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Microwave method for synthesizing nickel phosphates cobalt microporous material

A technology of microwave synthesis and nickel-cobalt phosphate, which is applied in the field of molecular sieve materials, can solve the problems of long synthesis time, uneven heating, and uneven particle size of the product, so as to reduce the grain size, improve the catalytic performance, and improve the particle size. evenly distributed effect

Inactive Publication Date: 2008-08-27
SHANGHAI SECOND POLYTECHNIC UNIVERSITY
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The invention discloses a microwave synthesis method of a nickel-cobalt phosphate microporous material, which aims at overcoming the disadvantages of uneven heating in the traditional hydrothermal synthesis method, resulting in uneven particle size of the product, and long time required for synthesis.

Method used

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  • Microwave method for synthesizing nickel phosphates cobalt microporous material
  • Microwave method for synthesizing nickel phosphates cobalt microporous material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Example 1: Weigh 2.31g of nickel chloride and 2.30g of cobalt chloride and dissolve them in 14mL of distilled water, add 2.24mL of orthophosphoric acid dropwise while stirring; then, add 0.97mL of hydrofluoric acid; finally add 1.18mL of ethylenediamine Template agent, after stirring for 30 minutes to mix evenly, move the mixed material into a digestion tank, and synthesize under microwave irradiation conditions. The heating mode of the microwave oven adopts the temperature control mode, set the crystallization temperature to 180°C, first use 1000W power to heat for 1 minute, and the temperature is displayed as 95°C; then use 400W power to continue heating for 2 minutes, and then the temperature rises to 180°C Keep it for 27min. After the temperature of the digestion tank dropped to room temperature, the obtained solid product was centrifuged and washed 3 times with deionized water, and freeze-dried to obtain the original powder. XRD analysis see figure 1 . The main c...

Embodiment 2

[0016] Embodiment 2: In embodiment 1, the proportion of reactants remains unchanged, and the order of addition remains unchanged. After the reactants are uniformly mixed, they are transferred into a digestion tank and synthesized under microwave irradiation conditions. The heating mode of the microwave oven adopts the temperature control mode, and the crystallization temperature is set to 130°C. First, use 1000W power to heat for 1 minute, and the temperature is displayed as 75°C; then use 400W power to continue heating for 3 minutes, and the temperature rises to 130°C. Keep for 26min. After the temperature of the digestion tank dropped to room temperature, the solid product was centrifuged and washed 3 times with deionized water, and the sample of Example 1 could still be obtained after freeze-drying.

Embodiment 3

[0017] Embodiment 3: In embodiment 1, the proportion of reactants remains unchanged, and the order of addition remains unchanged. After the reactants are uniformly mixed, they are transferred into a digestion tank and synthesized under microwave irradiation conditions. The heating mode of the microwave oven adopts the temperature control mode, set the crystallization temperature to 180°C, first use 1000W power to heat for 1 minute, and the temperature is displayed as 95°C; then use 400W power to continue heating for 2 minutes, and then the temperature rises to 180°C Keep for 12min. After the temperature of the digestion tank dropped to room temperature, the solid product was centrifuged and washed 3 times with deionized water, and the sample of Example 1 could still be obtained after freeze-drying.

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Abstract

Disclosed is a microwave synthesis method of nickel phosphates cobalt cellular materials. The steps comprise preparing nickel source substance, cobalt source substance, phosphorus source substance, template, mineralizer and water according to oxide molecular ratio, initially dissolving the nickel source and the cobalt source in the water, adding with the phosphorus source when stirring, then adding with the template and the mineralizer and continuing to stir evenly, moving the reaction solution into a microwave synthesis reactor, irradiating for 3-360 minutes step by step under the temperature of 130-180 DEG C, then centrifugal separating, washing and freeze-drying, and thereby the nickel phosphates cobalt CoVSB-1 materials is obtained. The frequency of the microwave is 2450 megahertz, and the power is 400-1000 watt. A microwave is heated by employing the temperature controlling mode. Compared with the conventional hydro-thermal method, the synthesis time of the invention is shorter, the grain size distribution is more uniform, and the reducing of the size of crystal grain is in favor of the increasing of the catalytic performance of the product.

Description

technical field [0001] The invention relates to a microwave synthesis method of a nickel-cobalt phosphate microporous material, belonging to the field of molecular sieve materials. Background technique [0002] Microwave hydrothermal method has been widely used in the synthesis of various silicon aluminum and phosphorus aluminum molecular sieves (G.A.Tompsett, W.C.Conner, K.S.Yngvesson, ChemPhysChem 7:296 (2006); Chinese patent ZL 99107790.3), such as A type, Y type, L-type, Beta, ZSM-5 and other zeolites and AlPO 4 -5, SAPO-5, SAPO-34, AlPO 4 -11 and other phosphorus aluminum molecular sieves. Metal phosphate MeAPO / MeAPSO is a new type of molecular sieve formed by introducing metal ions into the framework of phosphate molecular sieve during the synthesis process. This type of molecular sieve can also be synthesized by microwave hydrothermal method, such as MgAPO-5, CoAPO-44 / CoAPSO- 44. CoAPO-5, VAPSO-44, VAPSO-5, MnAPO-5, MnAPO-44, etc. Synthesis by microwave heating, s...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/54C01B37/06
Inventor 解丽丽
Owner SHANGHAI SECOND POLYTECHNIC UNIVERSITY
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