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Method for preparing loading type ferric oxide catalyst

A preparation process and catalyst technology, which is applied in the direction of catalyst activation/preparation, physical/chemical process catalyst, catalyst carrier, etc. It can solve the problems of continuous organic synthesis operation of iron oxide, difficulty in ensuring product quality, and low production efficiency. , to achieve the effect of low iron content, long service life and good chroma

Inactive Publication Date: 2007-03-14
BOHAI UNIV
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  • Summary
  • Abstract
  • Description
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  • Application Information

AI Technical Summary

Problems solved by technology

At present, a new process for the synthesis of fine chemicals using iron oxide as an acylation catalyst has been developed. Iron oxide is a cheap and effective catalyst for the acylation of aromatic hydrocarbons, which can replace expensive AlCl in the preparation of certain organic compounds. 3 、TiCl 3 etc., in "US 5,296,636" and "Lv Jiuzhuo, 2,4,6,-Synthesis of trimethylbenzoic acid, fine petrochemical industry, 2001.3: 1", iron oxide was used as catalyst to effectively realize the acylation of aromatic hydrocarbons, but The usual iron oxide is in the form of powder, which is difficult to separate from the product during the organic synthesis reaction, and makes the product contain a large amount of iron, making it difficult to guarantee the quality of the product
On the other hand, powdered iron oxide is difficult to realize continuous organic synthesis operation, making the production efficiency low
Therefore, there are certain difficulties in industrial production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] At room temperature, 30 parts Fe(NO 3 ) 3 .6H 2 O, 5 Co(NO 3 ) 2 .4H 2 O and 65 parts of water are mixed to prepare an impregnation solution. Add 5 grams of 4A molecular sieve carrier to 25 grams of the prepared impregnation solution for 7 hours; then filter, dry at 120°C for 3 hours, then put it in a muffle furnace, and heat up to 450°C at a rate of 5°C / second Calcined for 4 hours to obtain a catalyst supported by iron oxide. The catalyst is used in the acylation reaction of mesitylene and chloroacetyl chloride, the conversion rate of mesitylene is 78%, and the selectivity of chloroacetyl 2,4,6-trimethylbenzene is 92%.

[0018] The activity of catalyst provided by the invention has been tested with following method:

[0019] The acylation reaction in the present invention is carried out in a round bottom flask with a reflux device, using mechanical stirring. The reaction process is: add a certain amount of catalyst provided by the present invention in mesitylen...

Embodiment 2

[0021] At room temperature, 30 parts Fe(NO 3 ) 3 .6H 2 O, 5 parts Ni(NO 3 ) 2 .4H 2 O and 65 parts of water are mixed to prepare an impregnation solution. 5 g TiO 2 The sieve carrier is added to 25 grams of the prepared impregnation solution and immersed for 7 hours; then filtered, dried at 120°C for 3 hours, then placed in a muffle furnace, and roasted at 5°C / second to 450°C for 4 hours. Then repeat the above steps twice. The catalyst is used in the acylation reaction of mesitylene and chloroacetyl chloride, the conversion rate of mesitylene is 88%, and the selectivity of chloroacetyl 2,4,6-trimethylbenzene is 94%.

Embodiment 3

[0023] At room temperature, 30 parts Fe(NO 3 ) 3 .6H 2 O, 5 Co(NO 3 ) 2 .4H 2 O and 65 parts of water are mixed to prepare an impregnation solution. 5 g α-Al 2 o 3 The carrier was added to 25 grams of the prepared impregnation solution and immersed for 7 hours; then filtered, dried at 120°C for 3 hours, then placed in a muffle furnace, and baked at 450°C for 4 hours at a rate of 5°C / sec. Repeat the above steps twice. The catalyst is used in the acylation reaction of mesitylene and chloroacetyl chloride, the conversion rate of mesitylene is 97%, and the selectivity of chloroacetyl 2,4,6-trimethylbenzene is 95%.

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Abstract

The invention relates to a method for producing carrier ferric oxide catalyst used to make aromatic hydrocarbons acyl. Wherein, it is characterized in that: it uses the mixture of metal oxide, zeolite molecule screen or metal oxide and zeolite molecule screen as carrier, uses the water solution of ferric salt, nickel salt, or cobalt salt as emerge liquid; (1) emerging said carrier for 6-12hours; (2) drying the carrier for 3-8hours at 60-150Deg. C, and baking it for 4-12hours under 300-700Deg. C, to obtain the precursor of catalyst; (3) repeating said operations to obtain final product. The invention can improve the activity, selectivity of catalyst, and reduce the iron content.

Description

technical field [0001] The invention belongs to the field of preparation technology of supported catalysts, in particular to a preparation technology of supported iron oxide catalyst for acylation of aromatic hydrocarbons. Background technique [0002] The acylation products of aromatic hydrocarbons are very important chemical products and are widely used in the synthesis of pharmaceutical, chemical and electronic products. The catalyst commonly used in the industry for the acylation of aromatic hydrocarbons is AlCl 3 , but with AlCl 3 The dosage is relatively large, and a large amount of acid gas will be generated during the reaction and post-treatment process, which will seriously corrode the equipment. At present, a new process for the synthesis of fine chemicals using iron oxide as an acylation catalyst has been developed. Iron oxide is a cheap and effective catalyst for the acylation of aromatic hydrocarbons, which can replace expensive AlCl in the preparation of cert...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J37/02B01J23/74B01J32/00B01J29/80
Inventor 钱建华张连红王道林刘琳邢锦娟李晓光龚树华
Owner BOHAI UNIV
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