Check patentability & draft patents in minutes with Patsnap Eureka AI!

A kind of preparation method of aliphatic dicarboxylic acid

A dicarboxylic acid and aliphatic technology, applied in the fields of pharmaceutical intermediates, polymer monomer preparation and chemical industry, can solve the problems of many by-products, harsh reaction conditions, difficult large-scale production, etc. Short, pure effect

Active Publication Date: 2021-03-16
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
View PDF5 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, these oxidation preparation methods require relatively expensive transition metal-metal oxide catalytic systems, the reaction conditions are harsh, and there are many by-products, making it difficult to produce on a large scale.

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
  • A kind of preparation method of aliphatic dicarboxylic acid
  • A kind of preparation method of aliphatic dicarboxylic acid
  • A kind of preparation method of aliphatic dicarboxylic acid

Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0026] In some embodiments, the preparation method of the aliphatic dicarboxylic acid may include: at least mixing and reacting acetyl carboxylic acid and / or acetyl carboxylic acid ester with halogen elements, and post-processing after the reaction To obtain aliphatic dicarboxylic acids.

[0027] In some more preferred specific embodiments, the preparation method includes:

[0028] a) adjust the pH value of the reaction system containing at least acetyl carboxylic acid and / or acetyl carboxylic acid ester and halogen element to be greater than or equal to 7, then remove the solid phase and retain the liquid phase,

[0029] b) and, adjusting the pH value of the liquid phase to be less than or equal to 4, thereby obtaining the aliphatic dicarboxylic acid.

[0030] Preferably, the halogen elements are from at least one of simple halogens and compounds containing halogens.

[0031] Further preferably, the halogen elements are from at least one of simple halogens and inorganic com...

Embodiment 1

[0065] In a 250mL reactor, dissolve 1.76g of acetylformic acid in 20mL of water, add 35.5g of iodine and 200mL of water dropwise at 20°C, then add NaOH aqueous solution (concentration: 2mol / L) dropwise to adjust the pH to 7, and filter to remove the precipitate , the pH value of the reaction solution was adjusted to 1 with hydrochloric acid (concentration: 0.5 mol / L), and the precipitated solid was filtered and dried to obtain oxalic acid with a yield of 75%. The purity measured by liquid chromatography-mass spectrometry (LC-MS) is 91.3%, and the molecular weight is 90.

Embodiment 2

[0067] In a 250mL reactor, dissolve 0.02mol of levulinic acid in 100mL of water, slowly feed 0.2mol of chlorine gas at 40°C, and at the same time add KOH aqueous solution (concentration: 1mol / L) dropwise, and use KOH solution (concentration: 1mol / L) to adjust the pH value to 8, remove the precipitate by filtration, adjust the pH value of the reaction solution to 2 with sulfuric acid (concentration is 0.5mol / L), filter the precipitated solid and dry to obtain succinic acid, the yield is 81 %.

[0068] see figure 1 shown by 1 H-NMR (400MHz, D 2 O) The test found that two CHs on the fatty chain of succinic acid 2 The chemical shift value of the group is 2.491ppm, the solvent (D 2 O) The peak is at 4.680ppm; the purity measured by liquid phase mass spectrometry (LC-MS) is 95.8%, and the molecular weight is 118.

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 for aliphatic dicarboxylic acids. The preparation method mainly employs acetyl carboxylic acids and / or acetyl carboxylates as raw materials for preparing the aliphatic dicarboxylic acids in a high yield through a nonoxidation process. The preparation technology is simple, efficient, short in flow, less in by-product and suitable for large-scale industrialized production, and the obtained aliphatic dicarboxylic acids are high in purity, and are applicable to synthesize polyesters, polyamides, polyurethanes and other engineering plastic and are used as chemical engineering raw materials and medicine intermediates.

Description

technical field [0001] The invention specifically relates to a preparation method of an aliphatic dicarboxylic acid, which belongs to the technical field of preparation of polymer monomers such as polyester, polyamide and polyurethane, and chemical and pharmaceutical intermediates. Background technique [0002] At present, the preparation process of bio-based aliphatic dicarboxylic acids from bio-based acetyl carboxylic acid or acetyl carboxylate is mainly based on the oxidation of acyl groups, but in this preparation process, transition metals are required to realize the oxidation process. Catalyst system and oxidant system. For example, Dunlop et al. (US 2,676,186) used a vanadium salt catalyst system and an oxygen oxidation system to convert levulinic acid into succinic acid at a high temperature of 200°C. For example, Subramaniam et al. (PCT / US12 / 52641) converted levulinic acid to succinic acid using a catalyst system containing cobalt, manganese and bromine and an oxyg...

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): C07C51/093C07C55/06C07C55/10C07C55/14C07C67/313C07C69/40C07C55/16
CPCC07C51/093C07C67/313C07C55/06C07C55/10C07C55/14C07C69/40C07C55/16
Inventor 刘斐王静刚那海宁刘小青朱锦
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY 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

Browse by: Latest US Patents, China's latest patents, Technical Efficacy Thesaurus, Application Domain, Technology Topic, Popular Technical Reports.

© 2025 PatSnap. All rights reserved.Legal|Privacy policy|Modern Slavery Act Transparency Statement|Sitemap|About US| Contact US: help@patsnap.com