Method for preparing nitrate intercalation cobalt and aluminum type hydrotalcite in one step through coprecipitation

A nitrate intercalation and hydrotalcite technology, applied in chemical instruments and methods, cobalt compounds, inorganic chemistry, etc., can solve the problem that nitrate intercalation cobalt-aluminum hydrotalcite cannot be prepared in one step, and achieve the effect of simple and rapid preparation

Active Publication Date: 2018-01-09
TAIYUAN UNIV OF TECH
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  • Summary
  • 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 cobalt-aluminum hydrotalcites in one step, the present invention provides a method for preparing nitrate-intercalated cobalt-aluminum hydrotalcites in one step by applying co-precipitation; the specific principle is to use acetic acid-sodium acetate buffer The buffering effect of the solution stabilizes the pH value of the preparation system at 4.00-5.00, effectively avoiding CO in the environment 2 Efficient one-step preparation of CoAl-NO based on the effect of dissolution on the prepared product 3 -LDH

Method used

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  • Method for preparing nitrate intercalation cobalt and aluminum type hydrotalcite in one step through coprecipitation
  • Method for preparing nitrate intercalation cobalt and aluminum type hydrotalcite in one step through coprecipitation

Examples

Experimental program
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Effect test

Embodiment 1

[0035] (1) Use a pipette to pipette 26.50±0.01 mL 0.2 mol·L -1 To 100 mL volumetric flask, and then add 73.50±0.01 mL 0.2 mol·L -1 Acetic acid solution, vortex to mix evenly, make 100 mL of acetic acid-sodium acetate buffer solution with pH=4.20±0.01 in constant volume.

[0036] (2) Weigh 31.43±0.01 g of cobalt nitrate hexahydrate and 20.26±0.01 g of aluminum nitrate nonahydrate, mix them into a beaker, add 90±1 mL of deionized water to the beaker, and stir with a magnetic stirrer for 10 min. Is completely dissolved, the prepared solution (c(Co 2+ )=1.20 mol·L -1 , C(Al 3+ )=0.60 mol·L -1 ) Transfer to a 250 mL bottle infusion set for later use.

[0037] (3) Weigh 4.00±0.01 g of sodium hydroxide into a beaker, add a small amount of deionized water to the beaker, and stir with a magnetic stirrer for 10 minutes to completely dissolve it. Transfer the dissolved solution to a 100 mL volumetric flask to make 1.00mol·L -1 Sodium hydroxide aqueous solution, then transfer it to a 250 mL bo...

Embodiment 2

[0042] (1) Use a pipette to pipette 59.00±0.01 mL 0.2 mol·L -1 To 100 mL volumetric flask, then add 41.00±0.01 mL 0.2 mol·L -1 Acetic acid solution, vortex to mix evenly, make 100 mL pH=4.80±0.01 acetic acid-sodium acetate buffer solution.

[0043] (2) Weigh 43.65±0.01 g of cobalt nitrate hexahydrate and 18.76±0.01 g of aluminum nitrate nonahydrate, mix them into a beaker, add 100±1 mL of deionized water to the beaker, and stir with a magnetic stirrer for 10 min. Is completely dissolved, the prepared solution (c(Co 2+ )=1.50 mol·L -1 , C(Al 3+ )=0.50 mol·L -1 ) Transfer to a 250 mL bottle infusion set for later use.

[0044] (3) Weigh 4.00±0.01 g of sodium hydroxide into a beaker, add a small amount of deionized water to the beaker, and stir with a magnetic stirrer for 10 minutes to completely dissolve it. Transfer the dissolved solution to a 100 mL volumetric flask to make 1.00mol·L -1 Sodium hydroxide aqueous solution, then transfer it to a 250 mL bottle infusion set for later u...

Embodiment 3

[0049] (1) Pipette 18.00±0.01 mL 0.2 mol·L with a pipette -1 To 100 mL volumetric flask, and then add 82.00±0.01 mL 0.2 mol·L -1 Acetic acid solution, vortex to mix evenly, make 100 mL pH=4.00±0.01 acetic acid-sodium acetate buffer solution.

[0050] (2) Weigh 27.94±0.01 g cobalt nitrate hexahydrate and 9.00±0.01 g aluminum nitrate nonahydrate, mix them into a beaker, add 120±5 mL deionized water to the beaker, and stir with a magnetic stirrer for 10 min. Is completely dissolved, the prepared solution (c(Co 2+ )=0.80 mol·L -1 , C(Al 3+ )=0.20 mol·L -1 ) Transfer to a 250 mL bottle infusion set for later use.

[0051] (3) Weigh 4.00±0.01 g of sodium hydroxide into a beaker, add a small amount of deionized water to the beaker, and stir with a magnetic stirrer for 10 minutes to completely dissolve it. Transfer the dissolved solution to a 100 mL volumetric flask to make 1.00mol·L -1 Sodium hydroxide aqueous solution, then transfer it to a 250 mL bottle infusion set for later use.

[00...

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Abstract

The invention discloses a method for preparing nitrate intercalation cobalt and aluminum type hydrotalcite in one step through coprecipitation. An acetic acid-sodium acetate buffer solution is used; the pH value of a preparation system is stably controlled at 4.00 to 5.00; cobalt-nitrate hexahydrate and aluminum nitrate nonahydrate are used as raw materials; sodium hydroxide is used as a precipitator; deionized water is used as a solvent and a washing agent; the nitrate intercalation cobalt and aluminum type hydrotalcite is prepared through the steps of solution preparation, titration co-precipitation, hydro-thermal treatment, washing, suction filtration and drying. The preparation method has the advantages that the influence of CO3<2-> ion formation due to dissolution of CO2 in the environment can be effectively avoided; the method belongs to a fast preparation method of the pure phase nitrate intercalation cobalt and aluminum type hydrotalcite.

Description

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

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G51/00
Inventor 朱琳张鹏秦瑜吴旭杜星宇王璐
Owner TAIYUAN UNIV OF TECH
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