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Hydrophobic organic solid acid catalyst and preparation method thereof

An organic solid, catalyst technology, applied in organic chemistry, organic compound/hydride/coordination complex catalysts, chemical instruments and methods, etc., can solve the problem that small specific surface area affects the application of effective acid catalysts, and the yield of HMF cannot be obtained. Improve the stability of HMF, etc., to achieve the effects of easy recovery, high permeability and low density, and shortened reaction time

Inactive Publication Date: 2015-03-25
JIANGSU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] Cellulose, as the most widely distributed and abundant macromolecular polysaccharide in nature, is one of the most research-significant biomass energy sources for the production of 5-hydroxymethylfurfural (HMF), an important fine chemical raw material; the acidic catalyst provides Acid sites play a vital role in the cellulose conversion process, such as inorganic Bronsted acid, Lewis acid, organic acid, etc., but due to the advantages of easy recovery, low corrosion to equipment, and less environmental pollution, heterogeneous Catalysts show a trend of more development potential; perfluorosulfonic acid-type acidic resins provide the right direction for the synthesis of solid acids with strong thermal stability and hydrophobic network structure, but the lack of pores and small specific surface areas affect their ability to be used as effective acid catalysts. Applications
At present, the factors that restrict the yield of product HMF are mainly as follows: (1) the amount of catalyst used is large, but the yield of HMF cannot be improved
(2) The stability of HMF in the reaction system is not high, and it is easy to continue to convert into by-products

Method used

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  • Hydrophobic organic solid acid catalyst and preparation method thereof
  • Hydrophobic organic solid acid catalyst and preparation method thereof
  • Hydrophobic organic solid acid catalyst and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] (1) Preparation of organic solid hydrophobic acid catalyst

[0032] Add 1.08g of sodium p-phenylacesulfonate (SS), 0.03g of ammonium persulfate, 0.0258g of N,N-methylenebisacrylamide, and 0.028g of Span-20 into 3.256mL of deionized water to form a mixed solution as water phase, stirred for 20-30min to make it evenly mixed; take 18.45mL of paraffin as the oil phase, add the oil phase to the water phase drop by drop under constant stirring and mix to prepare a stable high internal phase emulsion system (HIPEs); stir After 10 to 20 minutes, the emulsion was kept at 60°C for 18 hours for thermally initiated polymerization; the obtained polymer was extracted with acetone to elute the surfactant and paraffin, and the product was dried at 50 to 55°C for 20 to 24 hours under vacuum to obtain a large Porous organic solid polymers;

[0033] Configure a 1.5mol / mL hydrochloric acid solution, grind 0.38g of the material obtained in the previous step into powder, and then add 50mL o...

Embodiment 2

[0050] (1) Preparation of organic solid hydrophobic acid catalyst

[0051] Add 1.2g SS, 0.04g potassium persulfate, 0.0309g N,N-methylenebisacrylamide, 0.04g Tween-85 into 4mL deionized water to form a mixed solution as the water phase, stir for 20-30min to mix Uniform; take 22.67mL paraffin as the oil phase, add the oil phase to the water phase drop by drop under constant stirring and mix to prepare stable HIPEs; after stirring for 10-20min, the emulsion is kept at 65°C for 21h for thermally initiated polymerization ; The obtained polymer is subjected to Soxhlet extraction with acetone to elute the surfactant and paraffin, and the product is dried under vacuum at 50-55°C for 20-24 hours to obtain a macroporous organic solid polymer;

[0052] Configure 1mol / mL sulfuric acid solution, then, after grinding 0.5g of the material obtained in the previous step into powder, add 50mL of 1mol / mL H 2 SO 4 solution, stirred for 22 hours, and vacuum-dried at 70-80°C to obtain a macropor...

Embodiment 3

[0061] (1) Preparation of organic solid hydrophobic acid catalyst

[0062] Add 1.32g SS, 0.05g azobisisobutylamidine hydrochloride, 0.036g N,N-methylenebisacrylamide, 0.052g fatty acid methyl ester polyoxyethylene ether to 4.744mL deionized water to form a mixed solution As the water phase, stir for 20-30 minutes to make it evenly mixed; take 26.88mL paraffin as the oil phase, and add the oil phase to the water phase drop by drop under constant stirring to prepare stable HIPEs; after stirring for 10-20 minutes, The emulsion is kept at 80°C for 24h for heat-initiated polymerization; the obtained polymer is extracted with acetone to elute the surfactant and dodecane, and the product is dried under vacuum at 55°C for 20-24h to obtain a macroporous organic solid polymer ;

[0063] Configure 2.5mol / mL nitric acid solution, then, after grinding 0.62g of the material obtained in the previous step into powder, add 50mL of 1.22mol / mL H 2 SO 4 solution, stirred for 24 hours, and vacu...

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Abstract

The invention provides a hydrophobic organic solid acid catalyst and a preparation method thereof, belonging to the field of solid catalysts. The hydrophobic organic solid acid catalyst solves the technical problems that many catalysts are used in the reaction of preparing 5-hydroxymethylfurfural (HMF) by cellulose, the yield of the HMF is not improved and the HMF can be further transformed into a by-product in the reaction. A high-internal-phase emulsion method is adopted for preparing macro-porous organic solid catalyst, and the macro-porous organic solid catalyst is subjected to acid and hydrophobic modification, and then is used as the catalyst for transforming the cellulose into HMF.

Description

technical field [0001] The invention belongs to the field of solid catalysts, in particular to an organic solid hydrophobic acid catalyst and a preparation method thereof. Background technique [0002] Cellulose, as the most widely distributed and abundant macromolecular polysaccharide in nature, is one of the most research-significant biomass energy sources for the production of 5-hydroxymethylfurfural (HMF), an important fine chemical raw material; the acidic catalyst provides Acid sites play a vital role in the cellulose conversion process, such as inorganic Bronsted acid, Lewis acid, organic acid, etc., but due to the advantages of easy recovery, low corrosion to equipment, and less environmental pollution, heterogeneous Catalysts show a trend of more development potential; perfluorosulfonic acid-type acidic resins provide the right direction for the synthesis of solid acids with strong thermal stability and hydrophobic network structure, but the lack of pores and small ...

Claims

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Application Information

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IPC IPC(8): B01J31/10C07D307/46
Inventor 张云雷潘建明高和平殷毅杰曾俊
Owner JIANGSU UNIV
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