Unlock instant, AI-driven research and patent intelligence for your innovation.

Method for preparing anchoic acid by microwave reaction

A microwave reaction, azelaic acid technology, applied in the preparation of carboxylates, chemical instruments and methods, preparation of organic compounds, etc., can solve the problems of low yield, low product purity, complicated post-processing, etc., and achieve the reaction process. Simple, non-polluting, environment-friendly effect

Inactive Publication Date: 2008-09-03
XINJIANG TECHN INST OF PHYSICS & CHEM CHINESE ACAD OF SCI
View PDF8 Cites 0 Cited by
  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0021] The selectivity of the nitric acid oxidation reaction is not high, and the equipment is severely corroded
The oxidized oleic acid method using potassium permanganate as an oxidant has a low yield and consumes a large amount of sulfuric acid and potassium permanganate, which not only has high cost but also causes serious pollution
Although the technology of potassium permanganate method can be improved by emulsification method, the consumption of potassium permanganate is still very large, and the post-treatment is very complicated, which is not economically desirable.
Using chromic acid as an oxidant is expensive, and it is easy to degrade the oxidation product to produce a low-carbon chain dibasic acid, and the resulting product is not high in purity
It can be seen that in many existing technologies, some methods pollute the environment, some methods have more complicated steps, some methods need to support noble metal catalysts, and need to pass oxygen for a long time, which is time-consuming and costly.
Some methods require high pressure, harsh implementation conditions, high cost, and difficult to scale production

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

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] 386.95g of oleic acid (73% by mass, 1.00mol in moles) and 1.92g of tungstic acid (0.0077mol in moles) were stirred and mixed evenly, and the temperature was raised. When the temperature rose to 55°C, 5% concentration was added dropwise. Hydrogen oxide 1156g (mole number 1.71mol) solution was added dropwise in 10 minutes, and the temperature was raised to 60°C. After reacting for 30 minutes, 5776g (mole number 3.80mol) of 5% peracetic acid was added and put into a microwave device. First preheat with low heat for 5 minutes, and then react for 1 hour under medium heat. After the reaction is over, extract 56.50 g of the product azelaic acid from the reaction solution through extraction, filtration, and drying. The yield (in terms of oleic acid) 30.0%, melting point 106-108°C. At the same time, 41.0 g of nonanoic acid was obtained as a by-product, with a yield (based on oleic acid) of 26.0%.

Embodiment 2

[0041] With oleic acid 386.95g (mass percentage composition is 73%, mole number 1.00mol) 2.90g tungstic acid 2.50g (mole number 0.010mol), tert-butanol 467g (mole number 6.30mol), stir and mix uniformly, heat up, when When the temperature rose to 60°C, a solution of 782.0 g (2.30 mol in moles) of 10% hydrogen peroxide was added dropwise, and the dropwise addition was completed in 15 minutes, and the temperature was raised to 65°C. After reacting for 40 minutes, tert-butanol was recovered by rotary evaporation. Add 15732g peroxybenzoic acid (5.70mol moles) with a concentration of 5% to the oil phase where tert-butanol is removed, put it in a microwave device, preheat it with a small fire for 8 minutes, and then react for 3 hours under a medium fire After the reaction, 75.3 g of the product azelaic acid was extracted from the reaction solution through extraction, filtration and drying, with a yield (calculated as oleic acid) of 40% and a melting point of 106-108° C. At the same ...

Embodiment 3

[0043] With oleic acid 386.95g (mass percentage is 73%, molar number 1.00mol) tungstic acid 3.90g (molar number 0.012mol), isoamyl alcohol 837g (molar number 9.5mol), stir and mix uniformly, heat up, when temperature rises When the temperature reached 65°C, a solution of 317.3g (2.8mol moles) of 30% hydrogen peroxide was added dropwise, and the dropwise addition was completed in 20 minutes, and the temperature was raised to 70°C. After reacting for 60 minutes, isoamyl alcohol was recovered by rotary evaporation. It is 5% peroxyformic acid 9424g (mole number 7.60mol) that adding concentration is 5% in the oily phase that evaporates isoamyl alcohol, puts into microwave device, preheats 10 minutes with low firepower earlier, reacts 1 hour under medium fire then, After the reaction, 103.50 g of the product azelaic acid was extracted from the reaction liquid through extraction, filtration and drying, with a yield (calculated as oleic acid) of 55.0% and a melting point of 106-108°C. ...

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

PropertyMeasurementUnit
melting pointaaaaaaaaaa
boiling pointaaaaaaaaaa
refractive indexaaaaaaaaaa
Login to View More

Abstract

The microwave reaction process of preparing anchoic acid includes mixing oleic acid, ttungstic acid and solvent, heating the mixture, dropping hydrogen peroxide solution, heating and rotating to evaporate and recover solvent, adding peracid into the oil phase, setting the oil phase with peracid into microwave equipment, preheating at low temperature and reaction at medium temperature, and extracting anchoic acid and side product nonoic acid from the reacted liquid. The said process has high anchoic acid yield up to 85 %, no environmental pollution, no need of noble metal catalyst, and other advantages and is suitable for large scale production.

Description

technical field [0001] The invention relates to a method for preparing azelaic acid by microwave reaction. Background technique [0002] Azelaic acid, also known as azelaic acid, is a white to yellowish monoclinic prism, needle-like crystal or powder. Molecular formula C 9 h 16 o 4 , molecular weight 188.22, specific gravity 1.0291 (4°C), 1.225 (25°C), melting point 106.5°C, boiling point 286.5°C (13.33kPa), refractive index 1.4303 (111°C), medium-length carbon chain plus two carboxyl groups, giving Azelaic acid has a wide range of uses and is an important intermediate in organic synthesis. [0003] Azelaic acid can be used to synthesize dioctyl azelate (DOZ) plasticizer, synthetic perfume, lubricating oil and polyamide and other products. Dioctyl azelate, didecyl azelate, and tridecyl azelate are good lubricants. Azelaic acid is also used in the production of nylon 69 and nylon 9. Azelaic acid is aminated and hydrogenated to produce aminononanoic acid, which can be d...

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 Patents(China)
IPC IPC(8): C07C55/18C07C51/285
Inventor 吾满江·艾力高军军张亚刚董昕胡书明樊莉
Owner XINJIANG TECHN INST OF PHYSICS & CHEM CHINESE ACAD OF SCI