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Preparation method for nanometer oxide-supported lithium phosphate catalyst for pilot-scale reaction

A nano-oxide, lithium phosphate technology, applied in physical/chemical process catalysts, chemical instruments and methods, chemical/physical processes, etc., can solve the problems affecting the large-scale industrial production of gas-phase isomerization of propylene oxide and the selection of unstable products. It can solve the problems of good catalytic isomerization reaction activity, enhanced strength and tolerance, and stable performance.

Active Publication Date: 2017-04-26
HUBEI UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although the single catalyst efficiency of lithium phosphate prepared by the catalyst disclosed in the above patent is high, the service life of the catalyst is very short, no more than 50h
[0005] Due to technical limitations, the total online life of catalysts in the small-scale gas-phase production process in my country is only about 500 hours, and only small-scale industrial production can be carried out, and it has not been possible to realize large-scale industrial production of gas-phase production from propylene oxide isomerization to allyl alcohol
At present, the research on the application of lithium phosphate catalysts at home and abroad has been very extensive, but the low substrate conversion rate, unstable product selectivity, relatively short online life, etc., have significantly affected the gas phase isomerization of propylene oxide. Large-scale industrial production, so it is of great significance to develop industrial-grade catalysts with high activity, high selectivity, and long online life

Method used

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  • Preparation method for nanometer oxide-supported lithium phosphate catalyst for pilot-scale reaction
  • Preparation method for nanometer oxide-supported lithium phosphate catalyst for pilot-scale reaction
  • Preparation method for nanometer oxide-supported lithium phosphate catalyst for pilot-scale reaction

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Experimental program
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Effect test

Embodiment 1

[0033] Weigh 68.4g of sodium phosphate (0.18mol Na 3 PO 4 12H 2 O) and 30.1g lithium hydroxide (0.72mol LiOH·H 2 O), in molar ratio n(Na 3 PO 4 ):n(LiOH)=1:4, respectively add hot water of 65°C and stir evenly until dissolving to obtain sodium phosphate solution, lithium hydroxide solution (the molar concentration of sodium phosphate solution is 0.5mol / L, the molar concentration of lithium hydroxide solution Concentration is 2.16mol / L); Simultaneously turn on the ultrasonic device (ultrasonic vibration frequency is 50Hz, heating temperature is 65 ℃) and high-speed shearing machine (high-speed shearing speed is 4.0Kr / min), then sodium phosphate solution and hydroxide Lithium solution was quickly and simultaneously added to the ultrasonic reaction device, poured out in 30 seconds, and the mixed solution was stirred and reacted for 2 hours to obtain the reaction product I; then the obtained reaction product I was subjected to aging treatment for 3 hours, and the aged solution...

Embodiment 2

[0036] Weigh 68.4g of sodium phosphate (0.18mol Na 3 PO 4 12H 2 O) and 22.7g lithium hydroxide (0.54mol LiOH·H 2 O), in molar ratio n(Na 3 PO 4 ):n(LiOH)=1:3, respectively add hot water of 65°C and stir evenly until dissolving to obtain sodium phosphate solution, lithium hydroxide solution (the molar concentration of sodium phosphate solution is 0.8mol / L, the molar concentration of lithium hydroxide solution Concentration is 3.0mol / L); Simultaneously open ultrasonic device (ultrasonic vibration frequency is 50Hz, heating temperature is 50 ℃) and high-speed shearing machine (high-speed shearing speed is 4.0Kr / min), then sodium phosphate solution and hydroxide The lithium solution was quickly and simultaneously added to the ultrasonic reaction device in parallel, poured out in 30 seconds, and the mixed solution was stirred and reacted for 3 hours to obtain the reaction product I; then the obtained reaction product I was aged for 2 hours, and the aged solution Carry out suct...

Embodiment 3

[0039] Weigh 68.4g of sodium phosphate (0.18mol Na 3 PO 4 12H 2 O) and 37.8g lithium hydroxide (0.9mol LiOH·H 2 O), in molar ratio n(Na 3 PO 4 ):n(LiOH)=1:5, add hot water of 65 ℃ and stir evenly until dissolving to obtain sodium phosphate solution, lithium hydroxide solution (the molar concentration of sodium phosphate solution is 0.72mol / L, the molar concentration of lithium hydroxide solution Concentration is 3.6mol / L); Simultaneously turn on the ultrasonic device (ultrasonic vibration frequency is 50Hz, heating temperature is 70 ℃) and high-speed shearing machine (high-speed shearing speed is 5.0Kr / min), then sodium phosphate solution and hydroxide Lithium solution was quickly and simultaneously added to the ultrasonic reaction device, poured out in 30 seconds, and the mixture was stirred and reacted for 2 hours to obtain the reaction product I; then the reaction product I was subjected to aging treatment for 2 hours; the aged solution was reduced Suction filtration a...

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Abstract

The invention discloses a preparation method for a nanometer oxide-supported lithium phosphate catalyst for pilot-scale reaction. The preparation method comprises the following steps of first, simultaneously adding a pretreated sodium phosphate solution and a pretreated lithium hydroxide solution into an ultrasonic reaction device, which is provided with a high-speed shearing machine, in a parallel flow manner for a mixed reaction to obtain a reaction generation liquid I; second, performing primary purifying treatment to obtain a white solid I; third, performing roasting treatment to obtain lithium phosphate which serves as a catalyst precursor; fourth, conducting a mixed reaction on the nanometer oxide and an aqueous solution of lithium phosphate by supporting a catalyst by adopting an impregnation method to obtain a reaction generation liquid II; fifth, performing secondary purifying treatment to obtain a white solid II; and finally, performing forming roasting treatment to obtain the nanometer oxide-supported lithium phosphate catalyst. According to the preparation method disclosed by the invention, the method for preparing the supported phosphotungstic acid catalyst by synthesizing, extruding and forming in the mode of combining ultrasonic oscillating and high-speed shearing is adopted; and the method is simple in process, low in cost, high in yield, and high in catalytic activity.

Description

technical field [0001] The invention relates to the technical field of preparation of inorganic non-metallic catalytic materials, in particular to a preparation method of a nanometer oxide-loaded lithium phosphate catalyst used in a pilot test reaction. Background technique [0002] Lithium phosphate is a colorless orthorhombic crystal or white crystal, which is similar to olives. Due to the advantages of no radioactivity, short light but long light effect, and low cost, it is an ideal raw material for the production of colored phosphors; Lithium film is the most widely used electrolyte film in the research of all-solid-state thin-film lithium cells; it is used as a catalyst in the industry for the isomerization of propylene oxide to produce allyl alcohol [Ma Weihua, Chinese patent CN103447056B], and is also used in gas sensors , Glass for special laser materials [Popovic L., Manoun B., Nieuwoudt MK., Comins JD., Journal of Raman Spectroscopy, 2003, 34(1): 77-83; Karthikeyan...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/18
CPCB01J27/1806
Inventor 夏清华鲁新环刘新泰周丹
Owner HUBEI UNIV
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