Method for preparing tert-butyl glycerol ether by glycerol etherification
A technology of tert-butyl glycerol and glycerol ether, which is used in the preparation of ether, the preparation of ether by addition of unsaturated compounds, chemical instruments and methods, etc. The effect of improving selectivity, improving glycerol conversion and improving reactivity
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preparation example Construction
[0024] According to the present invention, the preparation method of the glycerin etherification catalyst of described molding comprises:
[0025] Method 1: Mix the original powder of EWT structural molecular sieve with binder raw material, optionally contained acid, preferably nitric acid, and optionally contained water to obtain a mixture, knead the mixture uniformly and shape it to obtain a molded body, and the molded Body drying, roasting;
[0026] Convert the molecular sieve obtained after calcination into a hydrogen-type EWT structure molecular sieve, or alternatively, carry out silicon modification on the calcination molecular sieve to obtain a silicon-modified EWT structure molecular sieve, and convert the molecular sieve into a hydrogen-type molecular sieve before or after the silicon modification EWT structure molecular sieve;
[0027] Method 2: Convert the original powder of EWT structural molecular sieve into hydrogen-type EWT structural molecular sieve, or altern...
preparation example 1
[0056] Add 0.268g of sodium metaaluminate into a 45mL polytetrafluoroethylene container, and add 15.5g of an aqueous solution of template agent R (1,5-bis(N-propylpyrrolidinium)pentane dihydroxide) (of R content is 30% by mass), stirred for 30 minutes until uniform, then added 6g of solid silica gel (SiO 2 content is 98.05% by mass) and 17.5g deionized water, stirred for 5 minutes and fully mixed, wherein the molar ratio of each component is: SiO 2 / Al 2 o 3 =60,H 2 O / SiO 2 =10, Template R / SiO 2 =0.16, OH - / SiO 2 = 0.32.
[0057] The above mixture was put into a 45mL polytetrafluoroethylene-lined steel autoclave, covered and sealed, and the autoclave was placed in a rotating convection oven with the rotation speed set at 20rpm, and reacted at 150°C for 5 days. Take out the autoclave and let it cool down to room temperature quickly, separate the mixture on a 5000rpm high-speed centrifuge, collect the solid, wash it thoroughly with deionized water, and dry it at 100°C f...
preparation example 2
[0059] Prepare the original powder of EWT structural molecular sieve according to the method of Preparation Example 1. The difference is that the amount of sodium metaaluminate is 0.107g, and the types and amounts of other materials are the same as in Preparation Example 1, wherein the molar ratio of each component is: SiO 2 / Al 2 o 3 =150,H 2 O / SiO 2 =10, Template R / SiO 2 =0.16, OH - / SiO 2 = 0.32. Finally, the raw powder of molecular sieve with EWT structure is obtained. The scanning electron microscope image of the product is shown in image 3 As shown, the XRD pattern is as Figure 4 As shown, the silicon-aluminum ratio of the raw powder sample obtained by X-ray fluorescence spectroscopic analysis is 112. The total specific surface of the molecular sieve with the EWT structure is S 总 =601m 2 / g, the total pore volume is V 总 =0.386cm 3 / g.
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