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Nanometre complex solid superacid and preparation and application thereof

A solid super acid, nano-composite technology, applied in the preparation of carboxylate, the preparation of organic compounds, catalyst activation/preparation, etc., can solve the problems of unfavorable industrialization promotion, large specific surface area, high preparation cost, and low production cost. , Large specific surface area, good product quality effect

Inactive Publication Date: 2011-10-12
ANKANG UNIV
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AI Technical Summary

Problems solved by technology

Recently had S 2 o 8 2- / TiO 2 -Al 2 o 3 and S 2 o 8 2- / SnO 2 -SiO 2 The solid superacid of composite structure is reported, but the solid superacid of the above structure has the defects of low surface activity and high preparation cost
Applied Chemistry, 2003, 20(1): (10-14) reported a nanocomposite solid superacid-S 2 o 8 2- / CoFe 2 o 4 , although the acid catalytic activity of this product is high, the esterification rate can reach 93.6%, and the specific surface area is large, which can reach 146m 2 / g, but this product still has the defect of high preparation cost, which is still not conducive to the promotion and implementation of industrialization

Method used

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  • Nanometre complex solid superacid and preparation and application thereof
  • Nanometre complex solid superacid and preparation and application thereof
  • Nanometre complex solid superacid and preparation and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] a) press n (Fe 2+ ):n(Zn 2+ )=2.0:1 Weigh FeSO 4 ·7H 2 O and ZnSO 4 ·7H 2 O, mixed and ground into powder;

[0028] b) According to n(NaOH):n(Fe 2+ )=1.8:1 Add NaOH solution, and press n(PEG):n(Fe 2+ )=0.04:1 Add the dispersant polyethylene glycol (PEG-600), and stir at 50-70°C for 30-60 minutes;

[0029] c) Press n (NaHCO 3 ):n(Fe 2+ )=2.0:1 adding NaHCO 3 Solid, adjust pH=10, stir at 50-70°C for 10-20 minutes;

[0030] d) Aging at 20-40°C for 10 hours, suction filtering, and washing the obtained precipitate with absolute ethanol until neutral;

[0031] e) Infrared drying the precipitate at 90-100°C for 3-10 hours to obtain nano-zinc ferrite (ZnFe 2 o 4 )Precursor;

[0032] f) Naturally cool the precursor to room temperature, grind it into powder, and then impregnate it in 0.75mol / L (NH 4 ) 2 S 2 o 8 In the solution, after soaking for 10 hours, filter, and dry the obtained solid at 110°C for 6 hours;

[0033] g) Roasting at 500K for 3 hours, annealin...

Embodiment 2

[0040] a) press n (Fe 2+ ):n(Zn 2+ )=1.8:1 Weigh FeSO 4 ·7H 2 O and ZnSO 4 ·7H 2 O, mixed and ground into powder;

[0041] b) According to n(NaOH):n(Fe 2+ )=1.6:1 Add NaOH solution, and press n(PEG):n(Fe 2+ )=0.02:1 Add the dispersant polyethylene glycol (PEG-600), and stir at 50-70°C for 30-60 minutes;

[0042] c) Press n (NaHCO 3 ):n(Fe 2+ )=1.8:1 adding NaHCO 3 Solid, adjust pH=11, stir at 50-70°C for 10-20 minutes;

[0043] d) Aging at 20-40°C for 7 hours, suction filtering, and washing the obtained precipitate with absolute ethanol until neutral;

[0044] e) Infrared drying the precipitate at 90-100°C for 3-10 hours to obtain nano-zinc ferrite (ZnFe 2 o 4 )Precursor;

[0045] f) The precursor is naturally cooled to room temperature, ground into powder, and then impregnated in 1.2mol / L (NH 4 ) 2 S 2 o 8 In the solution, filter after soaking for 6 hours, and dry the obtained solid at 100°C for 8 hours;

[0046] g) Roasting at 550K for 3 hours, annealing a...

Embodiment 3

[0053] a) press n (Fe 2+ ):n(Zn 2+ )=1.5:1 Weigh FeSO 4 ·7H 2 O and ZnSO 4 ·7H 2 O, mixed and ground into powder;

[0054] b) According to n(NaOH):n(Fe 2+ )=1.5:1 NaOH solution was added, and n(PEG):n(Fe 2+ )=0.06:1 Add the dispersant polyethylene glycol (PEG-600), and stir at 50-70°C for 30-60 minutes;

[0055] c) Press n (NaHCO 3 ):n(Fe 2+ )=1.7:1 adding NaHCO 3 Solid, adjust pH=8, stir at 50-70°C for 10-20 minutes;

[0056] d) Aging at 20-40°C for 3 hours, suction filtering, and washing the obtained precipitate with absolute ethanol until neutral;

[0057] e) Infrared drying the precipitate at 90-100°C for 3-10 hours to obtain nano-zinc ferrite (ZnFe 2 o 4 )Precursor;

[0058] f) The precursor is naturally cooled to room temperature, ground into powder, and then impregnated in 0.5mol / L (NH 4 ) 2 S 2 o 8 In the solution, after soaking for 12 hours, filter, and dry the obtained solid at 90°C for 10 hours by infrared;

[0059] g) Roasting at 450K for 3 hours...

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Abstract

The invention discloses a nanometre complex solid superacid which is a composite S2O8<2-> / ZnFe2O4 composed of S2O8<2-> and ZnFe2O4. The nanometre complex solid superacid is in spinel structure, the average grain diameter of crystal grain is 20-60nm, acid strength is -11.99--14.52, specific surface area is 120-190m<2> / g, and the mass percentage of sulphur is 1.8-6.5%. The catalyst is prepared by using a coprecipitation-immersion method with simple preparation route and low cost, and the obtained catalyst has the advantages of complete crystal form, small crystal particle diameter, big specificsurface area, high catalytic activity, long service life and the like. When used for catalyzing and synthesizing benzyl acetate, the nanometre complex solid superacid S2O8<2-> / ZnFe2O4 of the invention has the esterification rate of 98.0%, and has the advantages of simple and easily-controlled operation, no three-waste pollution, good product quality and low production cost.

Description

technical field [0001] The present invention relates to a kind of solid superacid, specifically, relates to a kind of nanocomposite solid superacid-S 2 o 8 2- / ZnFe 2 o 4 Its preparation method and its application in the catalytic synthesis of benzyl acetate. Background technique [0002] Due to its advantages of no pollution, super acidity, no corrosion of equipment, and easy separation, solid superacid has become a new type of green catalyst with great potential. It is used in cracking, alkylation, esterification, acylation and photocatalysis and other industrial fields have attracted extensive attention. The existing solid superacid catalyst is mainly based on SO 4 2- As a promoter, this kind of solid acid has the defects of low surface activity, poor stability, and weak catalytic activity, which are restricted in industrial application. Existing literature (CN200710038382.7; Molecular Catalysis, 2002, 16(1): 65-68; Chemical Journal of Chinese Universities, 2000, ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/053B01J23/80B01J37/02B01J37/03B01J37/08C07C69/157C07C67/08
Inventor 金华锋黄宏升
Owner ANKANG UNIV
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