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Preparation method of solid acid catalyst

A solid acid catalyst and solid technology, applied in the field of chemical reagent synthesis, can solve the problems of limited acid strength and acid amount, difficult recycling and reuse, etc., and achieve the effects of strong acidity, good recycling performance, and simple and easy synthesis method

Inactive Publication Date: 2015-07-29
陕西延长石油(集团)有限责任公司炼化公司
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  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to overcome the problem that the existing solid acid catalyst is prone to partial dissolution, swelling and fragmentation in the catalytic reaction, difficult to recycle and reuse, and the acid strength and acid amount are limited

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  • Preparation method of solid acid catalyst
  • Preparation method of solid acid catalyst
  • Preparation method of solid acid catalyst

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Embodiment 1

[0029] In order to overcome the problems that the existing solid acid catalysts are prone to partial dissolution, swelling and fragmentation in the catalytic reaction, difficult to recycle and reuse, and the acid strength and calculation amount are limited, this embodiment provides a preparation method of a solid acid catalyst, including the following step:

[0030] Step 1) hydrolysis: take by weighing 7.012 g SnCl 4 ·5H 2 O, 13.280 g TiCl 4 , 2.414 g AlCl 3 ·6H 2 O (the molar percentage of metal is 20%:70%:10%), it was dissolved in 500 mL of water, and fully stirred to make it completely dissolved.

[0031] Step 2) neutralization: adding 10% sodium hydroxide solution to the above solution to adjust to pH=10.

[0032] Step 3) aging and washing: after the neutralized solution was left to age for 15 hours, it was washed 3 times with deionized water.

[0033] Step 4) drying: the above-mentioned washed solid is placed in an oven for 100 oC Dry for 15 hours.

[0034] Step ...

Embodiment 2

[0038] Weigh 7.012 g SnCl 4 ·5H 2 O, 15.177 g TiCl 4 , 1.363 g ZnCl 2 (the molar percentage of metal is 10%:80%:10%), dissolve it in 450 mL of water, fully stir to dissolve, add ammonia water with a concentration of 10% to the solution to adjust to pH=9; After aging for 20 hours, use deionized water to wash 5 times, and the washed solid is placed in an oven for 90 oC Dry for 20 hours; the dried solid powder is fully ground and passed through a 100-mesh sieve, and a certain amount of ammonium sulfate (mass is 20% of the solid powder) is weighed, and it is fully mixed with the ground solid powder after sieving ; The mixed solid powder is placed in the muffle furnace, 450 o C was calcined for 15 h to obtain a solid acid catalyst.

[0039] by pyridine IR and NH 3 -TPD characterizes the solid acid catalyst prepared by the present embodiment, and the results are as follows figure 2 and Figure 4 As shown, it shows that the synthesized solid acid catalyst contains both Lewi...

Embodiment 3

[0041] Weigh 3.506 g SnCl 4 ·5H 2 O, 18.656 g ZrCl 4 , 1.363 g ZnCl 2 , 1.207 g AlCl 3 ·6H 2 O (the molar percentage of metal is 5%:80%:10%:5%), it was dissolved in 750 mL water, fully stirred to dissolve, and the concentration of 5% potassium hydroxide was added to the solution to adjust to pH=8; After the neutralized solution was left to age for 10 hours, it was washed 3 times with deionized water; the washed solid was placed in an oven for 80 oC Dry for 10 hours; the dried solid powder is fully ground and passed through a 100-mesh sieve, and a certain amount of ammonium sulfate and ammonium chloride mixture is weighed, the total mass of which is 5% of the solid powder, and it is mixed with the ground solid The sieved powder is fully mixed; the mixed solid powder is placed in a muffle furnace, 300 o C was calcined for 3 h to obtain a solid acid catalyst.

[0042] The characterization shows that the solid acid catalyst synthesized in this example contains both Lewis a...

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Abstract

The invention particularly provides a preparation method of a solid acid catalyst. The method comprises the following steps: using metal chlorides as raw materials, performing hydrolysis, neutralization, aging, washing and drying, so as to obtain solid powder; fully grinding the solid powder, mixing the ground solid powder with ammonium salt, and roasting, so as to obtain the solid acid catalyst. According to the preparation method of the solid acid catalyst, the raw materials are low in cost and easy to obtain, the synthetic method is simple, and the analysis on a test result shows that the synthesized solid acid catalyst is high in acidity and excellent in heat stability, so that the preparation method has wide application prospect.

Description

technical field [0001] The invention belongs to the technical field of chemical reagent synthesis, and in particular relates to a preparation method of a solid acid catalyst. Background technique [0002] Acids are an important class of catalysts, which can be used to catalyze esterification reactions, Friedel-Crafts reactions, and aldol condensation reactions. Most of the acid catalysts currently used in industry are liquid acid catalysts, such as sulfuric acid, phosphoric acid, nitric acid, hydrochloric acid, p-toluenesulfonic acid, etc. Because the reaction catalyzed by liquid acid is a homogeneous reaction, the catalytic activity is high, but the liquid acid catalyst has problems such as corrosion of equipment, difficulty in separating from the product, and difficulty in recycling and reuse. [0003] Due to the advantages of easy separation from products and recyclability, solid acid has attracted extensive attention from academia and industry in recent years. The soli...

Claims

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Application Information

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IPC IPC(8): B01J27/24
Inventor 罗万明李军金德浩李稳宏王军峰李铖刘俊霞陈景润李佳王双福
Owner 陕西延长石油(集团)有限责任公司炼化公司
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