Supercharge Your Innovation With Domain-Expert AI Agents!

Preparation method of trimellitate

A technology for trimellitic acid ester and compound is applied in the field of preparation of trimellitic acid ester, and achieves the effects of abundant raw material sources, simplified reaction steps and environmental friendliness

Pending Publication Date: 2022-06-14
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
View PDF4 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, most of the current work focuses on the preparation of terephthalic acid and its derivatives, and there are few reports on the synthesis of trimellitic acid and trimellitic acid esters.

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
  • Preparation method of trimellitate
  • Preparation method of trimellitate
  • Preparation method of trimellitate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0070] Embodiment 1 Catalyst concentrated sulfuric acid affects esterification, Diels-Alder reaction

[0071] In this example, the effects of concentrated sulfuric acid as a catalyst on the esterification of muconic acid and acrylic acid and the Diels-Alder reaction were studied. It is specifically shown in the conversion rate of muconic acid and the yield of cyclized products.

[0072] In the reactor, add 1.7g muconic acid and 2.16g acrylic acid (muconic acid and acrylic acid molar ratio 1:3), add the concentrated sulfuric acid catalyst of 0.05g mass fraction 98% (protonic acid catalyst [H] proton amount / Muconic acid molar ratio, 10%), methanol as the reaction medium (muconic acid mass / methanol mass, 1 / 7). After stirring and mixing evenly at room temperature, the temperature was raised to 200° C. by electric heating, the reaction pressure was self-pressure, and the reaction was performed for 10 hours under magnetic stirring at 800 rpm. See Example 1 of Table 1 for the resu...

Embodiment 2

[0078] Embodiment 2 Catalyst silicotungstic acid affects esterification, Diels-Alder reaction

[0079] This example studies the effect of silicotungstic acid as a catalyst on the esterification of muconic acid and acrylic acid and the Diels-Alder reaction. It is specifically shown in the conversion rate of muconic acid and the yield of cyclized products.

[0080] The amount of reactant and the reaction conditions are the same as in Example 1, and the catalyst is changed into 0.17g silicotungstic acid (proton acid catalyst [H] proton amount / muconic acid molar ratio, 10%), and silicotungstic acid is used as a catalyst for the Diels-Alder reaction The results of the impact are shown in Example 2 of Table 1.

Embodiment 3

[0081] Embodiment 3 Catalyst SnCl 4 Effect on esterification and Diels-Alder reaction

[0082] This example studies the SnCl 4 Effect as a catalyst on the esterification of muconic acid with acrylic acid, the Diels-Alder reaction. It is specifically shown in the conversion rate of muconic acid and the yield of cyclized products.

[0083] Reactant charging amount and reaction condition are the same as embodiment 1, and catalyst changes into 0.72gSnCl 4 (metal salt catalyst / muconic acid mass ratio, 10wt%), SnCl 4 See Example 3 of Table 1 as a result of the effect of the catalyst on the Diels-Alder reaction.

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 discloses a preparation method of trimellitate, which at least comprises the following steps: step 1, reacting a mixture containing a compound I, a compound II and fatty alcohol in the presence of a catalyst to obtain a six-membered carbocyclic product; the compound I has conjugated C = C and-COOH groups; the compound II has C = C and-COOH groups; and step 2, carrying out dehydrogenation reaction on the six-membered carbocyclic ring product to obtain trimellitate. According to the method, the fatty alcohol is used as a reaction medium to perform continuous esterification and Diels-Alder reaction, so that the reaction steps are simplified; and the trimellitate can be obtained with high selectivity by controlling the dehydrogenation reaction conditions of the six-membered carbocyclic ring product. The raw materials adopted by the invention can be derived from biomass materials, so that the dependence of trimellitate preparation on petroleum resources is reduced.

Description

technical field [0001] The application relates to a preparation method of trimellitate, which belongs to the field of chemical synthesis. Background technique [0002] Trimellitic acid and its esters are important raw materials for synthetic polymers, and are widely used in the production of plasticizers, enameled wires, and coatings. At present, the industrial production of trimellitic acid mainly relies on the route of oxidation of trimellitic benzene under the action of Co-Mn-Br catalyst, and the raw material trimellitic is obtained by separating and extracting the C9 aromatic hydrocarbons in the petroleum fraction. The toluene content is about 40%. Trimellitic acid needs to be esterified to obtain trimethyl trimellitate. In addition, trimethyl trimellitate can also be synthesized by cycloaddition reaction of methyl propiolate as a raw material, but this method is catalyzed by Pd, Au, etc., and using toluene as a solvent, the yield of the target product is only 40%. %....

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
Patent Type & Authority Applications(China)
IPC IPC(8): C07C67/317C07C69/76C07C67/347C07C69/75C07C67/08C07C69/54C07C69/602
CPCC07C67/317C07C67/347C07C67/08C07C2601/16C07C69/54C07C69/602C07C69/75C07C69/76
Inventor 路芳罗晓琳卢锐司晓勤姜慧芳
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
Features
  • R&D
  • Intellectual Property
  • Life Sciences
  • Materials
  • Tech Scout
Why Patsnap Eureka
  • Unparalleled Data Quality
  • Higher Quality Content
  • 60% Fewer Hallucinations
Social media
Patsnap Eureka Blog
Learn More