Loaded organic sulfoacid solid catalyst and preparation method thereof

A solid catalyst, organic sulfonic acid technology, applied in the field of catalysis, can solve problems such as low acidity, achieve the effects of high catalytic efficiency, good solvent stability, and increase acid content

Inactive Publication Date: 2012-07-25
山东华阳油业有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] For this reason, the technical problem to be solved by the present invention lies in the low acidity problem of organic sulfonic acid solid catalyst in the prior art, and then provides a kind of loaded organic sulfonic acid with higher acid content, better catalytic activity, better stability solid catalyst

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] The supported organic sulfonic acid solid catalyst described in this embodiment is prepared by the following method:

[0037] (1) Impregnation load: Take 30g of macroporous activated carbon and soak it in 120g of 20% nitric acid aqueous solution for activation, and stir and react at 70°C for 2h. The reaction product was washed repeatedly with distilled water until the filtrate was neutral. After suction filtering to remove water, dry at 100°C for 24 hours for later use;

[0038] A 20% styrene solution with a mass fraction of 17ml (15.402g) of styrene and 68ml of dichloromethane was prepared, and 0.077g of azobisisobutyronitrile was added to prepare an impregnation solution. The activated carrier is impregnated in the manner of equal-volume impregnation using a titration operation method.

[0039] (2) Polymerization of styrene: After argon gas was filled into the reaction system from which the organic solvent was removed for 2 min, the reaction was carried out at 80° C...

Embodiment 2

[0044] The supported organic sulfonic acid solid catalyst described in this embodiment is prepared by the following method:

[0045] (1) Immersion loading: 30 g of diatomaceous earth was soaked in 240 g of 40% nitric acid aqueous solution for activation, and stirred and reacted at 90° C. for 2 h. The reaction product was washed repeatedly with distilled water until the filtrate was neutral. After suction filtering to remove water, dry at 100°C for 24 hours for later use;

[0046] 7.8ml of styrene (7.07g) and 11.7ml of acetone solution were used to prepare a 40% styrene solution, and 0.141g of benzoyl peroxide was added to prepare the impregnation solution. The activated carrier is impregnated by equal volume impregnation.

[0047](2) Polymerization of styrene: argon gas was filled into the reaction system from which the acetone solvent was removed for 2 minutes, and then reacted at 50° C. for 30 hours in a closed state, so that the supported styrene was polymerized. The obt...

Embodiment 3

[0052] The supported organic sulfonic acid solid catalyst described in this embodiment is prepared by the following method:

[0053] (1) Impregnation load: Take 30g of activated carbon and place it in 60g of 5% methanesulfonic acid solution for activation, and stir and react at 50°C for 2h. The reaction product was washed repeatedly with distilled water until the filtrate was neutral. After suction filtering to remove water, dry at 100°C for 24 hours for later use;

[0054] 24mL of styrene (21.84g) and 227mL of toluene were used to prepare an impregnation solution with a mass fraction of 10%, and 0.655g of azobisisobutyronitrile was added to prepare the impregnation solution. Take 10 g of the previously activated activated carrier and immerse it in the above impregnation solution, and impregnate the load by soaking in excess solution.

[0055] (2) Styrene polymerization: fill the reaction system with argon protection, stir at 110°C for 6 hours, then filter with suction, and ...

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Abstract

The invention belongs to the technical field of catalysis, in particular relates to a solid acid catalyst loaded with organic sulfoacid groups by an immersion method and a preparation method of the solid acid catalyst. The method for preparing the catalyst provided by the invention comprises the following steps: (1) throwing an activated carrier into an immersion solution prepared from styrene, an initiator and an organic solvent to immerse and load; (2) in the presence of protective gas, allowing styrene to conduct a polymerization reaction to obtain a load precursor loaded with polystyrene monomolecular film on the surface; and (3) mixing and sulfonating the load precursor and a sulfonating agent, and the like. The loaded organic sulfoacid solid catalyst utilizes the polymerization reaction of styrene for ensuring that the active groups of the catalyst partially form the structure of polystyrene, and after the sulfonating reaction, a plurality of sulfo group structures can be formed in each active group, so that the acid content of the whole catalyst is greatly improved; and the degree of polymerization of polystyrene in the catalyst can reach 2-100, and the quantity of the loaded sulfoacid groups is greatly increased.

Description

technical field [0001] The invention belongs to the technical field of catalysis, and in particular relates to a solid acid catalyst loaded with organic sulfonic acid groups by an impregnation method and a preparation method thereof. Background technique [0002] Acid-catalyzed reactions are one of the most important reactions in the chemical industry. Acid-catalyzed reactions involve petroleum refining processes such as hydrocarbon cracking, reforming, and isomerization, as well as olefin hydration, olefin polymerization, aromatic hydrocarbon alkylation, and aromatic hydrocarbon acylation. , Alkyd esterification and other petrochemical and fine chemical processes, it can be said that acid catalysts are the basis of this series of important industrial reactions. At present, liquid acid catalysts are still widely used in industrial production, such as H 2 SO 4 , HF, etc. However, liquid acid is easy to corrode equipment during use, requires special neutralization steps to ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/06B01J35/10C07C67/08C07C69/78
Inventor 徐永强林殷平商红岩盖帅李红娟刘晨光
Owner 山东华阳油业有限公司
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