Solid-form acid catalyst and its prepn

A technology of acid catalysts and catalysts, applied in chemical instruments and methods, physical/chemical process catalysts, chemical/physical processes, etc., can solve problems such as difficult liquid acid immobilization, uneven distribution of acid centers, and few active centers. Achieve the effect of improving stability, uniform distribution and large number

Inactive Publication Date: 2004-03-17
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

There are two commonly used methods, one is to load these liquid acids on the carrier, or use acidic oxides such as molecular sieves, amorphous silica-alumina and other "true" solid acid catalysts, but these two types of catalysts have some disadvantages. One is because the liquid acid is difficult to immobilize, and it is very easy to lose; the latter type of catalyst is due to the uneven distribution of acid centers, fewer active centers, and requires a higher reaction temperature. Therefore, in some reactions that require strong acid or low temperature, For example, it is difficult to replace liquid acid in the alkylation reaction of isobutane and butene

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Mix 100 grams of ethyl orthosilicate and 50 grams of ethanol in a 250ml three-necked flask with a reflux condenser, quickly add 15 grams of concentrated sulfuric acid into the resulting mixed solution, stir and heat to 100°C, and reflux for about 1 hour A gel is then formed. Separate the formed gel, put it in a vacuum oven, and vacuumize it at 50°C for 48 hours (the degree of vacuum is mmHg, the same below), to obtain a silicon-based solid acid, which is stored in a desiccator. Measured acid strength H 0 -12, the acid content was 3mmol / g, and the reaction performance was evaluated in a fixed-bed reaction system. The reaction results in 8 hours are shown in Table 5. The solid acid that present embodiment obtains is all 50% by weight before and after the acid-base titration method of reaction.

[0039] Olefin Conversion

Embodiment 2

[0041] Mix 10 grams of ethyl orthosilicate and 10 grams of methanol in a 100 ml three-necked flask with a reflux condenser. 6 grams of concentrated phosphoric acid was quickly added to the above mixed solution, stirred and heated to 100°C, and the above sol formed a uniform gel after refluxing for about 0.5 hours. Separate the formed gel, put it in a vacuum oven, and treat it under vacuum at 100°C for 24 hours to obtain a silicon-based solid acid, which is stored in a desiccator. Measure its acid strength H 0 -10, the measured acid content was 2.8mmol / g, and the reaction performance was evaluated in a fixed-bed reaction system. The reaction results in 8 hours are shown in Table 6. The solid acid obtained in this embodiment has an acid content of 70% by weight before and after the reaction by acid-base titration.

[0042] Olefin Conversion

Embodiment 3

[0044] Mix 100 grams of aluminate and 30 grams of ethanol in a 250 ml three-neck flask with a reflux condenser, heat to boiling, then quickly add 12 grams of 20% sulfuric acid to the above mixed solution, and stir for 1 hour under reflux to form The gel was separated, put into a vacuum oven, and treated under vacuum at 100° C. for 48 hours to obtain an aluminum-based solid acid, which was stored in a desiccator. The measured acid strength was -12, and the measured acid content was 1.8mmol / g. The reaction performance was evaluated in a fixed-bed reaction system, and the 8-hour reaction results are shown in Table 7. The acid content of the solid acid obtained in this embodiment before and after the reaction by acid-base titration is 15% by weight.

[0045] Olefin Conversion

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Abstract

The present invention is solid acid catalyst and its preparation. The solid acid catalyst contains liquid acid in 1-80 wt% and solid matter to coat the liquid acid in 20-99 wt%; and the liquid acid is hydrogen sulfate or hydrogen phosphate with one C1-C10 alkyl radical and contains sulfuric acid or phosphoric acid selectively with the ratio between sulfuric acid or phosphoric acid and hydrogen sulfate or hydrogen phosphate being 0-95 to 5-100. The solid acid catalyst of the present invention has a large number of acid centers distributed homogeneously and the active centers have the solid shape and the reaction performance of liquid acid. The catalyst is suitable for use in low temperature reaction of non-polar medium.

Description

technical field [0001] The invention relates to an acid catalyst in solid form and a preparation method thereof. Background technique [0002] h 2 SO 4 、H 3 PO 4 , HF and other catalysts are acid catalysts widely used in industry. Some important processes such as alkylation, esterification, isomerization, etc. have used these catalysts or are still in use. Although these acid catalysts have good catalytic activity, because these catalysts are catalyzed under homogeneous conditions, compared with heterogeneous reactions, they bring many disadvantages in production, such as difficult to achieve continuous production in the process , The catalyst is not easy to separate from the raw materials and products, and the equipment is corroded. In addition, in some important chemical processes, the above-mentioned acid catalysts also bring a large amount of by-products. Taking alkylation as an example, the traditional process uses sulfuric acid or hydrofluoric acid as a catalyst ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J35/02
Inventor 谢文华付强舒兴田闵恩泽
Owner CHINA PETROLEUM & CHEM CORP
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