Inorganic microporous nickle and cobalt phosphate molecular sieves materials and their synthesis method

A nickel-cobalt phosphate, molecular sieve-like technology, used in molecular sieve catalysts, molecular sieves and alkali-exchanged phosphates, chemical instruments and methods, etc., can solve the problems of high crystallization temperature, unfavorable industrial production, long crystallization time, etc. Synthesis conditions, the effect of shortening the synthesis time

Inactive Publication Date: 2007-03-14
SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The VSB-1 reported in the literature is hydrothermally synthesized by crystallization at 180°C for 144 hours. During the preparation process, the crystallization temperature is high and the crystallization time is long, which is not conducive to the realization of industrial production.
So far, there is no report on the doping of VSB-1 transition metal element system and related research

Method used

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  • Inorganic microporous nickle and cobalt phosphate molecular sieves materials and their synthesis method
  • Inorganic microporous nickle and cobalt phosphate molecular sieves materials and their synthesis method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Example 1Co mole fraction is 31% CoVSB-1

[0024] Dissolve 3.23g of nickel chloride and 1.38g of cobalt chloride in 14mL of distilled water, and add 2.24mL of orthophosphoric acid dropwise while stirring; then, add 0.97mL of hydrofluoric acid; finally add 1.18mL of ethylenediamine template, and stir for 0.5 After mixing evenly for 1 hour, the mixed material was moved into a polytetrafluoroethylene-lined stainless steel synthesis kettle and sealed, and the filling capacity was 70% (V). Crystallize at 170°C for 2 hours under autogenous pressure, wash the solid product three times with deionized water, and dry it in air at 60°C to obtain CoVSB-1. The XRD analysis is shown in Figure 2. Its unit cell parameters are: a=b=19.935(3) Ȧ; c=5.0476(1) Ȧ; V=1737.28 Ȧ 3 . The unit cell parameters of VSB-1 reported in the literature a=b=19.834(1) Ȧ; c=5.0379(1) Ȧ; V=1716.33 Ȧ 3 Compared with that, it has increased, indicating that cobalt atoms have entered the framework. The main ...

Embodiment 2

[0025] Embodiment 2Co mole fraction is 52% CoVSB-1

[0026] In Example 1, (3.23g NiCl 2 ·6H 2 O+1.38g CoCl 2 ·6H 2 O) was changed to (2.31g NiCl 2 ·6H 2 O+2.30g CoCl 2 ·6H 2 O), the rest of the synthesis conditions and synthesis steps are unchanged, the unit cell parameters of the CoVSB-1 product obtained are: a=b=19.960 (2) Ȧ; c=5.053 (1) Ȧ; V=1743.49 Ȧ 3 . The main component content of this product is: Co (22.06wt%), Ni (20.34wt%), P (14.32wt%), calculate its cobalt mole fraction [n Co / (n Co +n Ni )] at 52%.

Embodiment 3

[0027] Embodiment 3 Co mole fraction is 52% CoVSB-1

[0028] In Example 2, the components of the reaction mixture and other synthesis steps are kept unchanged, the crystallization temperature is changed to 150° C., and the crystallization time is changed to 4 hours, and the product of Example 2 can also be prepared.

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Abstract

An inorganic millipore nickel cabolt phosphate molecular sieve is prepared through proportionally mixing the inorganic or organic metal salts of Ni and Co, ethyldiamine, ammonia water, phosphoric acid and hydrofluorie acid, crystallizing, separation, washing and drying.

Description

technical field [0001] The invention provides an inorganic microporous nickel-cobalt phosphate molecular sieve material and a synthesis method thereof, belonging to the field of molecular sieve materials. Background technique [0002] The acidic characteristics and redox catalytic properties of molecular sieves such as aluminum phosphate can be changed by introducing other metal ions into the framework for isomorphic substitution. In 1986, US Patent No. 4,567,029 reported the synthesis of metal phosphate MeAPO / MeAPSO for the first time, and since then this field has attracted extensive research interest. Chinese patents 99127147.5, 99127145.9, and 99127144.0 respectively provide metalloaluminophosphate molecular sieves or metallosilicoaluminophosphate molecular sieves with different structures and their synthesis methods. [0003] VSB-1 is an inorganic microporous nickel phosphate molecular sieve functional material, which has properties such as ion exchange, adsorption, ca...

Claims

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Application Information

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IPC IPC(8): C01B39/54B01J29/82
Inventor 高秋明解丽丽
Owner SHANGHAI INST OF CERAMIC CHEM & TECH CHINESE ACAD OF SCI
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