Solid base catalyst for synthesis of 3, 5-dimethylphenol from acetone by vapor phase method, and preparation method and application thereof

A solid base catalyst, dimethylphenol technology, applied in catalyst activation/preparation, preparation of organic compounds, chemical elements of heterogeneous catalysts, etc., can solve the problems of low yield of 3,5 dimethylphenol, etc. The effect of high product selectivity, easy product and less carbon formation

Pending Publication Date: 2022-05-27
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In a word, the yield of 3,5 dimethylphenol synthesized by acetone gas phase method is generally low at present

Method used

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  • Solid base catalyst for synthesis of 3, 5-dimethylphenol from acetone by vapor phase method, and preparation method and application thereof
  • Solid base catalyst for synthesis of 3, 5-dimethylphenol from acetone by vapor phase method, and preparation method and application thereof
  • Solid base catalyst for synthesis of 3, 5-dimethylphenol from acetone by vapor phase method, and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0058] (1) ZrOCl 2 ·8H 2 O 104.6g (0.325mol) was dissolved in distilled water to prepare a solution with a Zr concentration of 0.1mol / L, and La(NO) was added. 3 ) 3 0.32g (0.000985mol), heated in a water bath to 70°C, add 10wt% ammonia water dropwise under stirring at 300rpm to adjust the pH to 9-10, continue stirring for 1.5h to fully react to obtain a suspension, and then at room temperature Aged at 25°C for 20h, the reaction solution was filtered and washed until no chloride ions were present, then dried at 100°C for 10h, and ZrO with a particle size of 3-5mm was sieved after grinding. 2 / La 2 O 3 composite carrier;

[0059] (2) Take Sr (NO 3 ) 2 , Ca(NO 3 ) 2 , Co(NO 3 ) 2 ·6H 2 O 3.67g (0.01734mol), 6.58g (0.04012mol), 2.966g (0.01019mol), wherein strontium: calcium: cobalt mass ratio is 1: 1.05: 0.4, after mixing, add 200g distilled water to prepare a solution, step ( 1) ZrO 2 / La 2 O 3 40 g of the composite carrier was added to the solution, left to sta...

Embodiment 2

[0062] (1) Zr (SO 4 ) 2 91.95g was dissolved in distilled water to prepare a solution with a Zr concentration of 0.06mol / L, and La(NO) was added. 3 ) 3 0.66g, heated in a water bath to 70°C, add 15% ammonia water dropwise under stirring to adjust pH to 9-10, continue stirring to fully react for 1.5h to obtain a suspension, and then age at room temperature for 25h, the reaction The liquid was filtered and washed until there was no chloride ion, and then dried at 110 °C for 8 hours. After grinding, ZrO with a particle size of 3 to 5 mm was sieved. 2 / La 2 O 3 composite carrier.

[0063] (2) Take Sr(Cl) respectively 2 , Ca(Cl) 2 , Co(Cl) 2 3.60g, 6.53g, 1.96g, wherein the mass ratio of strontium: calcium: cobalt is 1: 1.18: 0.45, after mixing, add 200g of distilled water to prepare a solution, mix the ZrO of step (1) 2 / La 2 O 3 40 g of the composite carrier was added to the solution, left to stand for 14 hours of immersion, taken out and dried at 100 °C for 8 hours,...

Embodiment 3

[0066] (1) ZrOCl 2 ·8H 2 O 104.6g was dissolved in distilled water to prepare a solution with a Zr concentration of 0.08mol / L, and La(NO) was added. 3 ) 3 0.40g, heated in a water bath to 70°C, add 15% ammonia water dropwise under stirring to adjust pH to 9-10 to make it fully react, continue stirring for 1.5h to obtain a suspension, then age at room temperature for 25h, The reaction solution was filtered and washed until there was no chloride ion, and then dried at 110 °C for 8 hours. After grinding, ZrO with a particle size of 3 to 5 mm was sieved. 2 / La 2 O 3 composite carrier.

[0067] (2) Take SrSO separately 4 , Ca(NO 3 ) 2 , CoSO 4 1.53g, 3.78g, 1.42g, wherein the mass ratio of strontium: calcium: cobalt is 1:1.27:0.74, after mixing, add 200g of distilled water to prepare a solution, mix the ZrO of step (1) 2 / La 2 O 3 40 g of the composite carrier was added to the solution, left to stand for 16 hours, dried at 100 °C for 8 hours, and then heated to 750 °C...

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Abstract

The invention discloses a solid base catalyst for synthesizing 3, 5-dimethylphenol from acetone by using a gas phase method as well as a preparation method and application of the solid base catalyst. The solid base catalyst comprises a ZrO2 / La2O3 composite carrier and active components, namely SrO, CaO and CoO, based on the total mass of the catalyst, the content of the ZrO2 / La2O3 composite carrier is 75-95%, and the content of the La element is 0.1-1%; in the active component, the content of SrO is 1-10%, the content of CaO is 1-10%, and the content of CoO is 0.1-3%. The solid base catalyst is used for catalyzing acetone gas phase synthesis of 3, 5-dimethylphenol, the acetone conversion rate can reach 80-90%, the product selectivity can reach 80-90%, and the carbon deposition amount is small. The process has the advantages of low cost, less carbon deposition, simple product separation, low equipment and material investment and simple three-waste treatment.

Description

technical field [0001] The invention belongs to the technical field of compound preparation, and in particular relates to a preparation method of a solid base catalyst and a method for preparing 3,5-dimethylphenol by using the catalyst to catalyze acetone. Background technique [0002] 3,5-Dimethylphenol is an important fine chemical raw material and organic chemical intermediate. It has many downstream products and a wide range of applications. It is mainly used for the preparation of resin adhesives, fungicides, vitamin E, and also for rubber promotion. Agents, pesticides, antioxidants, inks, coatings and other chemical fields. [0003] The methods for producing 3,5-dimethylphenol mainly include coal tar extraction, m-xylene sulfonation, isophorone aromatization, and acetone gas-phase synthesis. Among them, the coal tar extraction method has high separation cost and low product yield and purity; the m-xylene sulfonation method has complicated technological process, seriou...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/83B01J37/03B01J37/08B01J37/02C07C45/74C07C49/203C07C49/603C07C37/07C07C39/07
CPCB01J23/83B01J23/002B01J37/038B01J37/082B01J37/0201B01J37/088C07C45/74C07C37/07B01J2523/00C07C2601/16B01J2523/23B01J2523/24B01J2523/3706B01J2523/48B01J2523/845C07C49/203C07C49/603C07C39/07Y02P20/52
Inventor 董科刘振峰安丽艳牟通刘超赵聪王加琦
Owner WANHUA CHEM GRP CO LTD
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