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A method for preparing 3,5-dimethylphenol

A technology of dimethylphenol and catalyst, applied in the field of preparation of 3,5-dimethylphenol, which achieves the effects of less pollution, reduced filling frequency, and reduced material consumption and energy consumption

Active Publication Date: 2017-10-13
CHAMBROAD CHEM IND RES INST CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there is no report that a heterogeneous catalyst can realize the continuous operation of the reaction under the condition of ensuring product selectivity. For the first time, we applied the multi-component oxide prepared by precipitation hydrothermal or sol-gel method to this reaction, which can realize Product selectivity realizes the continuous operation of the reaction under higher conditions, and can realize the large-scale production of products

Method used

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  • A method for preparing 3,5-dimethylphenol
  • A method for preparing 3,5-dimethylphenol
  • A method for preparing 3,5-dimethylphenol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] 1. Put the 20-40 mesh iron-nickel-chromium mixed oxide catalyst into the constant temperature zone of the stainless steel reaction tube of the fixed-bed microreactor.

[0028] 2. Use a metering pump to continuously inject the raw material isophorone into the catalyst bed of the fixed-bed microreactor, and carry out aromatization reaction with the iron-nickel-chromium mixed oxide catalyst. The reaction temperature is 450°C, the pressure is 1.5MPa, and the mass is empty. The speed is 0.5h -1 , the nitrogen flow rate is 20ml / min, and the reaction time is 5h, that is, the aromatization of isophorone catalyzed by iron-nickel-chromium mixed oxide is completed to prepare 3,5-dimethylphenol;

[0029] The iron-nickel-chromium mixed oxide catalyst described in this example is synthesized by a co-precipitation hydrothermal method, and the specific synthesis method is as follows: ferric nitrate nonahydrate, nickel nitrate hexahydrate, and chromium nitrate nonahydrate are mixed acco...

Embodiment 2

[0034] 1. Put the 20-40 mesh iron-nickel-chromium mixed oxide catalyst into the constant temperature zone of the stainless steel reaction tube of the fixed-bed microreactor.

[0035] 2. Use a metering pump to continuously inject the raw material isophorone into the catalyst bed of the fixed-bed micro-reactor, and carry out aromatization reaction with the iron-nickel-chromium mixed oxide catalyst. The reaction temperature is 600°C, the pressure is 5MPa, and the mass space velocity for 2h -1, the nitrogen flow rate is 60ml / min, and the reaction time is 5h, that is, the preparation of 3,5-dimethylphenol by the catalyzed isophorone aromatization of iron-nickel-chromium mixed oxide is completed;

[0036] The iron-nickel-chromium mixed oxide catalyst described in this example is synthesized by co-precipitation hydrothermal method, and the specific synthesis method is as follows: iron nitrate nonahydrate, nickel nitrate hexahydrate, and chromium nitrate nonahydrate are divided into i...

Embodiment 3

[0041] 1. Load the 20-40 mesh iron-nickel-chromium mixed oxide catalyst into the constant temperature zone of the stainless steel reaction tube of the fixed bed microreactor.

[0042] 2. Using a metering pump, the raw material isophorone is continuously injected into the catalyst bed of the fixed-bed microreactor, and the aromatization reaction is carried out with the iron-nickel-chromium mixed oxide catalyst. The reaction temperature is 570 ° C, the pressure is 2.5 MPa, and the mass is empty. Speed ​​is 1h -1 , the nitrogen flow rate is 40ml / min, and the reaction time is 5h, that is, the iron-nickel-chromium mixed oxide catalyzed isophorone aromatization is completed to prepare 3,5-dimethylphenol;

[0043] The iron-nickel-chromium mixed oxide catalyst described in this example is synthesized by co-precipitation hydrothermal method, and the specific synthesis method is as follows: iron nitrate nonahydrate, nickel nitrate hexahydrate, and chromium nitrate nonahydrate are divide...

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Abstract

The invention relates to a method for preparing 3,5-dimethylphenol through an isophorone aromatization reaction catalyzed by a mixed oxide catalyst. The invention relates to a method for preparing 3,5-dimethylphenol. The method comprises the following steps: 1, an iron-nickel-chromium mixed oxide catalyst is sieved; 2, isophorone is subjected to an aromatization reaction with formed and roasted iron-nickel-chromium oxide. According to the invention, the iron-nickel-chromium oxide is synthesized with a precipitate hydrothermal method or a traditional sol-gel method. The iron-nickel-chromium oxide is used for catalyzing the isophorone aromatization reaction, such that defects such as non-continuous reaction, difficult separation with product, serious equipment corrosion and environment pollution caused by homogenous catalysts such as iodomethane are overcome. The catalyst has higher reactivity, higher 3,5-dimethylphenol selectivity and higher anti-coking capacity. The reaction product can be easily separated from the catalyst. Operation is simple. The method is suitable for large-scale productions.

Description

technical field [0001] The invention relates to a method for preparing 3,5-dimethylphenol, in particular to a method for preparing 3,5-dimethylphenol by catalyzing the aromatization of isophorone with an iron-nickel-chromium mixed oxide catalyst. Background technique [0002] 3,5-Dimethylphenol is an important industrial intermediate, mainly used in the production of antioxidants, antibiotics, resin adhesives and vitamin E, etc. It is also widely used in various antibacterial and anti-mildew treatments, such as leather Antibacterial and anti-mildew treatment of paper, textiles and photos. The demand for 3,5-dimethylphenol is increasing day by day in today's world, but the annual output of the world is relatively small, and the domestic output is even less, so it is difficult to meet the demand of the market. At present, the domestic production method of 3,5-dimethylphenol is the m-xylene sulfonation alkali solution method, which is complicated in process, seriously polluted...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07C39/07C07C37/07B01J23/86
CPCB01J23/002B01J23/866B01J2523/00C07C37/07C07C39/07B01J2523/842B01J2523/847B01J2523/67
Inventor 王文静李寿丽李顺凯郭文娟韩立霞李晓红
Owner CHAMBROAD CHEM IND RES INST CO LTD
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