Nickel base catalyst preparation method

A nickel-based catalyst and catalyst technology, applied in chemical instruments and methods, physical/chemical process catalysts, metal/metal oxide/metal hydroxide catalysts, etc., can solve the problem that the catalyst has a small average pore size and is not suitable for the reaction of macromolecular substances and other issues to achieve stable performance

Active Publication Date: 2013-12-04
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Zhang Yuhong et al. prepared AlOOH sol by pseudo-boehmite peptization method, by dispersing Ni(NO 3 ) 2 Solution Preparation of NiO/γ-Al with High Thermal Stability 2 o 3 catalyst( Petroleum Re

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Example Embodiment

[0015] 【Example 1】

[0016] With nitric acid in [H + ] / [AlOOH] molar ratio is under the condition of 0.25, peptized pseudo-boehmite powder 24 hours, obtains alumina sol 1500g that alumina solid content is 5%, nickel chloride is dissolved in an appropriate amount of water, obtains 0.10 grams of nickel / ml of nickel salt solution. Add an appropriate amount of nickel salt solution to the aluminum sol, adjust the PH~8.5 of the sol with ammonia water, and then o Under aging for 24 hours under C, then through filtration, washing and vacuum drying (vacuum tightness 30KPa, drying time 20 hours, promptly obtain corresponding catalyst precursor. Catalyst precursor is in 400 o C roasting for 4 hours to obtain oxidized NiO / Al 2 o 3 catalyst. Catalyst in 1.5 L / min pure hydrogen flow, at 450 o Reduction at C for 12 hours to obtain metallic Ni / Al 2 o 3 catalyst.

[0017] Change the amount of nickel salt solution added to the aluminum sol to obtain catalysts 1-2 in turn, see Table 1. ...

Example Embodiment

[0019] [Example 2]

[0020] With nitric acid in [H + ] / [AlOOH] molar ratio of 0.25, the pseudo-boehmite powder was peptized for 24 hours to obtain 1500 g of alumina sol with a solid content of 5% alumina. In terms of molar ratio, basic nickel carbonate: ammonia water: ammonium carbonate = 1: 6.0: 1.5, adding an appropriate amount of water to obtain a nickel-ammonia complex solution of 0.10 g nickel / ml. Add an appropriate amount of nickel ammonia complex solution to the aluminum sol, at 95 o Heat and decompose the complexed nickel ions at C for 8 hours, and then filter, wash and vacuum dry (vacuum degree 50KPa, drying time 25 hours) to obtain the corresponding catalyst precursor. catalyst precursor at 400 o C roasting for 4 hours to obtain oxidized NiO / Al 2 o 3 catalyst. Catalyst in 1.5 L / min pure hydrogen flow, at 450 o Reduction at C for 12 hours to obtain metallic Ni / Al 2 o 3 catalyst.

[0021] Change the amount of nickel-ammonia complex solution added to the alumi...

Example Embodiment

[0030] [Example 3]

[0031] The hydrogenation activity test and 800-hour stability test of the catalyst of the present invention were carried out. The properties of the raw oil used in the experiment are shown in Table 3. Catalyst 4 in embodiment 2 and catalyst 7 in comparative example 1 were respectively at 450 o C was reduced with hydrogen for 24 hours. The hydrogenation reaction uses an adiabatic fixed-bed reactor, and the process conditions are: the inlet temperature is 50 o C, pressure 3.0 MPa, fresh oil space velocity LHSV=1.5 hours -1 , the volume ratio of hydrogen to oil H 2 / Feed oil = 600:1, the evaluation results of Catalyst 4 and Catalyst 7 are shown in Table 4 and Table 5.

[0032] table 3

[0033]

[0034] Table 4

[0035]

[0036] table 5

[0037]

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Abstract

The invention relates to a nickel base catalyst preparation method, wherein technical problems of low specific surface and small average pore size in the prior art are mainly solved with the present invention. The technical scheme comprises: adopting an alumina sol as a carrier precursor, and adding a nickel salt aqueous solution or a nickel-ammonia complex to the alumina sol at a temperature of 45-80 DEG C to obtain a nickel-aluminum sol; at a temperature of 45-120 DEG C, carrying out standing aging on the nickel-aluminum sol or carrying out heating decomposition on the nickel-ammonia complex to obtain a nickel-aluminum gel; and carrying out washing, drying, forming, calcination and reduction on the obtained gel to obtain the required nickel base catalyst, wherein the gel is subjected to vacuum freeze drying after being washed, a vacuum freeze drying time is 20-40 h, and a vacuum degree is 30-100 KPa. With the technical scheme, the problems are well solved, and the preparation method can be widely used for hydrogenation industrial production.

Description

technical field [0001] The invention relates to a preparation method of a nickel-based catalyst. Background technique [0002] Currently, for cleaving C9 + The hydrogenation catalyst is mainly Ni / Al 2 o 3 or Ni / Al 2 o 3 -SiO 2 , due to C 9 + There are a large number of polymerizable active components in the distillate, mainly styrene and its derivatives, dicyclopentadiene and its derivatives, indene and its derivatives, etc., and As, S, O, N and other impurities and colloid content Higher, the catalyst deactivates quickly, so the catalyst has to be activated and regenerated frequently. Therefore, it is hoped that the hydrogenation catalyst has high low-temperature activity, high resistance to impurity poisoning and appropriate gel capacity, so as to increase the catalyst regeneration cycle and prolong the service life of the catalyst. Liang Shunqin of Lanhua Institute prepared a new type of Ni / Al with high nickel content by co-precipitation method 2 o 3 -SiO 2 Ca...

Claims

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Application Information

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IPC IPC(8): B01J23/755B01J35/10C10G45/36
Inventor 赵多王建强刘仲能任杰
Owner CHINA PETROLEUM & CHEM CORP
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