Method for Synthesizing Glyoxylic Acid by Ozonation of Maleic Anhydride Mixed Solvent
A maleic anhydride and mixed solvent technology, applied in the field of glyoxylic acid preparation, can solve the problems of low space-time yield of equipment, low yield of raw materials, easy corrosion of equipment, etc., and achieve good mass transfer effect, method and process Simple, short hydrolysis time effect
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Embodiment 1
[0069] a. First melt 19.6120g of maleic anhydride in a hydrolysis reactor, heat it in a water bath, then add 5mL of distilled water + 5mL of methanol + 10mL of ethyl acetate to carry out the hydrolysis reaction, the hydrolysis temperature is 65°C, and the hydrolysis time is 50min.
[0070] b. After the hydrolysis is completed, move the hydrolyzate into a self-made bubbling reactor, add 5mL methanol + 10mL ethyl acetate mixed solvent, and carry out ozonation. To be able to fully contact, control the reaction temperature at 5°C and the time for 3h.
[0071] c. At the end of the ozone oxidation stage, stop feeding ozone, and continue feeding air for 10 minutes to purge the residual ozone in the system.
[0072] d. Slowly add the reacted solution into the 8% sulfurous acid solution, and control the system temperature at 55-65°C.
[0073] e. After all the addition, slowly add about a certain amount of CaO, then add 5mL of water, and control the temperature below 10°C, after that, ...
Embodiment 2
[0078] a. First melt 19.6120g of maleic anhydride in a hydrolysis reactor, heat it in a water bath, then add 5mL of distilled water + 5mL of methanol + 10mL of n-hexane to carry out the hydrolysis reaction, the hydrolysis temperature is 60°C, and the hydrolysis time is 60min.
[0079] b. After the hydrolysis is completed, move the hydrolyzate into a self-made bubbling reactor, add 7.5mL methanol + 15mL n-hexane mixed solvent, and carry out ozonation. Ozone is blown in from the bottom of the maleic acid solution to make the ozone and solution To be able to fully contact, the reaction temperature is controlled at 0°C and the time is 2.5h.
[0080] c. At the end of the ozone oxidation stage, stop feeding the ozone, and continue feeding air for 10 minutes to purge the residual ozone in the system.
[0081] d. Slowly add the reacted solution into 8% sulfurous acid solution, and control the system temperature at 55-65°C.
[0082] e. After all the addition, slowly add about a certain ...
Embodiment 3
[0087] a. First melt 19.6120g of maleic anhydride in a hydrolysis reactor, heat in a water bath, then add 5mL of distilled water + 5mL of methanol + 10mL of ethyl acetate to carry out the hydrolysis reaction, the hydrolysis temperature is 65°C, and the hydrolysis time is 30min.
[0088] b. After the hydrolysis is completed, move the hydrolyzate into a self-made bubbling reactor, add 5mL methanol + 10mL ethyl acetate mixed solvent, and carry out ozonation. To be able to fully contact, control the reaction temperature to 5°C and the time to 2.5h.
[0089] c. At the end of the ozone oxidation stage, stop feeding ozone, and continue feeding air for 10 minutes to purge the residual ozone in the system.
[0090] d. Slowly add the reacted solution into the 10% sulfurous acid solution, and control the system temperature at 55-65°C.
[0091] e. After all the addition, slowly add about a certain amount of CaO, then add 5mL of water, and control the temperature below 20°C, after that, l...
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