Method of large scale synthesizing glutaric acid by environment friendly catalyzing and oxidizing cyclopentene
A catalytic oxidation, environmentally friendly technology, applied in chemical instruments and methods, preparation of organic compounds, catalysts for physical/chemical processes, etc. The effect of reducing equipment use costs, high industrial application prospects, and improving production capacity
Patent Information
- Authority / Receiving Office
- CN · China
- Current Assignee / Owner
- Publication Date
- 2007-01-31
- Estimated Expiration
- Not applicable · inactive patent
Abstract
Description
technical field
[0001] The invention belongs to the technical field of chemical industry, and in particular relates to an environment-friendly method for large-scale industrial preparation of glutaric acid by catalytic oxidation of cyclopentene with aqueous hydrogen peroxide solution. Background technique
[0002] Glutaric acid is an extremely important chemical raw material, and has a wide range of applications in chemistry, construction, medicine, agriculture, etc. In the plastic industry, glutaric acid and its alkyl glutarate are used as intermediates of plasticizers such as polyvinyl chloride, polyester, polyamide, etc., and can also be used as a composition of polyester plasticizers for polyvinyl chloride ingredients. As a plasticizer, polyglutarate has a durable plasticizing effect and is used in the manufacture of polyvinyl chloride. In medicine, because of its broad-spectrum bactericidal ability, it is used to prepare various bactericidal and disinfecting lotions a...
Examples
Embodiment 1
[0016] In a 5000-liter enamel reaction kettle equipped with stirring, reflux condensation and a thermometer, add 52.7 kg of tungstic acid dihydrate H 2 WO 4 2H 2 O and 500 kilograms of cyclopentene, stirred at room temperature for 30 minutes, added 23.2 kilograms of oxalic acid (C 4 h 2 o 4 2H 2 (0), continue to stir for 30 minutes, then add dropwise 2200 kilograms of 50% hydrogen peroxide. Through steam heating and jacket cooling, control the temperature of the kettle to rise from 46°C to 70°C in about 6-16 hours, maintain the reflux of the reactant for 12-24 hours, and raise the temperature to 90-90°C after the cyclopentene is consumed. 110°C. After another 6-8 hours of reaction, samples were taken for analysis.
[0017] Analysis results: glutaric acid, 94.8%; 1,2-cyclopentanediol, 0.4%; glutaraldehyde, 2.1%; other 2.7%. The reaction mixture was concentrated by distillation, cooled, left overnight at 0°C, and filtered. Wash once with a small amount of cold water to ...
Embodiment 2～4
[0019] The dosages of tungstic acid monohydrate, tungstic acid trihydrate and tungstic acid tetrahydrate are respectively: 42.2 kg and 31.6 kg; corresponding oxalic acid addition amounts: 18.6 kg, 13.9 kg; 14.0 kg. Other charging amount, operating process and time are all with embodiment 1. After the reaction is completed, the analysis results are shown in Table 1.
Embodiment 5～8
[0021] The dosage of tungstic acid dihydrate is 4.2 kg; 8.4 kg; 84 kg; 105 kg.
[0022] The organic ligand co-catalysts are respectively:
[0023] Oxalic acid: 1.9 kg
[0024] Niacin: 41 kg
[0025] 8-hydroxyquinoline: 21.8 kg
[0026] Salicylic acid: 5.4 kg
[0027] The reaction time was 24 hours, and other charging amounts and operating procedures were all the same as the implementation example 1. After the reaction is completed, the analysis results are shown in Table 1.
[0028]
Reality
apply
example
organic ligand
Catalyst and use
Amount (with tungstic acid moles
Alby)
dosage **
(mol%)
reaction
time
(h)
Product composition (%)
1,2-
Pentadiol
other
***
Pentadiol
sour
1...