Nano-size layered double hydroxide and step-by-step precipitation preparation method thereof

A layered composite and hydroxide technology, applied in chemical instruments and methods, nickel compounds, titanium compounds, etc., can solve problems such as application performance limitations

Inactive Publication Date: 2013-06-19
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Since the thickness of the LDH sheet prepared by these methods is usually greater than 20nm and the length is greater than 150nm, its BET specific surface area is usually less than 120m 2 / g, which greatly limits the application performance

Method used

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  • Nano-size layered double hydroxide and step-by-step precipitation preparation method thereof
  • Nano-size layered double hydroxide and step-by-step precipitation preparation method thereof
  • Nano-size layered double hydroxide and step-by-step precipitation preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Step A: take by weighing 18.75g Al(NO 3 ) 3 .9H 2 O was added to 100.25 g of deionized water to make a solution with a concentration of about 0.5 mol / L.

[0030] Step B: take by weighing 6gNaOH and join in 75g deionized water and be mixed with alkali solution, this alkali solution is mixed with the Al(NO 3 ) 3 The solution was mixed to form aluminum hydroxide precipitate, and then left to age for 10 minutes.

[0031] Step C: take by weighing 1.92g Mg(NO 3 ) 2 .6H 2 O is added in the aluminum hydroxide precipitation slurry that 10g step B prepares, mix well, make Mg(NO 3 ) 2 .6H 2 O is completely dissolved.

[0032] Step D: Weigh 2.4g urea and 0.54g Na 2 CO 3 Add to 40ml of deionized water to prepare an alkaline solution.

[0033] Step E: Add the alkali solution prepared in step D directly to the mixture prepared in step C under stirring at 80°C, and then continue to stir and react at 100°C for 24 hours. After the reaction, cool the slurry to room temperatur...

Embodiment 2

[0035] Steps A and B are the same as in Example 1.

[0036] Step C: take by weighing 2.56g Mg(NO 3 ) 2 .6H 2 O is added in the aluminum hydroxide precipitation slurry that 10g step B prepares, mix well, make Mg(NO 3 ) 2 .6H 2 O is completely dissolved.

[0037] Step D: Weigh 3.3g urea and 0.54g Na 2 CO 3 Add to 40ml of deionized water to prepare an alkaline solution.

[0038] Step E: Add the alkali solution prepared in step D directly to the mixture prepared in step C at 90°C with stirring, then continue to stir and react at 100°C for 20 hours, cool the slurry to room temperature after the reaction, and remove the precipitate Wash by centrifugation until the pH value is less than 8, and dry the sample in an oven at 100°C for 12 hours to obtain the LDH product. Elemental analysis shows that the chemical composition formula of the product is: Mg 0.8 Al 0.2 (OH) 2 (CO 3 ) 0.1 0.63H 2 O, BET analysis shows that its specific surface area is 177m 2 / g.

Embodiment 3

[0040] Steps A and B are the same as in Example 1.

[0041] Step C: take by weighing 0.641g Mg(NO 3 ) 2 .6H 2 O and 0.727g Ni(NO 3 ) 2 .6H 2 O is added in the aluminum hydroxide precipitation slurry that 10g step B prepares, mix well, make Mg(NO 3 ) 2 .6H 2 O and Ni(NO 3 ) 2 .6H 2 O is completely dissolved.

[0042] Step D: Weigh 1.6g urea and 0.2g Na 2 CO 3 Add to 40ml of deionized water to prepare an alkaline solution.

[0043] Step E: Add the alkali solution prepared in step D directly to the mixture prepared in step C at 95°C with stirring, then continue to stir and react at 100°C for 10 hours, cool the slurry to room temperature after the reaction, and remove the precipitate Wash by centrifugation until the pH value is less than 8, and dry the sample in an oven at 100°C for 12 hours to obtain the LDH product. Elemental analysis shows that the chemical composition formula of the product is: Mg 0.33 Ni 0.33 Al 0.33 (OH) 2 (CO 3 ) 0.165 0.63H 2 O, BET a...

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Abstract

The invention provides a nano-size layered double hydroxide and a step-by-step precipitation preparation method thereof. The preparation method comprises the following steps: based on a soluble salt of a metal and an alkali as raw materials, respectively precipitating metal ions constituting an LDH (layered double hydroxide) layer plate through step-by-step precipitation reaction and generating the LDH during the second-step precipitation process. As the activity of the hydroxide prepared by the first-step precipitation reaction is high, the LDH can fast nucleate and grow during the second-step precipitation, an obtained LDH sheet is thinner, the thickness of the layer plate is 5-15nm, the length of the layer plate is 50-150nm, and the specific surface area of a BET (Brunauer-Emmett-Teller) is 140-280m<2> / g, which is much larger than the specific surface area of the common LDH. By adopting the method, the shortcoming of small specific surface area during the preparation of the LDH through a co-precipitation method can be overcome. The preparation method adopted by the invention is simple and convenient, high temperature and high pressure are not required, special equipment is not required, sources of the raw materials are rich, and the cost is low. The layered double hydroxide can be widely applied to the fields of adsorption separation, catalysis, high polymer materials and the like.

Description

[0001] Field [0002] The invention relates to the field of inorganic non-metallic functional materials and their preparation, in particular to a nano-layered composite hydroxide and a preparation method thereof. Background technique [0003] Layered double hydroxides (LDH for short) is a kind of anionic layered clay, its chemical formula is [M 2+ 1-x m 3+ x (OH) 2 ] x+ (A n- x / n ).mH 2 O, where M 2+ , M 3+ Represent divalent and trivalent metal cations respectively, x represents the change of the content of metal elements, A n- Represents interlayer anions. LDHs have attracted extensive attention in recent years due to their unique two-dimensional layered structure and the exchangeability of interlayer anions. The unique properties of LDH make it widely used in the fields of catalysis, adsorption, ion exchange and polymer additives (flame retardants, thermal stabilizers and other functional additives). [0004] The specific surface area of ​​a material has an imp...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F7/00C01G53/00C01G23/00C01G9/00B82Y30/00C01F7/785
CPCC01F7/785
Inventor 李殿卿唐平贵冯拥军冯俊婷
Owner BEIJING UNIV OF CHEM TECH
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