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Prepn process of solid super acidic catalyst

A solid super acid, catalyst technology, applied in chemical instruments and methods, physical/chemical process catalysts, chemical/physical processes, etc., can solve the problems of insignificant, inconspicuous, and low specific surface area of ​​dispersion effect, and achieve the distribution of acid centers. The effect of uniformity, increasing acid content and good thermal stability

Inactive Publication Date: 2003-06-04
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The current research results show that there are two main reasons for limiting the density of such solid superacid acid centers: one reason is that the number of acid centers formed is limited due to its low specific surface area, and some studies will make the acid-promoting type The solid superacid is loaded on a certain carrier, but the dispersion effect is not obvious, so the effect of increasing the acid content is not obvious; another reason is that this type of solid superacid is formed by the combination of sulfate anion and oxide, and the existing The preparation conditions relying solely on the oxide itself cannot provide enough binding sites, which also limits the number of acid centers of this type of solid superacid

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] 12 grams of methyl orthosilicate and 2 grams of ethanol are mixed in a 100ml beaker, and then 20ml of a zirconium oxychloride solution with a concentration of 33% by weight is added to the above mixed solution, and 1:1 ammonia water is added dropwise while stirring until the pH is 6. Aging for 24 hours, filtered and washed, dried at 50°C for 48 hours, and then 1 g of Zr(SO 4 ) 2 It was dissolved in 10 ml of sulfuric acid with a concentration of 5% by weight, impregnated with the obtained solid for 2 hours, and then roasted at 500° C. for 4 hours to obtain a solid superacid. Measure its acid strength H 0 <-14.6, acid content 1.2mmol / g, alkylation reaction activity was evaluated in a fixed bed reaction system, the results are shown in Table 3.

[0034] Olefin Conversion

Embodiment 2

[0036] Mix 12 grams of methyl titanate and 20 grams of butanol in a 100ml beaker, then add 4ml of zirconium oxychloride solution with a concentration of 33% by weight into the above mixed solution, and add 1:1 ammonia water dropwise while stirring until the pH is 6 , aged for 24 hours, filtered and washed, dried at 50°C for 48 hours, and then 1 g of Zr(SO 4 ) 2 It was dissolved in 10 ml of sulfuric acid with a concentration of 5% by weight, impregnated with the obtained solid for 2 hours, and then roasted at 500° C. for 4 hours to obtain a solid superacid. Measure its acid strength H 0 <-14.6, acid content 1.0mmol / g, alkylation reaction activity was evaluated in a fixed bed reaction system, the results are shown in Table 4.

[0037] Olefin Conversion

Embodiment 3

[0039] Mix 12 grams of methyl orthosilicate and 10 grams of propanol in a 100ml beaker, then add 16ml of ferric chloride solution with a concentration of 33% by weight into the above mixed solution, stir while adding 1:1 ammonia water dropwise until the pH is 6 , aged for 24 hours, filtered and washed, dried at 50°C for 48 hours, and then 1 g of Zr(SO 4 ) 2 It was dissolved in 10 ml of sulfuric acid with a concentration of 5% by weight, impregnated with the obtained solid for 2 hours, and then roasted at 500° C. for 4 hours to obtain a solid superacid. Measure its acid strength H 0 <-14.6, acid content 1.2mmol / g, alkylation reaction activity was evaluated in a fixed bed reaction system, the results are shown in Table 5.

[0040] Olefin Conversion

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PUM

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Abstract

The preparation process of solid acidic catalyst includes: dissolving organic ester in C1-C10 alcohol to prepare solution, mixing the ester alcohol solution with water solution of compound of Zr, Ti,Fe or Al, regulating the pH of the mixture solution with alkali solution to 6-11, ageing of the mixture in the temperature of room temperature to 100 deg.C for 1-24 hr, and filtering to obtain solid;water washing the solid, drying in 50-200 deg.c for 2-48 hr; dissolviong zirconium sulfate in the water solution of sulfuric acid of 1-15% concentration, soaking the solid in the solution, and roasting the product at 500-800 deg.c for 1-24 hr. The solid acidic catalyst of the present invention has high acidity, high reaction activity and high selectivity.

Description

technical field [0001] The present invention relates to a kind of preparation method of solid superacid catalyst, relate to a kind of SO 4 ＝ The preparation method of / oxide type solid superacid catalyst. Background technique [0002] A super acid is one with an acid strength higher than 100% sulfuric acid, i.e. H 0 <-12.0 acid, the solid acid with such an acid strength is a solid superacid (R.J.Gillespie, T.E.Peel, Adv.Phys.Org.Chem., 9, 1 (1972); J.Am.Che.Soc. , 95, 5173 (1973)). Super acid has extremely high acid strength, especially liquid super acid, such as Friedl-Crafts acid catalyst, the acid strength is 10% of 100% sulfuric acid 3 to 10 6 times, and the acid strength of fluorosulfonic acid and some corresponding conjugated systems known as magic acid is as high as 10% of 100% sulfuric acid 7 to 10 9 Therefore, superacids can activate saturated hydrocarbons that are almost inactive under normal reaction conditions, enabling reactions such as isomerization, d...

Claims

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Application Information

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IPC IPC(8): B01J27/053
Inventor 谢文华付强舒兴田闵恩泽
Owner CHINA PETROLEUM & CHEM CORP
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