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Preparation method of solid acid catalyst for preparing dimethyl dodecanedioate

A technology of dimethyl dodecanedioate and solid acid catalyst is applied in the preparation of organic compounds, chemical instruments and methods, catalysts for physical/chemical processes, etc. High selectivity and strong catalytic activity

Pending Publication Date: 2022-04-12
SINOPEC NANJING RES INST OF CHEM IND CO LTD +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, this kind of carbonized sulfonated solid acid catalyst still has the problems of easy pulverization and low mechanical strength during use, which limits its large-scale application

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] 20g charcoal particles, 10g SnCl 4 ·5H 2 O. Add 70g of diatomaceous earth to 250g of deionized water, stir for 2 hours, add concentrated ammonia water dropwise to adjust the pH to 6, add 10% binder to extrude and dry to obtain the precursor after suction filtration and drying. Soak the precursor in 1mol / L H 2 SO 4 The solution was dried after 12h, and the product was in N 2 Calcined at 450°C for 6h under protection to obtain the final solid acid catalyst. Take by weighing dodecanedioic acid 16g, methyl alcohol 27g, add a certain proportion catalyst, react certain hour on reflux reactor, its reaction result is as follows through gas chromatography detection after suction filtration:

[0030] (catalyst / acid) / % Reaction temperature / ℃ Conversion rates / % Selective / % 2 60 71 91 4 80 82 87 10 100 83 85

Embodiment 2

[0032] 20g charcoal particles, 10g SnCl 4 ·5H 2 O. Add 70g of diatomaceous earth to 250g of deionized water, stir for 2 hours, add concentrated ammonia water dropwise to adjust the pH to 6, add 10% binder to extrude and dry to obtain the precursor after suction filtration and drying. Soak the precursor in 2mol / L H 2 SO 4 The solution was dried after 12h, and the product was in N 2 Calcined at 450°C for 6h under protection to obtain the final solid acid catalyst. Take by weighing dodecanedioic acid 16g, methyl alcohol 27g, add a certain proportion catalyst, react certain hour on reflux reactor, its reaction result is as follows through gas chromatography detection after suction filtration:

[0033] (catalyst / acid) / % Reaction temperature / ℃ Conversion rates / % Selective / % 2 60 73 91 4 80 83 88 10 100 83 84

Embodiment 3

[0035] 20g charcoal particles, 10g SnCl 4 ·5H 2 O. Add 70g of diatomaceous earth to 250g of deionized water, stir for 2 hours, add concentrated ammonia water dropwise to adjust the pH to 6, add 10% binder to extrude and dry to obtain the precursor after suction filtration and drying. Soak the precursor in 3mol / L H 2 SO 4 The solution was dried after 12h, and the product was in N 2 Calcined at 450°C for 6h under protection to obtain the final solid acid catalyst. Take by weighing dodecanedioic acid 16g, methyl alcohol 27g, add a certain proportion catalyst, react certain hour on reflux reactor, its reaction result is as follows through gas chromatography detection after suction filtration:

[0036] (catalyst / acid) / % Reaction temperature / ℃ Conversion rates / % Selective / % 2 60 78 92 4 80 85 92 10 100 86 84

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PUM

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Abstract

The invention discloses a preparation method of a solid acid catalyst for preparing dimethyl dodecanedioate, and belongs to the field of catalysts. The preparation method of the catalyst comprises the following steps: weighing 20-40% by mass of charcoal particles, 10-30% by mass of SnCl4. 5H2O and 30-70% by mass of diatomite, adding the charcoal particles, the SnCl4. 5H2O and the diatomite into a certain amount of deionized water, neutralizing, stirring and extruding to obtain a precursor; and soaking the precursor in a 1-5 mol / L H2SO4 solution, drying, and calcining at 400-650 DEG C under the protection of N2 to obtain the solid acid catalyst. The catalyst has high conversion rate and selectivity when applied to preparation of dimethyl dodecanedioate, and can be reused.

Description

technical field [0001] The invention relates to a preparation method of a solid acid catalyst for preparing dimethyl dodecanedioate, belonging to the technical field of catalysts. Background technique [0002] As an important fine chemical product, dimethyl dodecanedioate is widely used in medicine, plastics, polyurethane and coating industries. [0003] The current synthesis methods mainly include biological fermentation and cyclohexanone oxidation. [0004] The fermentation method has the problems of long process time and many impurities and cannot be popularized in the fields of spices and medicine. [0005] The cyclohexanone oxidation method has the problems of high cost and low yield due to the consumption of a large amount of hydrogen peroxide as an oxidizing agent. [0006] CN1670010A discloses a method for preparing dimethyl dodecanedioate by oxidation of cyclohexanone. The method adopts methanol as a solvent, cyclohexanone as a raw material, and through phase tran...

Claims

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Application Information

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IPC IPC(8): B01J23/14C07C67/08C07C69/34
CPCY02P20/584
Inventor 魏开轩黄冬逯贵广曾志强
Owner SINOPEC NANJING RES INST OF CHEM IND CO LTD
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