), method for controlling gas hydrate formation and plugging of gas hydrate forming fluids, and use of compounds of formula (I) and (II).
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Page/Page column 36-38
(2010/09/18)
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- Process for reactive esterification distillation
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A process for producing organic acid di- or tri-esters, particularly citric acid tri-esters, with the available acid groups esterified using countercurrent reactive distillation using acid catalysts in a structured packing is described. In the reactive distillation an organic acid di- or triester is formed by chemical reaction and purified to its final state within the single column. Organic acid di- or tri-esters are produced at relatively low cost, with less waste production in by-products of the reaction, and in a less complicated manner than prior processes. Organic acid di- and tri-esters have uses as solvents, as plasticizers and in conversion products.
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Page/Page column 5-6; 7-18; 26-77
(2008/06/13)
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- Liquid antacid compositions
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Liquid antacid compositions containing a tri- or di-ester buffer have a reduced final product pH providing for a more efficacious preservative system and better tasting product without compromising to acid neutralization capacity of the antacid.
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- Regio- and enantioselectivity of the enzyme-catalyzed hydrolysis of citric acid derivatives
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The hydrolysis of triethyl citrate in the presence of three serine proteases (chymotrypsin, subtilisin BPN', subtilisin carlsberg) is highly regioselective and gives the symmetric diester. Several lipases and proteases have the complementary regioselectivity and give the chiral diester. Pig liver esterase, Aspergillus niger lipase and Candida antarctica lipase give the chiral (R)-diester with good regio- and enantioselectivity. The stereoselective hydrolysis of the meso citric derivatives 7a,b in the presence of Candida antarctica lipase gives the corresponding (R)-monoester.
- Chenevert, Robert,Tchedam Ngatcha, Beatrice,Yannick, Stephane Rose,Goupil, Daniel
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p. 4325 - 4329
(2007/10/03)
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