CN85102809A - A kind of decomposable non-pollutant technology of dip type nickel series conversion catalyzer preparation - Google Patents
A kind of decomposable non-pollutant technology of dip type nickel series conversion catalyzer preparation Download PDFInfo
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- CN85102809A CN85102809A CN 85102809 CN85102809A CN85102809A CN 85102809 A CN85102809 A CN 85102809A CN 85102809 CN85102809 CN 85102809 CN 85102809 A CN85102809 A CN 85102809A CN 85102809 A CN85102809 A CN 85102809A
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Abstract
The present invention is the non-pollution technology of dip type nickel series Preparation of Catalyst, promptly after the nickel nitrate maceration extract adds catalyst base, adds amount of urea again, makes its reaction.Whole process does not produce the nitrogen oxide (NO that pollutes
X), and the molten mistake of nickel is few, and activity intensity and surface strength all improve than conventional method.The present invention is simple, does not need special installation, is applicable to the production of new factory of old factory dip type nickel series conversion catalyzer, replaces the technology that conventional generation is polluted.
Description
The invention belongs to the preparation method of dip type nickel series conversion catalyzer, employing be a kind of decomposable non-pollutant technology, this catalyst uses in the production process of producing hydrogen from steam conversion of hydrocarbons.And hydrogen is widely used in the hydrogenation process of synthetic ammonia methyl alcohol and petroleum refining industry.
At home and abroad in the production of dip type nickel series conversion catalyzer, the generation type of active component nickel oxide, the overwhelming majority are nickel nitrate directly decomposes, and discharges a large amount of nitrogen oxide NO in the decomposable process
x, corrosion catalyst prod and production equipment, and cause serious environmental to pollute,
Ways of addressing this issue has the lime cream absorption method of Denmark abroad, and alkali wash and ammonification catalytic reduction method etc. are arranged at home, but because of NO
xRelease be intermittently erratic process, all can not reach equalization operation with alkali cleaning and catforming, thus purify far not thorough, and also complexity of equipment.
Once addressing in G ', C, Maiti et all J.Indian chem soc, 1975.10 with nickel-ammonium complex ion is that maceration extract replaces the nickel nitrate maceration extract, can improve the dispersiveness of nickel, helps activity of such catalysts; In United States Patent (USP) 4191664, once addressed nickel-ammonium complex ion solution and produced immersion-type or sedimentation type reforming catalyst and methanation catalyst,, but all do not relate to decomposing N O also from the catalyst modification angle
xPollution and elimination problem.
The present invention is directed to preceding method and have NO
xPollution problem, and it is unsatisfactory to handle the way that these pollutions take, and studies and solves for seeking simpler more perfect processing approach.
In producing the process of dip type nickel series conversion catalyzer, the present invention is according to common method.
Characteristics of the present invention are: in decomposable process, not to decompose with the form of nickel nitrate, but decompose with the form of nickel hydroxide, like this, just can not produce this harmful polluter of nitrogen oxide in the decomposable process, on the contrary, also can generate ammonium nitrate, can wash with water and get rid of or reclaimed as useful fertilizer.
For satisfying above-mentioned condition, the present invention adopt add a kind of solid form during the course contain the ammonium material in carrier, this is the most simple and easy to do, also can not cause the volatilization of ammonia and contaminated environment, the ammonia loss is minimum again.This material is exactly urea and carbonic hydroammonium.
Technical process of the present invention is as follows:
After the nickel nitrate maceration extract adds catalyst base, introduce the amount of urea aqueous solution again, the addition of urea is: URe/Ni(NO
3)
26H
2O=0.3～1.1/1(mol), best scope is 0.7～1.1/1.Flooded 30～90 minutes being lower than under 60 ℃ of temperature, deliver to heater then, added thermal response 1～2 hour at this, temperature is controlled in 60 ℃～100 ℃ scopes, and best temperature range is 60 ℃～80 ℃.Make nickel nitrate be converted into nickel hydroxide in catalyst, reaction equation is:
Urea the OH that provides in the solution is provided
-And NH
+ 4Ion.Reaction equation:
In this reaction, obtain nickel hydroxide and ammonium nitrate.Ammonium nitrate can the water extraction be cleaned discharge, also can reclaim as fertilizer sources and be used.The present invention is not that routinely method washes with water in this washing procedure, but with the ammonium bicarbonate soln washing, its effect is the molten mistake that can reduce nickel, because the carbonic hydroammonium hydrolysis can provide OH
-, the pH value of change solution, the addition that helps the stable carbonic hydroammonium of nickel hydroxide is: contain NH in the washings
4HCO
3Big in 0.1%～1% scope, best scope is dry under 80 ℃～100 ℃ conditions, last again after the washing of 0.2%～0.5% carrier, and the nickel hydroxide that reaction generates decomposes in roasting process again, does not just generate the material NO that has corrosion and pollute
x.Reaction equation is as follows:
The decomposition temperature of this reaction is in 450 ℃～700 ℃ scopes.Best scope is 500～600 ℃.Obtain the catalyst finished product at this, whole process does not have polluter to emit.
Experiment embodiment:
Maceration extract preparation: get 8.5～9N nickel nitrate aqueous solution, in urea: ratio nickel nitrate=0.8(molecular proportion), add industrial urea, at room temperature gentle agitation is about 10 minutes, promptly get all-transparent urea-nickel nitrate binary aqueous, can be for dipping usefulness, solution at room temperature can be stabilized and deposits, repeatedly multiplexing, must not be heated to more than 60 ℃.
Catalyst base drops in the above-mentioned maceration extract and soaked 2 hours, and taking-up drains.Put again in the baking oven in heating more than 80 ℃ 1～2 hour.
The oven dry thing changes in the beaker, adds thin ammonium bicarbonate aqueous solution (about weight concentration 0.5%), and its amount is with submergence oven dry thing degree of being.Soaked 2 hours, and drained, go washing lotion.This embathes operation repetition 3～5 times, does not have NO substantially to washing lotion
- 3End (analyse to test with 2% diphenylamine sulfate and do not show blue look) when analyzing.In case of necessity, washing can be carried out under heating and air-flow stirring.
Clean thing drains, and puts in the baking oven and dries.500 ℃ * 3h adds thermal decomposition, so that make Ni(OH)
2Change NiO into.Substantially there is not NO during decomposition
xTobacco.
Aforementioned dipping operation splitting can repeat 2～3 times, to guarantee NiO amount enough in the catalyst.
The present invention is simple and easy to do, is applicable to the production of the multiple immersion-type catalyst of Xin Chang, old factory, does not need special installation, need only increase washings make-up tank (being the carbonic hydroammonium dissolving tank) water pump and a head tank and get final product.The auxiliary material that increased consume limitedly, experiment showed, that the molten mistake of nickel of this law is few, and activity intensity also increases to some extent.
Constant with one group of homemade industrialized catalyst Z405 carrier, adopt catalyst (representing) that this technology makes to compare experiment with corresponding external trade mark ICI-46-4 with GZ405, the normal pressure activity is with carbon space velocity 40000h
-1, 800 ℃ of reduction temperatures, 750 ℃ of operating temperatures, the active methane milliliter numerical table that transforms with per minute on every gram catalyst shows.Following table is the performance comparison of catalyst:
Last table has illustrated that non-pollution technology of the present invention helps the raising of the active and intensity of raw catalyst, and the mechanical wear rate is decline to some extent also, and in these areas performance is better than the ICI46-4 catalyst after the processing.
Claims (11)
1, the non-pollution technology of dip type nickel series catalysts replaces the conventional method for preparing catalyst, it is characterized in that, after the nickel nitrate maceration extract adds catalyst base, introduces amount of urea again, makes its reaction generate nickel hydroxide.
2, by claim 1 described method, the addition of urea is about URe: Ni(NO
3)
26H
2O=(0.3～1.1): 1(mol).
3, by claim 2 described URe/Ni(NO
3)
26H
2O=0.7～1.1/1 best results.
4, by claim 1 described method, it is characterized in that, in cleaning solution, add an amount of carbonic hydroammonium, can change the pH value of solution, reduce the molten mistake of nickel.
5, described by claim 4, the concentration of the carbonic hydroammonium of adding is greatly in 0.1～1% scope.
By claim 1 described method, it is characterized in that 6, reaction is to carry out under the condition of heating, the control temperature is in 60 ℃～100 ℃ scopes.
By claim 1 described method, it is characterized in that 7, the ammonium nitrate that reaction obtains is cleaned with the extraction of carbonic hydroammonium weak solution.
8, by claim 1 described method, it is characterized in that the nickel hydroxide of generation carries out decomposition reaction again, do not contained the material of atmosphere pollution.
9, described by claim 8, the temperature that nickel hydroxide decomposes is greatly in 450 ℃～700 ℃ scopes.
10, described by claim 9, decomposition temperature is controlled at best results in 500 ℃～600 ℃ scopes.
11, by claim 1,4,5 described methods, it is characterized in that comprising the relevant devices for preparing ammonium bicarbonate soln, comprise preparation vessel, pump, head tank etc.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 85102809 CN85102809A (en) | 1985-04-13 | 1985-04-13 | A kind of decomposable non-pollutant technology of dip type nickel series conversion catalyzer preparation |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 85102809 CN85102809A (en) | 1985-04-13 | 1985-04-13 | A kind of decomposable non-pollutant technology of dip type nickel series conversion catalyzer preparation |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN85102809A true CN85102809A (en) | 1987-03-25 |
Family
ID=4792775
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 85102809 Pending CN85102809A (en) | 1985-04-13 | 1985-04-13 | A kind of decomposable non-pollutant technology of dip type nickel series conversion catalyzer preparation |
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|---|---|
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103055957A (en) * | 2011-10-24 | 2013-04-24 | 中国石油化工股份有限公司 | Preparation method of supported catalyst |
| CN104772154A (en) * | 2014-01-15 | 2015-07-15 | 南京大学 | Preparation method of silica supported nickel phosphide catalyst |
| CN105709800A (en) * | 2014-12-04 | 2016-06-29 | 中国石油化工股份有限公司 | Low-NOx-emission preparation method for hydrocracking catalyst |
-
1985
- 1985-04-13 CN CN 85102809 patent/CN85102809A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103055957A (en) * | 2011-10-24 | 2013-04-24 | 中国石油化工股份有限公司 | Preparation method of supported catalyst |
| CN104772154A (en) * | 2014-01-15 | 2015-07-15 | 南京大学 | Preparation method of silica supported nickel phosphide catalyst |
| CN105709800A (en) * | 2014-12-04 | 2016-06-29 | 中国石油化工股份有限公司 | Low-NOx-emission preparation method for hydrocracking catalyst |
| CN105709800B (en) * | 2014-12-04 | 2019-03-19 | 中国石油化工股份有限公司 | A kind of low NOxThe hydrocracking catalyst preparation method of discharge |
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