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Cu/Cr-based catalyst, preparation method thereof and application of Cu/Cr-based catalyst in preparation of 1, 2-pentanediol

A catalyst, propylene glycol technology, applied in the preparation of hydroxyl compounds, physical/chemical process catalysts, metal/metal oxide/metal hydroxide catalysts, etc., can solve the problems of dependence on imports, low catalytic activity, high cost, etc., and achieve low prices , efficient conversion, high selectivity effect

Pending Publication Date: 2022-05-31
QINGDAO INST OF BIOENERGY & BIOPROCESS TECH CHINESE ACADEMY OF SCI
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  • Abstract
  • Description
  • Claims
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AI Technical Summary

Problems solved by technology

In the olefin oxidation method, olefins are used as raw materials, and 1,2-pentanediol is obtained through multi-step reactions and operations in the presence of catalysts and oxidants. The complex reaction route and high production costs limit its large-scale application.
The latter uses a wide range of stable biomass resources as raw materials to produce 1,2-pentanediol through catalytic hydrogenolysis technology. The catalytic hydrogenolysis of biomass-based furan derivatives mainly uses noble metals as catalysts and has low catalytic activity, making it difficult to produce 1,2-pentanediol. Promote application
[0005] There are very few domestic enterprises producing 1,2-pentanediol, especially those with large output. This makes domestic 1,2-pentanediol have to rely on imports, which largely restricts the production of propiconazole and high-end skin care products in my country. product development
In addition, the 1-pentene and 1,2-pentanediol raw materials used to synthesize 1,2-pentanediol depend on imports, and the high cost is also an important reason for restricting the synthesis of 1,2-pentanediol in my country.

Method used

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  • Cu/Cr-based catalyst, preparation method thereof and application of Cu/Cr-based catalyst in preparation of 1, 2-pentanediol
  • Cu/Cr-based catalyst, preparation method thereof and application of Cu/Cr-based catalyst in preparation of 1, 2-pentanediol
  • Cu/Cr-based catalyst, preparation method thereof and application of Cu/Cr-based catalyst in preparation of 1, 2-pentanediol

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0043] Catalyst preparation: 1) Mix copper nitrate, aluminum nitrate, and zinc nitrate into 200mL mixed solution (referred to as solution I), and the molar concentrations are 0.4mol / L, 0.2mol / L, and 0.3mol / L respectively; 2) prepare Concentration is 1.0mol / L ammonium chromate solution 150mL, add a certain volume of concentrated ammonia water, make n(NH 3 ) / n(Cr)=2 (referred to as solution II); 3) titrate solution II into solution I, and stir while titrating; 4) after titration, stir at room temperature for 1 h; 5) Suction filter and wash the obtained mixture until the filtrate becomes neutral, and dry the precipitate at 110°C for 12h; 6) Rise the dried solid to 100°C at 3°C / min in a muffle furnace After keeping at ℃ for 1h; continue to raise the temperature to 200℃ and keep for 1h; raise the temperature to 300℃ and keep for 1h; then raise the temperature to 400℃ and keep for 1h and then lower to room temperature to obtain catalyst 1, figure 1 It is the XRD pattern of catalyst...

Embodiment 2

[0046] Catalyst preparation: 1) Mix copper nitrate and magnesium nitrate into 400mL mixed solution (referred to as solution I), and the molar concentrations are 0.4mol / L, 0.2mol / L, 0.1mol / L respectively; 2) The prepared concentration is 1.3 mol / L ammonium chromate solution 160mL, add a certain volume of concentrated ammonia water to make n(NH 3 ) / n(Cr)=1.8 (referred to as solution II); 3) titrate solution II into solution I, and stir while titrating; 4) after titration, stir at room temperature for 2 h; 5) Suction filter and wash the obtained mixture until the filtrate becomes neutral, and dry the precipitate at 110°C for 24h; 6) Rise the dried solid to 120°C at 2°C / min in a muffle furnace After keeping at ℃ for 1h; continue to raise the temperature to 210℃ and keep for 1h; raise the temperature to 320℃ and keep for 1h; then raise the temperature to 450℃ and keep for 3h and then cool down to room temperature to obtain catalyst 2, figure 2 It is the XRD pattern of catalyst 2....

Embodiment 3

[0049] Catalyst preparation: 1) Mix copper nitrate, aluminum nitrate, and calcium nitrate into 400mL mixed solution (referred to as solution I), and the molar concentrations are 0.4mol / L, 0.2mol / L, and 0.1mol / L respectively; 2) Prepare Concentration is 1.3mol / L ammonium chromate solution 160mL, add a certain volume of concentrated ammonia water, make n(NH 3 ) / n(Cr)=1.8 (referred to as solution II); 3) titrate solution II into solution I, and stir while titrating; 4) after titration, stir at room temperature for 2 h; 5) Suction filter and wash the obtained mixture until the filtrate becomes neutral, and dry the precipitate at 110°C for 24h; 6) Rise the dried solid to 110°C at 3°C / min in a muffle furnace After keeping ℃ for 1 hour; continue to raise the temperature to 230 ℃ and keep it for 1 hour; raise the temperature to 320 ℃ and keep it for 1 hour;

[0050] Reaction evaluation: Add 20mmol 1,2-propanediol into the batch autoclave, add 15mL of ethanol, add 0.25g catalyst 3 pre...

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Abstract

The invention discloses a Cu / Cr-based composite metal oxide catalyst, a preparation method of the Cu / Cr-based composite metal oxide catalyst and application of the Cu / Cr-based composite metal oxide catalyst in preparation of 1, 2-pentanediol from ethanol and 1, 2-propylene glycol. The catalyst is represented as Cum1Crm2Xm3Om4, m1, m2 and m3 are respectively molar ratios of metal Cu, Cr and X active components, and m4 is the chemical oxygen demand of the stoichiometric ratio. Wherein m1 is in the range of 0.1 to 10, m2 is in the range of 0.1 to 10, m3 is in the range of 0 to 5, and m4 is the chemical oxygen demand of the stoichiometric ratio. The invention provides a new preparation route of bio-based 1, 2-pentanediol by taking rich and cheap low-carbon alcohol as a raw material, and solves the problems that the price of raw materials in the existing 1, 2-pentanediol production technology is high, and the existing 1, 2-pentanediol production technology is generally complicated in process flow, relatively high in production cost, serious in equipment corrosion and the like. According to the non-noble metal copper / chromium-based catalyst, efficient conversion of 1, 2-propylene glycol under mild conditions is achieved, the selectivity of the target product 1, 2-pentanediol can reach 60% or above, and the catalyst has the advantages of being easy to prepare and low in price.

Description

technical field [0001] The invention belongs to the field of chemical catalysts, and relates to a preparation method of 1,2-pentanediol, in particular to a Cu / Cr-based composite metal oxide catalyst, a preparation method thereof and a method for preparing 1,2-pentanediol use. Background technique [0002] 1,2-Pentanediol is a key intermediate for the synthesis of the fungicide propiconazole. In recent years, with the gradual promotion of the application of this fungicide, the demand for 1,2-Pentanediol has increased year by year; at the same time, 1,2- Pentylene glycol has excellent moisturizing properties and antiseptic effects, and can be used in various skin care products such as skin cream, eye cream, skin care water, baby care products, and sunscreen; in addition, 1,2-pentanediol is also used in the production of polyester fibers, surface active Important raw materials for pharmaceuticals, medicines and other products. [0003] At present, the traditional method of pr...

Claims

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Application Information

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IPC IPC(8): B01J23/86C07C29/34C07C31/20
CPCB01J23/868C07C29/34C07C31/20Y02P20/52
Inventor 杨勇郭星翠
Owner QINGDAO INST OF BIOENERGY & BIOPROCESS TECH CHINESE ACADEMY OF SCI
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