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Supported transition metal phosphide catalyst, preparation method and application thereof

A transition metal and catalyst technology, applied in the field of supported transition metal phosphide catalyst and its preparation, can solve the problems of poor stability, increased catalyst production cost, easy aggregation and deactivation of copper-based catalyst, etc., and achieves good stability and production cost. Low effect, simple preparation method

Active Publication Date: 2017-12-15
中科合成油内蒙古技术研究院有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although both copper-based catalysts and silver-based catalysts have good hydrogenation results, copper-based catalysts are prone to aggregation and deactivation, and have poor stability, while the use of noble metals greatly increases the production cost of the catalyst. These two aspects currently restrict glycolic acid production. The bottleneck of the large-scale industrial production of methyl ester and ethylene glycol, therefore, there is an urgent need to develop a new catalyst for the synthesis of methyl glycolate and ethylene glycol with high activity, high selectivity and long life

Method used

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  • Supported transition metal phosphide catalyst, preparation method and application thereof
  • Supported transition metal phosphide catalyst, preparation method and application thereof
  • Supported transition metal phosphide catalyst, preparation method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0048] 1) Weigh 7.7g of nickel nitrate and 3.5g of diammonium hydrogen phosphate, add them into 23ml of deionized water to form a precipitate, add 2.4ml of nitric acid dropwise within 6min to dissolve the precipitate, and obtain an impregnation solution;

[0049] 2) impregnate an equal volume of 14g SiO with the impregnating solution obtained in step 1) 2 on the carrier, placed at room temperature for 8 hours, dried at 110°C for 14 hours, and calcined at 420°C for 3 hours to obtain the catalyst precursor;

[0050] 3) The catalyst precursor obtained in step 2) is heated to 550°C at a heating rate of 4°C / min in a hydrogen atmosphere to perform a reduction reaction, and H 2 The airspeed is 2000h -1 , treated at constant temperature for 3 hours, after the reaction was completed, the temperature was cooled to room temperature, and 1v% O 2 / N 2 Mixed gas passivation treatment for 4 hours to obtain the supported transition metal phosphide catalyst provided by the present invention...

Embodiment 2

[0058] 1) Weigh 14.5g of nickel nitrate and 6.6g of diammonium hydrogen phosphate, add them into 18ml of deionized water to form a precipitate, add 4.5ml of nitric acid dropwise within 12min to dissolve the precipitate, and obtain an impregnating solution;

[0059] 2) impregnating an equal volume of 31 g of ZnO carrier with the impregnating solution obtained in step 1), placing it at room temperature for 4 hours, drying at 110°C for 12 hours, and roasting at 400°C for 5 hours to obtain a catalyst precursor;

[0060] 3) The catalyst precursor obtained in step 2) is heated to 600 ° C at a heating rate of 2 ° C / min in a hydrogen atmosphere to perform a reduction reaction, H 2 The airspeed is 2500h -1 , treated at constant temperature for 3 hours, after the reaction was completed, the temperature was lowered to room temperature, and 1% O 2 / N 2 Mixed gas passivation treatment for 4 hours to obtain the supported transition metal phosphide catalyst provided by the present invent...

Embodiment 3

[0069] 1) Weigh 9.73g of nickel nitrate and 4.42g of diammonium hydrogen phosphate, add them into 14ml of deionized water to form a precipitate, add 3ml of nitric acid dropwise within 8min to dissolve the precipitate, and obtain an impregnation solution;

[0070] 2) impregnate an equal volume of 18.5g TiO with the impregnating solution obtained in step 1) 2 on the carrier, placed at room temperature for 7 hours, dried at 110°C for 9 hours, and calcined at 480°C for 4 hours to obtain the catalyst precursor;

[0071] 3) The catalyst precursor obtained in step 2) is heated to 650°C at a heating rate of 1°C / min in a hydrogen atmosphere to perform a reduction reaction, and H 2 The airspeed is 3600h -1 , treated at a constant temperature for 4 hours, after the reaction was completed, the temperature was cooled to room temperature, and 1v% O 2 / N 2 Mixed gas passivation treatment for 4 hours to obtain the supported transition metal phosphide catalyst provided by the present invent...

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Abstract

The invention discloses a supported transition metal phosphide catalyst, a preparation method and application thereof. The supported transition metal phosphide catalyst consists of NixPy and a carrier; the NixPy is loaded on the carrier. In the above-mentioned loaded transition metal phosphide catalyst, the carrier is selected from at least one of silicon dioxide, titanium dioxide, zinc oxide and activated carbon; the mass parts of the NixPy are 8-16 parts; the mass parts of the carrier are 84‑92 parts; the molar ratio of Ni and P is (0.5‑2):1. The catalyst uses diammonium hydrogen phosphate as the phosphorus source, uses metal nickel nitrate as the precursor, and uses one of silicon dioxide, zinc oxide, titanium dioxide, activated carbon, etc. as the carrier, and adopts the method of temperature-programmed reduction. Rapid and efficient synthesis of supported NixPy catalyst under reducing atmosphere, which has good hydrogenation activity of dimethyl oxalate and selectivity of methyl glycolate and ethylene glycol.

Description

technical field [0001] The invention belongs to the field of petrochemical industry, and relates to a supported transition metal phosphide catalyst and its preparation method and application. Background technique [0002] Ethylene glycol (EG) is an important basic organic raw material in petrochemical industry, from which more than 100 chemical products and chemicals can be derived. Ethylene glycol is mainly used to react with terephthalic acid (PTA) to produce polyethylene terephthalate (PET), that is, polyester resin, which can be used as a raw material for polyester fibers and polyester plastics. In addition, it can also be used in the production of unsaturated polyester resins, lubricants, plasticizers, nonionic surfactants and explosives, etc., and has a wide range of uses. [0003] According to the source of raw materials, the production methods of ethylene glycol can be divided into two categories: petroleum route and non-petroleum route. At present, large-scale eth...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/185C07C31/20C07C29/149C07C69/675C07C67/31
CPCY02P20/52
Inventor 陈红梅朱玉雷郑洪岩丁国强高晓庆杨勇李永旺
Owner 中科合成油内蒙古技术研究院有限公司
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