Solid acid as well as preparation method and application thereof
A technology of solid acid and carboxylic acid, which is applied in the field of solid acid and its preparation, can solve the problems of easy loss of active substances, decrease of catalytic activity, and low product yield, and achieve the goal of not easy to lose, increase product yield, and stable and reliable quality Effect
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Embodiment 1
[0051] The present embodiment provides a kind of preparation method of solid acid, comprises the steps:
[0052] (1) Add methyl orthosilicate (1 mole, 152 g) and acetic acid (5 moles, 300 g) into a three-necked flask, raise the temperature to 75° C., and stir for 20 min to obtain a sol-gel.
[0053] (2) Add sulfuric acid (0.1 mol, 9.8g) with a mass percentage of 98% into the sol-gel, age at 75°C for 4h, transfer to a vacuum oven and dry at 120°C for 5h to obtain 102g of solid Acid, denoted as A-1.
[0054] This embodiment also provides a preparation method of simethicone oil, which can only carry out a single experiment, or continue to carry out mechanical experiments after a single experiment, and the solid acid can be recycled, including the following steps:
[0055] Single experiment: Put 1483g of D4 and 162g of MM into the flask, put 16.5g of solid acid A-1 into the flask, heat to 35°C, keep stirring at 35°C for 2h, and filter with suction to obtain simethicone. And reco...
Embodiment 2
[0058] The present embodiment provides a kind of preparation method of solid acid, comprises the steps:
[0059] (1) Ethyl orthosilicate (1 mole, 208 g) and acetic acid (3 moles, 180 g) were put into a three-necked flask, the temperature was raised to 60° C., and stirred for 20 min; a sol-gel was obtained.
[0060] (2) Methanesulfonic acid (0.1 mol, 9.6 g) was added dropwise into the sol-gel, and aged at 60° C. for 4 h to obtain a gel. The gel was transferred to a vacuum drying oven and dried at 120°C for 5 hours to obtain 116g of solid acid, which was designated as A-2.
[0061] The present embodiment also provides a kind of preparation method of simethicone oil, comprises the steps:
[0062] Single experiment: Put 1483g of D4 and 162g of MM into the flask, put 16.5g of solid acid A-2 into the flask, heat to 35°C, keep stirring at 35°C for 3h, filter with suction to obtain simethicone and To recover the solid acid, the filter cake was washed twice with water, and the solid ...
Embodiment 3
[0065] The present embodiment provides a kind of preparation method of simethicone oil, comprises the steps:
[0066] Get 30g of solid acid A-2 and pack into existing conventional solid bed packed column, the outer diameter of packed column is 1 inch, and length is 15cm, and volume is 50mL, two feed ports are arranged at the two ends of packed column, sidewall A discharge port is provided at the top.
[0067] Keep the column temperature at 35°C, use two plunger pumps to pump D4 and MM into the packed column from the inlet of the packed column respectively, the flow rate of D4 is 0.83mL / min, and the flow rate of MM is 0.17mL / min. At the same time, the collected reaction solution is pumped into the packed column at a speed of 1ml / min by the third plunger pump, and the total reaction time is 2h from the start of D4 and MM feeding, and it is collected from the outlet after the reaction. The reaction liquid is obtained as simethicone oil.
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Abstract
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