ZnO/SBA-15 composite nano-catalyst, preparation method and application thereof

A nano-catalyst and catalyst technology, applied in physical/chemical process catalysts, molecular sieve catalysts, metal/metal oxide/metal hydroxide catalysts, etc., can solve the problems of corrosion reaction equipment, long reaction time, consumption of tertiary amines, etc. To achieve the effect of simple post-processing, low preparation cost and good selectivity

Inactive Publication Date: 2008-09-24
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In the process of preparing aromatic isocyanate by the decomposition of aromatic amino acid ester, Sydor (U.S.Pat.3,734,941) proposes that 2,4-toluene-ethyl carbamate is decomposed in the presence of ferric chloride, and the shortcoming of this reaction is that the yield is low , the formation of a large number of polymerization by-products, the catalyst is easy to decompose, and the reaction equipment is corroded
Alper etc. (U.S.Pat.5,457,229) propose to add halogenated catechol borane to receive the alcohol that generates, improve the yield of diphenylmethane diisocyanate, the shortcoming ...

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Take about 0.5g of SBA-15 and disperse it into 30mL ethanol-water mixed solution with a volume ratio of 3 / 2, and raise the temperature to 120°C while stirring. Subsequently, 16 mL each of 0.04 mol / L zinc nitrate solution and 0.8 mol / L triethylamine solution were added simultaneously. Aged at 120°C for 3h, centrifuged the obtained precipitate, washed with deionized water until neutral, dried at 110°C and calcined at 600°C for 4h to obtain ZnO / SBA-15 (mass percentage composition: ZnO , 8.5%; SBA-15, 91.5%) composite nanocatalysts. The performance indicators are shown in Table 1.

[0026] Add 0.5g of methyl phenylcarbamate and 40mL of nitrobenzene into the Erlenmeyer flask and dissolve under stirring, and pour the dissolved solution into a constant pressure dropping funnel. Add 0.030g of ZnO / SBA-15 and 150mL of paraffin oil into the flask, control the temperature of the paraffin oil at 260°C, and maintain the vacuum of the reaction system at 0.02MPa. Place the constant ...

Embodiment 2

[0028] Take about 0.6g of SBA-15 and disperse it into 40mL ethanol-water mixed solution with a volume ratio of 2 / 3, and raise the temperature to 70°C while stirring. Subsequently, 8 mL each of 0.06 mol / L zinc sulfate solution and 2.4 mol / L triethanolamine solution were added simultaneously. After aging at 70°C for 6h, the obtained particles were centrifuged, washed with deionized water, dried and calcined at 550°C for 8h. A ZnO / SBA-15 (mass percentage composition: ZnO, 6.1%; SBA-15, 93.9%) composite nanocatalyst is obtained. The performance indicators are shown in Table 1.

[0029] Add 1 g of methyl naphthalene carbamate and 80 mL of dimethyl phthalate into an Erlenmeyer flask, dissolve under magnetic stirring, and pour the dissolved solution into a constant pressure dropping funnel. Add 0.05g ZnO / SBA-15 and 110mL dioctyl phthalate to the flask, control the temperature of dioctyl phthalate to 270°C, and maintain the vacuum of the reaction system at 0.03MPa. Place the consta...

Embodiment 3

[0031] Disperse about 1.0 g of SBA-15 into 60 mL of ethanol-water mixed solution with a volume ratio of 1 / 1, and raise the temperature to 90°C while stirring. Subsequently, 20 mL each of 0.10 mol / L zinc acetate solution and 3.2 mol / L hexamethylenediamine solution were added simultaneously. Aging at 90°C for 1h, centrifugation of the obtained particles, washing with deionized water, drying and roasting at 700°C for 1h to obtain ZnO / SBA-15 (mass percentage composition: ZnO, 12.5%; SBA-15 , 87.5%) composite nanocatalysts. The performance indicators are shown in Table 1.

[0032] Add 0.2g of methyl 4,4'-diphenylmethanedicarbamate and 15mL of dibutyl phthalate into the Erlenmeyer flask, heat to 100°C under magnetic stirring to dissolve, and pour the dissolved solution into constant pressure drops liquid funnel. Add 0.05 g of ZnO / SBA-15 and 80 mL of di-isooctyl phthalate to the flask, control the temperature of di-iso-octyl phthalate to 275° C., and maintain the vacuum of the rea...

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PUM

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Abstract

The invention relates to a nano composite catalyst ZnO/SBA-15, which has the mass percentage of compositions as follows: ZnO ranges from 5 to 15 percent; SBA-15 ranges from 85 to 95 percent. SBA-15 ethanol-water suspension is mixed from an ethanol aqueous solution and SBA-15; the SBA-15 ethanol-water suspension, being stirred at the temperature ranging from 60 DEG C to 120 DEG C, is added with the zinc salt-absolute ethanol solution with a concentration of 0.001 to 0.20 mol/L and equivoluminal ethanol solution organic amines with a concentration of 0.01to 1.6 mol/L; then the mixed solution is aged for 1 to 5 hour(s), and then is let stand and filtrated; the sediments are washed by deionized water to be neutral; and the ZnO/SBA-15 catalyst is made by drying and roasting the sediments. The nano composite catalyst has the advantages of simple process, homogeneous distribution of particles, good dispersion, high conversion rate of aromatic isocyanate, good selectivity, etc.

Description

technical field [0001] The invention belongs to a ZnO / SBA-15 composite nano-catalyst and its preparation method and application, in particular to a catalyst for directly synthesizing nano-ZnO on the surface of molecular sieve SBA-15 and its preparation method and aromatic carbamate decomposition to produce aromatic Applications in isocyanate reactions. Background technique [0002] Nano-ZnO has excellent optical, electrical, chemical and biological properties and is widely used in chemical, electronic, biopharmaceutical and coatings, sensors, dielectric materials, inks, chemical fibers, rubber and other production and research fields. In the chemical industry, ZnO is widely used as a catalyst and desulfurizer, and the high surface activity of nano-ZnO can improve the selectivity and catalytic efficiency of the catalyst. In recent years, nano-ZnO particles have become a research hotspot. The main methods for preparing ZnO nanostructures include carbothermal reduction, vapor ...

Claims

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Application Information

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IPC IPC(8): B01J29/70B01J23/06C07C263/04C07C265/12
Inventor 王建国郭星翠秦张峰王国富
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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