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Method using co-precipitation to prepare nitrate intercalation nickel-aluminum layered double hydroxides in one step

A technology of nitrate intercalation and hydrotalcite, which is applied in the fields of chemical instruments and methods, nickel compounds, inorganic chemistry, etc., can solve the problem of not being able to prepare nitrate intercalation nickel-aluminum hydrotalcite in one step, and achieve the effect of simple and rapid preparation

Active Publication Date: 2018-02-02
TAIYUAN UNIV OF TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] Aiming at the problem that the traditional co-precipitation method cannot prepare nitrate-intercalated nickel-aluminum hydrotalcites in one step, the present invention provides a method for preparing nitrate-intercalated nickel-aluminum hydrotalcites in one step by applying co-precipitation; the specific principle is to use acetic acid-sodium acetate buffer solution The buffering effect of the preparation system stabilizes the pH of the preparation system at 4.00-5.00, effectively avoiding CO in the environment 2 Efficient one-step preparation of NiAl-NO based on the effect of dissolution on the prepared product 3 -LDH

Method used

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  • Method using co-precipitation to prepare nitrate intercalation nickel-aluminum layered double hydroxides in one step
  • Method using co-precipitation to prepare nitrate intercalation nickel-aluminum layered double hydroxides in one step

Examples

Experimental program
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Effect test

Embodiment 1

[0035] (1) Use a pipette to pipette 18.00±0.01 mL of 0.2 mol L -1 sodium acetate solution into a 100 mL volumetric flask, and then add 82.00±0.01 mL 0.2 mol L -1 acetic acid solution, shake it to make it evenly mixed, and make it into 100 mL pH=4.00±0.01 acetic acid-sodium acetate buffer solution.

[0036] (2) Weigh 31.41 ± 0.01 g of nickel nitrate hexahydrate and 20.26 ± 0.01 g of aluminum nitrate nonahydrate, mix them into a beaker, add 90 ± 1 mL of deionized water into the beaker, and stir with a magnetic stirrer for 10 min. It is completely dissolved, the prepared solution (c(Ni 2+ )=1.20 mol L-1 , c(Al 3+ )=0.60 mol L -1 ) into a 250 mL hanging bottle infusion set for use.

[0037] (3) Weigh 4.00±0.01 g of sodium hydroxide into a beaker, add a small amount of deionized water into the beaker, and stir with a magnetic stirrer for 10 min to completely dissolve it. Transfer the dissolved solution to a 100 mL volumetric flask to make 1.00mol L -1 sodium hydroxide aqueous...

Embodiment 2

[0042] (1) Pipette 49.00±0.01 mL 0.2 mol L -1 sodium acetate solution into a 100 mL volumetric flask, and then add 51.00±0.01 mL 0.2mol L -1 acetic acid solution, shake it to make it evenly mixed, and make it into 100 mL pH=4.60±0.01 acetic acid-sodium acetate buffer solution.

[0043] (2) Weigh 43.62±0.01 g of nickel nitrate hexahydrate and 18.76±0.01 g of aluminum nitrate nonahydrate, mix them into a beaker, add 100±1 mL of deionized water into the beaker, and stir for 10 min with a magnetic stirrer It is completely dissolved, the prepared solution (c(Ni 2+ )=1.50 mol L -1 , c(Al 3+ )=0.50 mol L -1 ) into a 250 mL hanging bottle infusion set for use.

[0044] (3) Weigh 4.00±0.01 g of sodium hydroxide into a beaker, add a small amount of deionized water into the beaker, and stir with a magnetic stirrer for 10 min to completely dissolve it. Transfer the dissolved solution to a 100 mL volumetric flask to make 1.00mol L -1 sodium hydroxide aqueous solution, and then trans...

Embodiment 3

[0049] (1) Use a pipette to pipette 70.00±0.01 mL of 0.2 mol L -1 sodium acetate solution into a 100 mL volumetric flask, and then add 30.00±0.01 mL 0.2 mol L -1 acetic acid solution, shake it to make it evenly mixed, and make it into 100 mL pH=5.00±0.01 acetic acid-sodium acetate buffer solution.

[0050] (2) Weigh 34.89±0.01 g of nickel nitrate hexahydrate and 11.25±0.01 g of aluminum nitrate nonahydrate, mix them into a beaker, add 120±5 mL of deionized water into the beaker, and stir it with a magnetic stirrer for 10 min. It is completely dissolved, the prepared solution (c(Ni 2+ )=1.00 mol L -1 , c(Al 3+ )=0.25 mol L -1 ) into a 250 mL hanging bottle infusion set for use.

[0051] (3) Weigh 4.00±0.01 g of sodium hydroxide into a beaker, add a small amount of deionized water into the beaker, and stir with a magnetic stirrer for 10 min to completely dissolve it. Transfer the dissolved solution to a 100 mL volumetric flask to make 1.00mol L -1 sodium hydroxide aqueous...

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Abstract

The invention discloses a method using co-precipitation to prepare nitrate intercalation nickel-aluminum layered double hydroxides in one step. The method is characterized in that an acetic acid-sodium acetate buffer solution is used to stably control the pH of a preparation system to be at 4.00-5.00, nickel nitrate hexahydrate and aluminum nitrate nonahydrate are used as the raw materials, sodiumhydroxide is used as the precipitator, deionized water is used as the solvent and the washing agent, and solution preparation, titration co-precipitation, hydrothermal processing, washing, suction filtration and drying are performed to prepare the nitrate intercalation nickel-aluminum layered double hydroxides. The method has the advantages that influence caused by the fact that CO2 in an environment is dissolved to form CO3<2-> ions can be avoided effectively, and the method is a fast preparation method of the pure-phase nitrate intercalation nickel-aluminum layered double hydroxides.

Description

technical field [0001] The invention belongs to the field of novel inorganic layered materials, and specifically relates to a method for preparing nitrate-intercalated nickel-aluminum hydrotalcite in one step by adjusting the pH value of the system and adopting co-precipitation. Background technique [0002] Layered Double Hydroxides (LDHs for short) are layered double metal hydroxides with a layered crystal structure, composed of hydroxides of divalent and trivalent metal elements, and anions should be filled between the structural layers. Co-precipitation method is the main preparation method of LDHs, because the preparation process is usually carried out in an open system, and the CO in the environmental system 2 It is often unavoidably dissolved into the solution system and transformed into carbonate with stronger laminate binding force and preferentially enters the interlayer of the hydrotalcite-like structure. Therefore, the traditional co-precipitation method usually ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G53/00
CPCC01G53/006C01P2002/72
Inventor 吴旭刘雪贞康伟伟成强强侯本辉谢鲜梅
Owner TAIYUAN UNIV OF TECH
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