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Composite solid acid catalyst as well as preparation method and application thereof

A technology of composite solid acid and catalyst, applied in chemical instruments and methods, preparation of organic compounds, catalysts for physical/chemical processes, etc., can solve the problem of low catalyst activity and achieve the effect of strong acidity, high selectivity and good activity

Active Publication Date: 2014-08-20
湖南瑞冠生物化工科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The purpose of this invention is to provide a kind of composite solid acid catalyst, to overcome the not high defect of catalyst activity in the prior art, and the application of this catalyst in the synthesis of 2,6-di-tert-butyl-4-methylphenol

Method used

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  • Composite solid acid catalyst as well as preparation method and application thereof
  • Composite solid acid catalyst as well as preparation method and application thereof
  • Composite solid acid catalyst as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] 1. Composite solid acid [(SO 4 2- +ZnCl 2 ) / silica gel] catalyst preparation

[0025] Using silica gel as a carrier, water as a solvent, and p-cresol to be reacted as a benchmark, according to p-cresol: carrier (silica gel) = 1: 0.03 (mass ratio), p-cresol: ZnCl 2 =1:0.33% (mass ratio), p-cresol:H 2 SO 4 =1:0.66% (mass ratio) to prepare a composite solid acid catalyst.

[0026] After thermal pretreatment, the silica gel was placed in 0.7mol / L ZnCl 2 Soak in water solution overnight, then dry. Then add 1mol / L of H 2 SO 4 The aqueous solution was immersed overnight, and after drying, it was activated at 200°C for 3 hours.

[0027] 2. Preparation of 2,6-di-tert-butyl-4-methylphenol

[0028] In a 100mL round-bottomed flask with a magnetic stirrer, condenser, thermometer and isobutylene introduction tube, add 7.5g p-cresol and the composite solid acid [(SO 4 2- +ZnCl 2 ) / Silicone] Catalyst, a balloon is fixed on the top of the condensation tube to play a role of...

Embodiment 2

[0036] 1. Composite solid acid [(SO 4 2- +ZnCl 2 ) / silica gel] catalyst preparation

[0037] With silica gel as carrier, with water as solvent, take p-cresol to be reacted as benchmark, according to p-cresol: carrier (silica gel)=1:0.03 (mass ratio), p-cresol: ZnCl 2 =1:0.66% (mass ratio), p-cresol:H 2 SO 4 =1:0.66% (mass ratio) to prepare a composite solid acid catalyst.

[0038] After thermal pretreatment, the silica gel was placed in ZnCl 2 Soak overnight in aqueous solution, then dry. Then add 1mol / L of H 2 SO 4 The aqueous solution was immersed overnight, and after drying, it was activated for 3 hours, and the activation temperature was 250°C, 200°C and 150°C for comparative tests.

[0039] 2. Preparation of 2,6-di-tert-butyl-4-methylphenol

[0040]In a 100mL round-bottomed flask with a magnetic stirrer, condenser tube, thermometer and isobutylene inlet tube, add 7.5g p-cresol and the composite solid acid [(SO 4 2- +ZnCl 2 ) / Silicone] Catalyst, fix a balloon ...

Embodiment 3

[0047] 1. Composite solid acid [(SO 4 2- +ZnCl 2 ) / silica gel] catalyst preparation

[0048] The preparation method of the catalyst is the same as in Example 2, but the activation temperature is 200°C.

[0049] 2. Preparation of 2,6-di-tert-butyl-4-methylphenol

[0050] 7.5g p-cresol and the prepared composite solid acid [(SO 4 2- +ZnCl 2 ) / silica gel] catalyst was added to a 100 mL round bottom flask equipped with a magnetic stirrer, condenser, thermometer and isobutylene inlet. Fix a balloon on the top of the condenser for sealing and safety. Raise the temperature of the reactant to 80°C while stirring; slowly feed high-purity isobutene gas and adjust the feeding speed to ensure that no gas overflows the reaction device. Ventilation was done for 4h and 8h respectively, and the ventilation was stopped.

[0051] 3. Analysis of crude product of 2,6-di-tert-butyl-4-methylphenol

[0052] Sampling was taken from the crude product of 2,6-di-tert-butyl-4-methylphenol obtai...

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Abstract

The invention belongs to the technical field of organic synthesis and provides a composite solid acid catalyst. The composite solid acid catalyst is (SO4<2->+ZnCl2) / silica gel and is formed by compositing zinc chloride, sulfuric acid and silica gel. A preparation method of the catalyst comprises the following steps: hot pretreating the silica gel, dipping in zinc chloride solution, drying, adding into sulfuric acid solution, dipping for one night, drying and activating to obtain the (SO4<2->+ZnCl2) / silica gel composite solid acid catalyst. The composite solid acid catalyst provided by the invention has the characteristics of strong acidity, good activity, high selectivity, recyclability and environmental friendliness; when being used for synthetizing 2, 6-di-tert-butyl-4-methylphenol, the composite solid acid catalyst has the characteristics of simplicity and convenience in operation, low reaction temperature, normal pressures, no use of any organic solvent, high conversion ratio, short reaction time, high selectivity and environmental friendliness; the composite solid acid catalyst meets the requirements of green process and is very suitable for industrial production.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and in particular relates to a composite solid acid catalyst, a preparation method thereof and the application of the catalyst in synthesizing 2,6-di-tert-butyl-4-methylphenol. Background technique [0002] The chemical name of BHT (Butylated Hydroxytoluene) is 2,6-di-tert-butyl-4-methylphenol, commonly known as antioxidant 264 (the rubber industry in my country is used to call it antioxidant, and the synthetic resin and plastic industry is used to call it antioxidant. Also known as stabilizer), also known as T501. It is a general-purpose phenolic antioxidant with a wide range of uses and a large dosage. It can be used in synthetic rubber, synthetic resin and plastics, petroleum products (lubricating oil, grease, paraffin, etc.), food and feed, etc. [0003] BHT has a long history of development since its industrialization in 1937. Although it is an old variety of phenolic anti-aging ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/138C07C37/14C07C39/06
Inventor 胡汉忠赵振华高晓慧陈弘
Owner 湖南瑞冠生物化工科技有限公司
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