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Method for preparing nickel catalyst supported on SiO2 microspheres and application of nickel catalyst

A technology of nickel catalyst and microspheres, which is applied in the field of catalyst preparation, can solve the problems of low utilization rate of metal Ni, increase of catalyst cost, unutilization of fine powder, etc., achieve low surface acidity, avoid increased side reactions, and reduce cost The effect of risk

Active Publication Date: 2018-04-13
WANHUA CHEM GRP CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the alloy powder needs to be sieved, and the fine powder cannot be used, resulting in an increase in the cost of the catalyst; NaOH is used during activation, which produces a large amount of lye wastewater, and the post-processing cost is high.
[0007] CN101439285A discloses a catalyst preparation method for catalytic hydrogenation of nitro compounds to prepare corresponding amino compounds. The catalyst prepared by the method has high activity and good selectivity, but needs to add solvent ethanol, and the metal nickel in the catalyst is The loading capacity is as high as 55%, the metal Ni utilization rate is low, and the catalyst cost is high
[0008] CN102274724A discloses a preparation method of a highly active aromatic compound hydrogenation catalyst, which uses graphene as a carrier and Pt as an active component, and its production cost is very high
[0009] Based on the defects in the above-mentioned prior art, it is necessary to seek a new preparation method for dinitrotoluene hydrogenation catalysts, avoiding the use of noble metals or excessive loading (more than 50%), while reducing catalyst costs, Solve the problems such as the need to add solvent and the reaction pressure is too high in the hydrogenation reaction

Method used

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  • Method for preparing nickel catalyst supported on SiO2 microspheres and application of nickel catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Preparation of Solution A: Weigh 500g of distilled water, add 50g of methyl orthosilicate and 100g of formic acid, stir for 100min, and distill to 200ml under reduced pressure. Configuration of emulsifier B: Measure 450ml of phenylethyl alcohol into a three-necked bottle, add 45ml of methylcellulose aqueous solution and 15ml of OP-10, and stir until clear. Preparation of solution C: Weigh 30g of nickel acetate and 4.5g of molybdenum acetate into 115.5g of dilute ammonia water, stir to dissolve. Turn on the stirring, adjust the speed to 500r / min, add 64ml of solution A to the three-necked flask containing emulsifier B, stir and emulsify for 90min, distill off water under reduced pressure at 70°C, filter with suction, wash with deionized water and ethanol three times each, Dry in vacuum at 50°C. Add the filter cake to 200g of ammonia solution with a pH of 9.5, stir, heat to 80°C, and treat for 12hr; add 140g of solution C to the treatment liquid, remove water by rotary e...

Embodiment 2

[0048] Preparation of solution A: Weigh 250g of distilled water, add 50g of ethyl silicate and 50g of acetic acid, stir for 80min, and distill to 90ml under reduced pressure. Configuration of emulsifier B: Measure 300ml of phenylethyl alcohol into a three-necked bottle, add 30ml of methylcellulose aqueous solution and 15ml of OP-8, and stir until clear. Preparation of solution C: Weigh 25g of nickel oxalate, 2g of iron acetate and 2g of manganese acetate into 221g of dilute ammonia water, stir to dissolve. Turn on the stirring, adjust the rotation speed to 400r / min, add 68ml of solution A to the three-necked flask containing emulsifier B, stir and emulsify for 30min, distill off water under reduced pressure at 70°C, filter with suction, wash with deionized water and ethanol three times each, Dry in vacuum at 50°C. Add the filter cake to 200g of ammonia solution with a pH of 8.5, stir, heat to 70°C, and treat for 8hr; add 240g of solution C to the treatment liquid, remove wate...

Embodiment 3

[0053] Preparation of Solution A: Weigh 400g of distilled water, add 50g of ethyl silicate and 75g of acetic acid, stir for 90min, and distill to 150ml under reduced pressure. Configuration of emulsifier B: Measure 380ml of phenylethyl alcohol into a three-necked bottle, add 30ml of methylcellulose aqueous solution, 10ml of OP-6, 5ml of OP-7, and stir until clear. Preparation of solution C: Weigh 15g of nickel oxalate, 12g of nickel acetate, 2g of copper acetate and 2g of iron acetate into 200g of dilute ammonia water, stir to dissolve. Turn on the stirring, adjust the rotation speed to 450r / min, add 100ml of solution A to the three-necked flask containing emulsifier B, stir and emulsify for 60min, distill off water under reduced pressure at 70°C, filter with suction, wash with deionized water and ethanol three times each, Dry in vacuum at 50°C. Add the filter cake to 200g of ammonia solution with a pH of 9.0, stir, heat to 75°C, and treat for 10hr; add 220g of solution C to ...

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Abstract

A method for preparing a nickel catalyst supported on SiO2 microspheres comprises the steps of preparing a water-soluble silicon source solution A; preparing an emulsifier B; preparing an aqueous solution C of a nickel salt and an optional additive metal salt; adding the emulsifier B to the solution A, and performing stirring, suction filtration, washing and drying, so as to obtain SiO2 microspheres; and performing post-treatment on the microspheres by using dilute ammonia water, adding the solution C, and performing impregnation, rotary evaporation, microwave drying, roasting and reduction toobtain the nickel catalyst supported on the SiO2 microspheres. When the nickel catalyst is applied to catalytic hydrogenation of dinitrotoluene DNT for preparing toluene diamine TDA, the conversion rate of DNT is 100% and the selectivity of TDA is 99.9%.

Description

Technical field: [0001] The present invention relates to a preparation method and application of a catalyst, in particular to a catalyst loaded on SiO 2 Preparation method of Ni catalyst on microspheres and its application to DNT hydrogenation to prepare TDA. Background technique: [0002] Toluene diamine (TDA) is an intermediate for the preparation of toluene diisocyanate (TDA), and TDA is an important primary product for the preparation of polyurethane (PU), which is widely used in elastomers, foam plastics, coatings, adhesives and fibers, etc. It is one of the most promising synthetic materials at present. TDA synthesis process mainly includes: iron powder reduction method, alkali sulfide reduction method, electrolytic reduction method, catalytic hydrogenation method, etc. Due to the simple process, high product quality and low environmental pollution, the catalytic hydrogenation method has broad development prospects. Catalytic hydrogenation is divided into gas-phase ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/755B01J23/883B01J23/889C07C209/36B01J35/02B01J35/10C07C211/50B01J35/00
CPCC07C209/36B01J23/755B01J23/883B01J23/8892B01J35/40B01J35/615C07C211/50
Inventor 叶飞崔娇英王磊王同济靳少华易光铨初乃波黎源
Owner WANHUA CHEM GRP CO LTD
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