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Three-dimensional flower-like layered double hydroxide and preparation method thereof

A layered compound and hydroxide technology, applied in the direction of aluminum oxide/aluminum hydroxide, zinc oxide/zinc hydroxide, nickel oxide/nickel hydroxide, etc., can solve the inconvenience of industrial production, high production cost, environmental hazards, etc. problem, achieve the effect of low cost and simple preparation method

Inactive Publication Date: 2014-11-05
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Since these methods usually require the use of organic solvents or surfactants, they are potentially harmful to the environment, and the production cost is high, which is not convenient for industrial production.

Method used

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  • Three-dimensional flower-like layered double hydroxide and preparation method thereof
  • Three-dimensional flower-like layered double hydroxide and preparation method thereof
  • Three-dimensional flower-like layered double hydroxide and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Step A: Weigh 10g of aluminum sulfate and add it to 190g of deionized water to prepare an aluminum sulfate solution, weigh 36g of urea, add it to the aluminum sulfate solution and mix well. Under vigorous stirring, adjust the pH value of the aluminum solution to 3.85 with a mass fraction of 2.5% ammonia solution, and then place the aluminum solution in a water bath at 98°C for a heating reaction for 30 minutes, so that the aluminum ions in the aluminum solution rapidly form an amorphous form. Aluminum hydroxide is precipitated, and the precipitate is centrifuged and washed to prepare an aluminum hydroxide slurry with a mass fraction of 5%.

[0026] Step B: Weigh 1.2g MgSO 4 Add it into 20 g of deionized water to prepare a solution, then add it into 7.8 g of the above-mentioned aluminum hydroxide slurry, and mix well.

[0027] Step C: Weigh 6g of urea and 0.08g of NaOH and add it to 80g of deionized water to prepare an alkali solution. Add the alkali solution directly t...

Embodiment 2

[0029] Step A is the same as in Example 1.

[0030] Step B: take by weighing 3.84g Mg(NO 3 ) 2 ·6H 2 O was added to 20 g of deionized water to prepare a solution, then added to 7.8 g of aluminum hydroxide slurry, and mixed evenly.

[0031] Step C: Weigh 6g urea and 0.53g Na 2 CO 3 Add it into 80g of deionized water to prepare an alkaline solution, and directly add the alkaline solution to the slurry prepared in step B at 95°C under stirring, then continue the reaction at 98°C for 9 hours, and cool the slurry to room temperature after the reaction. The precipitate was washed by centrifugation until the pH value was less than 8, and the sample was dried in an oven at 100°C for 12 hours to obtain a three-dimensional flower-like LDH product. Elemental analysis shows that the chemical composition formula of the product is: Mg 0.75 Al 0.25 (OH) 2 (CO 3 ) 0.125 0.65H 2 O, BET analysis shows that its specific surface area is 183m 2 / g.

Embodiment 3

[0033] Step A is the same as in Example 1.

[0034] Step B: take by weighing 5.12g Mg(NO 3 ) 2 ·6H 2 O was added to 20 g of deionized water to prepare a solution, then added to 7.8 g of aluminum hydroxide slurry, and mixed evenly.

[0035] Step C: Weigh 7.2g urea and 0.53g Na 2 CO 3 Add it into 80g of deionized water to prepare an alkali solution, and directly add the alkali solution to the slurry prepared in step B at 95°C under stirring, then continue the reaction at 98°C for 12 hours, and cool the slurry to room temperature after the reaction. The precipitate was washed by centrifugation until the pH value was less than 8, and the sample was dried in an oven at 100°C for 12 hours to obtain a three-dimensional flower-like 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 0.71H 2 O, BET analysis shows that its specific surface area is 175m 2 / g.

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Abstract

The invention provides a three-dimensional flower-like layered double hydroxide and a preparation method thereof. In the preparation of the three-dimensional flower-like layered double hydroxide, aluminum sulfate or aluminum ammonium sulfate, soluble divalent metal salt and alkali are used as raw materials; the characteristic that sphere-like micron-sized aluminium hydroxide particles can be rapidly formed by solution of aluminum sulfate and aluminum ammonium sulfate, of which the pH value is 3.7 to 4, under a temperature of 95 to 100 DEG C is utilized; after being prepared, the micron-sized particles react with the divalent metal salt and the alkali, so that a great amount of LDH (Layered Double Hydroxide) crystal nuclei can be rapidly formed on the surface of aluminium hydroxide; and finally, three-dimensional flower-like structure LDH are formed. A prepared LDH laminate has a thickness of about 10 to 20nm; and the BET (Brunauer-Emmett-Teller) specific surface area of the prepared LDH laminate is greater than 140 m<2> / g and is much greater than that of common LDH. The preparation method disclosed by the invention is simple, is simple and convenient to operate, does not require high temperature and high pressure, does not need to use an organic solvent and a surfactant and is low in cost. The three-dimensional flower-like layered double hydroxide can be widely applied to the fields of adsorption separation, catalysis, high polymer materials and the like.

Description

technical field [0001] The invention relates to the field of inorganic non-metallic functional materials and preparation thereof, in particular to a three-dimensional flower-like layered composite hydroxide and a preparation method thereof. Background technique [0002] 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 material additives (flame retardants, thermal stabilizers and other functional additives). [0003] The size, mor...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01F7/02C01G53/04C01G9/02
Inventor 李殿卿唐平贵冯拥军冯俊婷钱磊磊
Owner BEIJING UNIV OF CHEM TECH
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