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Novel Dawson polyacid intercalation hydrotalcite composite material and method of preparing the same

A composite material and hydrotalcite technology, applied in chemical instruments and methods, catalyst activation/preparation, physical/chemical process catalysts, etc., can solve the problems of Dawson polyacid molecules intercalated into hydrotalcite layers, etc.

Inactive Publication Date: 2011-04-13
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The purpose of the present invention is to synthesize a series of new Dawson multi-acid intercalated hydrotalcite composite materials, which solves the problem of large-volume Dawson multi-acid molecules intercalating between hydrotalcite layers

Method used

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  • Novel Dawson polyacid intercalation hydrotalcite composite material and method of preparing the same
  • Novel Dawson polyacid intercalation hydrotalcite composite material and method of preparing the same
  • Novel Dawson polyacid intercalation hydrotalcite composite material and method of preparing the same

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] a. Take 0.06mol Zn(NO 3 ) 2 ·6H 2 O, 0.03mol Al(NO 3 ) 3 9H 2 O, 0.053mol NaNO 3 Mix and dissolve in 80ml deCO 2 Dissolve 0.133mol NaOH in 50ml of deionized water 2 in deionized water, N 2 Slowly drop the lye into the mixed salt solution under protection, stir vigorously, stop the drop when the pH is 6.0, transfer the slurry to an autoclave, age at 100°C for 18h, and then centrifuge and wash to obtain Zn 2 Al-NO 3 Hydrotalcite precursor;

[0024] b. Take 2.5g Zn 2 Al-NO 3 Hydrotalcite precursor dispersed in 50ml deCO 2 dilute nitric acid to adjust the pH value to 5.5 after swelling in deionized water for 5 hours;

[0025] c. Add 3.09mol of 85% H 3 PO 4 Added to 0.76mol of Na 2 WO 4 2H 2 O solution, heated to reflux for 8h, after cooling, add 100g of NH 4 Cl, the obtained precipitate was dissolved in water to form a solution, and 100 g of NH 4 Cl, the obtained precipitate was dissolved in water again to form a solution, stood still for 5d, filtered, t...

Embodiment 2

[0028] a. Take 0.06mol Zn(NO 3 ) 2 ·6H 2 O, 0.03mol Al(NO 3 ) 3 9H 2 O, 0.053mol NaNO 3 Mix and dissolve in 80ml deCO 2 Dissolve 0.133mol NaOH in 50ml of deionized water 2 in deionized water, N 2 Slowly drop the lye into the mixed salt solution under protection, stir vigorously, stop the drop when the pH is 6.0, transfer the slurry to an autoclave, age at 100°C for 18h, and then centrifuge and wash to obtain Zn 2 Al-NO 3 Hydrotalcite precursor;

[0029] b. Take 2.5g Zn 2 Al-NO 3 Hydrotalcite precursor dispersed in 50ml deCO 2 dilute nitric acid to adjust the pH value to 4.5 after swelling in deionized water for 10 hours;

[0030] c. Add 32.8mmol of NaVO 3 Dissolve in water, add 6M HCl to it, and immediately present a yellow solution, then add 10.7mmol of Na 12 [α-P 2 W 15 o 56 ]·24H 2 After stirring for 10 minutes, 1350 mmol of KCl was added, and an orange-yellow turbid liquid appeared, which was filtered to obtain an orange-yellow solid, which was mixed wit...

Embodiment 3

[0033] a. Take 0.06mol Zn(NO 3 ) 2 ·6H 2 O, 0.03mol Al(NO 3 ) 3 9H 2 O, 0.053mol NaNO 3 Mix and dissolve in 80ml deCO 2 Dissolve 0.133mol NaOH in 50ml of deionized water 2 in deionized water, N 2 Slowly drop the lye into the mixed salt solution under protection, stir vigorously, stop the drop when the pH is 6.0, transfer the slurry to an autoclave, age at 100°C for 18h, and then centrifuge and wash to obtain Zn 2 Al-NO 3 Hydrotalcite precursor;

[0034] b. Take 2.5g Zn 2 Al-NO 3 Hydrotalcite precursor dispersed in 50ml deCO 2dilute nitric acid to adjust the pH value to 5 after swelling in deionized water for 20 hours;

[0035] c. Add 0.5M NaVO to 0.5M hydrochloric acid 3 , continue to join K 10 [α 2 -P 2 W 17 o 61 ]·20H 2 O, after complete dissolution, add KCl, filter the resulting precipitate, dissolve it in 6ml of 0.1M hydrochloric acid and recrystallize to obtain Dawson polyacid 1-K 7 P 2 VW 17 o 62 18H 2 O;

[0036] d. Take 7.43g 1-K 7 P 2 VW 1...

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Abstract

The present invention discloses a series of novel Dawson polyacid intercalation hydrotalcite composite material belonging to inorganic composite material preparation technical field and method of preparing the same. The preparation process is: first preparing hydrotalcite precursor; preparing polycaid solution; inserting the polyacid Dawson into confined space of the hydrotalcite by ion exchange reaction. The polyacid intercalation hydrotalcite composite material has functional characteristics of both anionic clay and polyanionic, and has practical significance for resolving the immobilized problem of heteropolyacid in industry catalysis process; meanwhile, the intercalation hydrotalcite composite material has micropore structure that is suitable for optional shape catalytic reaction, which is similar to the functional characteristic of molecular sieve.

Description

technical field [0001] The invention belongs to the technical field of preparation of inorganic composite materials, and in particular relates to a series of new Dawson multi-acid intercalation hydrotalcite composite materials and a preparation method thereof. Background technique [0002] Hydrotalcite-like intercalation materials (LDHs) are a new type of nano-inorganic functional materials with a layered structure. Its structure is similar to that of brucite. The general composition formula can be expressed as: [M 2+ 1-x m 3+ x (OH) 2 ] x+ (A n- ) x / n mH 2 O, where M 2+ and M 3+ Respectively, divalent and trivalent metal cations in the laminate, such as: Mg 2+ 、Ni 2+ 、Co 2+ , Zn 2+ 、Cu 2+ and Al 3+ 、Cr 3+ , Fe 3+ 、Sc 3+ etc.; A n- is an interlayer anion, such as: CO 3 2- , NO 3 - , Cl - , OH - , SO 4 2- 、PO 4 3- 、C 6 h 4 (COO) 2 2- , heteropolyanions, etc.; x is M 3+ / (M 2+ +M 3+ ) molar ratio, its value is generally between 0.1 and 0.5; ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/06B01J21/04B01J27/188B01J27/199B01J21/10B01J37/03B01J37/10B01J37/00
Inventor 宋宇飞张洁赵燊徐军华
Owner BEIJING UNIV OF CHEM TECH
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