Environmental pretection type process for synthesizing pentandioic acid by catalyzing oxidizing glutaraldehyde
A technology for oxidizing glutaraldehyde and glutaric acid, applied in chemical instruments and methods, preparation of organic compounds, organic chemistry, etc., can solve environmental pollution and other problems
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Embodiment 1
[0012] In a 250 ml three-necked round bottom flask equipped with stirring, reflux condensation and a thermometer, add 2.15 g (7.5 mmol) tungstic acid dihydrate H 2 WO 4 2H 2 O and 83 milliliters (0.75 moles) of hydrogen peroxide with a concentration of 27.5%, stirred at room temperature for 10 minutes, pH≈1. Add dropwise the 50% aqueous solution containing glutaraldehyde 30g (0.3 moles) and then the stirring speed rises to about 1000 R.P.M. By heating in an oil bath, control the bath temperature from 60°C to 100°C in about 3 to 4 hours to maintain the reflux of the reactant. After 8 hours of reaction, samples were taken for analysis.
[0013] Analysis results: glutaric acid, 98.6%; succinic acid, 1.0%; other products 0.4%. The reaction mixture was cooled, left overnight at 0°C, and filtered. Wash once with a small amount of cold water to obtain 31.7 g of glutaric acid (yield 80%). m.p.=97~99°C, purity (according to GC analysis)≥99.0%. The remaining filtrate was further ...
Embodiment 2～4
[0015] The dosages of tungstic acid dihydrate, tungstic acid, tungstic acid trihydrate and tungstic acid tetrahydrate are respectively: 4.03g (15 mmol), 1.27g (4.5 mmol), and 0.19g (0.6 mmol). 0.8 moles of 27.5%, 0.6 moles of 30%, and 0.9 moles of 50% aqueous hydrogen peroxide were used as oxidizing agents. Other charging amount, operating process and time are all with embodiment 1.
[0016] After the reaction is completed, the analysis results are shown in Table 1.
Embodiment 5～8
[0018] The amount of 12-tungstophosphoric acid was 0.009g (0.003 mmol); 1.79g (0.6 mmol); the amount of 12-tungstosilicate was 0.009g (0.003 mmol); 1.79g (0.6 mmol). Both use 0.6-0.75 moles of 50% aqueous hydrogen peroxide as the oxidizing agent. Reaction time is 8~24 hours, other charging amount, operation process are all the same as embodiment example 1. After the reaction is completed, the analysis results are shown in Table 1.
[0019]
Reality
apply
example
catalyst
Catalyst
quantity **
(mol%)
reaction
time
(h)
Product composition (%)
glutaric acid
glutaric acid
1
h 2 WO 4 2H 2 o
2.5
10
0
0.4
1.0
98.6
2
h 2 WO 4
5.0
8
0.2
0
0.9
98.9
3
h 2 WO 4 ·3H 2 o
1.5
18
0
0.6
3.1
96.3...
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