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Vanadium phosphorus oxide catalyst precursor and catalyst prepared from same

A catalyst, vanadium phosphorus oxygen technology, applied in the direction of catalyst activation/preparation, physical/chemical process catalyst, organic chemistry, etc., can solve the problems of crystal spontaneous agglomeration, reduce the degree of continued reaction, shorten the time, and realize control Effect

Active Publication Date: 2022-05-06
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] Aiming at the drying and other treatment methods after preparing the vanadium phosphorus oxygen catalyst precursor in the prior art, it is easy to cause crystal spontaneous agglomeration, and it is usually necessary to re-granulate before tableting, and the change of the catalyst itself during the drying process also directly affects the performance of the catalyst. The invention provides a preparation method of a vanadium phosphorus oxygen catalyst precursor, changes the drying method, avoids the problem that the crystal is easy to spontaneously agglomerate and the components in the precursor continue to react during the traditional drying process, and improves the catalyst activity

Method used

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  • Vanadium phosphorus oxide catalyst precursor and catalyst prepared from same
  • Vanadium phosphorus oxide catalyst precursor and catalyst prepared from same

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Experimental program
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Effect test

Embodiment 1

[0032] (1) Liquid phase reaction: In the reaction kettle, add 649mL of isobutanol solution, 29.53g of vanadium pentoxide, 0.3g of ferric nitrate hexahydrate, 0.5g of zirconium nitrate, 34.98g of concentrated phosphoric acid, and start stirring , raise the reaction temperature and keep it at 100°C, carry out the reflux reaction, keep the reflux time for 6 hours, the reaction is over, after the reaction solution is cooled to room temperature, it is vacuum filtered, and the filter cake is rinsed three times with a small amount of isobutanol.

[0033] (2) Drying: Place the filter cake in a microwave blast dryer with a microwave pulse frequency of 30Hz, and the drying container rotates at 5r / min. Drying is carried out in three stages, the air speed of the first stage is 800h -1 , adjust the microwave heating power, the temperature of the wet material is at 80°C, and the drying time is 3 hours; after the first stage of drying process is completed, the second stage of drying is carri...

Embodiment 2

[0037] (1) Liquid phase reaction: same as step (1) of Example 1.

[0038] (2) Drying: Drying: Place the filter cake in a microwave blast dryer with a microwave pulse frequency of 30Hz, and the drying container rotates at 5r / min. Drying is carried out in three stages, the air speed of the first stage is 2000h -1 , adjust the microwave heating power, the wet material temperature is 100 ℃, and the drying time is 3 hours; after the first stage of drying process is completed, the second stage of drying is carried out, and the blast air speed in the second stage of drying furnace is 1000h -1 , the temperature of the wet material is 120°C, and the drying time is 1h; after the second stage of drying, the third stage of drying is carried out, and the blast air speed in the third stage of drying furnace is 500h -1 , wet material temperature at 150 ℃, drying time 1h.

[0039] Other steps are with embodiment 1. The finished catalyst C2 was obtained, and its specific surface area and po...

Embodiment 3

[0041] Except that the drying process in step (2) does not carry out rotary stirring, other are the same as embodiment 1. The finished catalyst C3 was obtained, and its specific surface area and pore diameter results are shown in Table 1.

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Abstract

The invention relates to a vanadium phosphorus oxide catalyst precursor, which is prepared by the following steps: filtering a vanadium phosphorus oxide catalyst precursor solution prepared by a liquid phase method, and carrying out microwave forced air drying and roasting on the obtained solid to obtain catalyst precursor powder; the microwave forced air drying is divided into three sections, in the first section, the drying temperature is 60-120 DEG C, the drying time is 1-24 h, and the air blowing air speed is 500-2000 h <-1 >; in the second stage, the drying temperature is adjusted to be 80-140 DEG C, the drying time is 0.5-12 h, and the air blowing air speed is 300-1000 h <-1 >; and the third-stage drying temperature is 100-180 DEG C, the drying time is 0.5-8 hours, and the blast air speed is 50-500 h <-1 >. According to the drying mode, the inside and the outside of the precursor wet material are rapidly and uniformly heated, the solvent is uniformly escaped, the evaporation partial pressure of the solvent is obviously reduced by combining high-airspeed forced air drying treatment and introducing air or inert atmosphere, the heated solvent in the wet material is rapidly removed, crystal grains are not agglomerated, the dispersion is good, and the product quality is improved. And re-granulation is not needed before subsequent tabletting preparation of the catalyst.

Description

technical field [0001] The invention relates to the technical field of catalyst preparation, in particular to a vanadium phosphorus oxygen catalyst precursor and a catalyst prepared therefrom. Background technique [0002] Vanadium phosphorus oxygen catalyst is a catalyst composed of vanadium, phosphorus and oxygen. It has good electron transport function and oxygen transport performance. It is often used in the reaction of C4 hydrocarbon oxidation to maleic anhydride. The most effective catalyst used in the maleic anhydride production reaction system, its main active phase component is vanadyl pyrophosphate, and its catalytic performance is also closely related to the preparation method. Since the first commercial application of VPO catalyst by Monsanto Company in the United States in 1974, people have conducted in-depth research on its preparation method, see CATAL.REV.-SCI.ENG.27 (1985): 373. [0003] There are many studies on the preparation of vanadium phosphorus oxyge...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/198B01J35/10B01J37/34B01J37/08B01J35/02C07D307/60
CPCB01J27/198B01J37/346B01J37/08B01J37/0009C07D307/60B01J35/50B01J35/613B01J35/643
Inventor 姜睿王海波勾连科张霞彭绍忠周峰
Owner CHINA PETROLEUM & CHEM CORP