Spherical attapulgite mesoporous composite carrier, supported catalyst, preparation methods of spherical attapulgite mesoporous composite carrier and supported catalyst, use of supported catalyst and preparation method of ethyl acetate
A technology of composite carrier and attapulgite, which is applied in the preparation of organic compounds, organic compound/hydride/coordination complex catalysts, catalyst carriers, etc., can solve the problem of low conversion rate of reaction raw materials, and reduce production costs. Does not corrode equipment and has less side effects
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[0035] The present invention also provides a method for preparing the spherical attapulgite mesoporous composite carrier, which includes the following steps:
[0036] (1) In the presence of a template agent and butanol, contact ethyl orthosilicate with an acid agent, and crystallize and filter the contacted product to obtain a mesoporous molecular sieve material with a three-dimensional cubic pore structure. Cake
[0037] (2) Contact water glass with inorganic acid, and filter the product obtained after contact to obtain silica gel filter cake;
[0038] (3) Mixing the filter cake of the mesoporous molecular sieve material with three-dimensional cubic pore structure, the silica gel filter cake and attapulgite uniformly and ball milling, and the solid powder obtained after ball milling is slurried with water and then spray dried, The templating agent in the product obtained after spray drying is removed.
[0039] In the preparation process of the spherical attapulgite mesoporous compos...
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[0075] Example 1
[0076] This example is used to illustrate the spherical attapulgite mesoporous composite carrier and the supported benzenesulfonic acid catalyst provided by the present invention and the preparation method thereof.
[0077] (1) Preparation of spherical attapulgite mesoporous composite carrier
[0078] Dissolve 6g (0.001mol) triblock copolymer polyethylene glycol-polyglycerol-polyethylene glycol (P123) in 10mL, pH 4 hydrochloric acid aqueous solution and 220mL deionized aqueous solution, stir for 4h until P123 dissolves , Form a transparent solution, and then add 6g (0.08mol) n-butanol to the transparent solution and stir for 1h, then place the solution in a water bath at 40°C, and slowly drop 12.9g (0.062mol) ethyl orthosilicate Add to this solution, keep the temperature at 40℃, and stir for 24h under the condition of pH 4.5, then hydrothermally heat at 100℃ for 24h, then filter and wash with deionized water 4 times, and then suction filter to obtain Mesoporous m...
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[0102] Example 2
[0103] This example is used to illustrate the spherical attapulgite mesoporous composite carrier and the supported benzenesulfonic acid catalyst provided by the present invention and the preparation method thereof.
[0104] (1) Preparation of spherical attapulgite mesoporous composite carrier
[0105] Dissolve 6 g (0.001 mol) of the triblock copolymer P123 in 10 mL of a hydrochloric acid aqueous solution with a pH of 5 and 220 mL of a deionized aqueous solution, stir for 4 hours until P123 is dissolved to form a transparent solution, and then add 4.5 g to the solution (0.06mol) n-butanol was stirred for 1h, then the solution was placed in a 60℃ water bath, 10.4g (0.05mol) ethyl orthosilicate was slowly added dropwise to the solution, and the temperature was maintained at 60℃, pH Stir for 48h under the condition of 5.5, and then hydrothermally heat at 80℃ for 20h, filter and wash with deionized water 4 times, and then suction filter to obtain a mesoporous molecular...
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