CN107055583A - The method that ammonia-alum is prepared by raw material of dead catalyst - Google Patents
The method that ammonia-alum is prepared by raw material of dead catalyst Download PDFInfo
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- CN107055583A CN107055583A CN201710299511.1A CN201710299511A CN107055583A CN 107055583 A CN107055583 A CN 107055583A CN 201710299511 A CN201710299511 A CN 201710299511A CN 107055583 A CN107055583 A CN 107055583A
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- alum
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- dead catalyst
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/68—Aluminium compounds containing sulfur
- C01F7/74—Sulfates
- C01F7/76—Double salts, i.e. compounds containing, besides aluminium and sulfate ions, only other cations, e.g. alums
- C01F7/762—Ammonium or alkali metal aluminium sulfates
- C01F7/765—Ammonium aluminium sulfates
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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Abstract
A kind of method that ammonia-alum is prepared by raw material of dead catalyst, step：Sulfuric acid is added in the dead catalyst containing aluminium produced into petrochemical industry production process and is soaked, immersion puts into the container with agitating device and heater after terminating and is stirred reaction in the on state, stirring reaction is transferred to centrifugal separating device centrifugation after terminating, obtain the thick liquid of aluminum sulfate；Concentrated ammonia liquor is added into the thick liquid of obtained aluminum sulfate, neutralization reaction is carried out under stirring and heated condition, the mixing speed for controlling agitator, the heating-up temperature for controlling heater, the time of control neutralization reaction and the pH value for controlling reaction system, obtain the thick liquid of alum；The thick liquid of obtained alum is first transferred to crystallizing pond and carries out crystallization reaction, then carries out press filtration, thick ammonia-alum filter cake is obtained；To obtained thick ammonia-alum filter cake elution and Non-leaching degree, through drying, finished product ammonia-alum is obtained.Meet preparation of industrialization requirement；Economize on resources, environmental protection；Purity is preferable.
Description
Technical field
The invention belongs to fixed-end forces and inorganic salts preparing technical field, and in particular to one kind is using dead catalyst as raw material system
The method of standby ammonia-alum.
Background technology
Above mentioned dead catalyst（Also dead catalyst containing aluminium can be claimed, it is as follows）Refer mainly to but be not definitely limited to refer to stone
Change the solid waste rich in aluminium element that industry is produced in production process such as catalytic cracking process（Custom is referred to as " solid waste "）.
Petrochemical industry is to support one of mainstay of China economy, in recent years whether total size or actual production capacity
All constantly expanding, so the dead catalyst produced every year is also being continuously increased, 400,000 tons or so are reached at present.Due to oil
Industrial and commercial bank's industry used catalyst is universal using aluminum oxide as carrier and the mass fraction of aluminium（That is quality % contents）25% or so is reached, because
This is recycled to dead catalyst, can not only be avoided dead catalyst from directly discharging and be undermined environment, and can become give up into
Treasured, realizes maximally utilizing for resource.However, at present, many small-scale petroleum chemical enterprises of China are for reply environment protection standard row
Extremely simple processing can only mostly be made to dead catalyst by putting requirement, or even because processing cost looks for an opportunity to arrange steathily greatly.Although being no lack of rule
The big enterprise of mould is handled dead catalyst, but is due to be subject to processing that cost is high, treatment technology falls behind relatively, special skill personnel are short
Scarce etc factor restricts and is still unable to reach the degree of recycling, that is, is not enough to embody the saving that the current whole society advocates
Type, circular-type economy spirit.Accordingly, it would be desirable to which development process cost is low, the simple spent catalyst recovery method of operating procedure.
Ammonia-alum is Monoaluminum monoammonium disulfate Dodecahydrate（Also referred to as " aluminium ammonium alum ", " ammonium alum " or " jewel alum "）Due to uniqueness
Performance, be widely used in water purification industry, paper-making industry, alumina producing industry, dyeing industry, pharmaceutical sector and grocery trade.Current ammonia-alum
Main production process be with sulfuric acid treatment bauxite be made aluminum sulfate, then with ammonium sulfate or ammoniacal liquor reaction be made, because of the method
Using bauxite, therefore exhaustive exploitation and the waste of resource can be caused.
The natural resources of bauxite etc can both be protected by preparing ammonia-alum using solid waste, be avoided that again and undermined environment, and
The technical information that ammonia-alum is prepared using solid waste can be seen in disclosed Chinese patent literature, it is typical such as CN104445330B
" a kind of production method of ammonia-alum " recommended, it is to utilize the solid waste produced in aluminum profile extrusion pretreatment process to give up
Aluminium slag be raw material successively through slurrying, prepare the thick liquid sedimentation of the thick liquid of aluminum sulfate, aluminum sulfate, the thick liquid preparation of alum, crystallisation by cooling,
Wash and dry, obtain ammonia-alum.The patent realizes the recycling of aluminum dross, emerges from the 0016th section of note of its specification
The technique effect of load.But it is more to there is operating procedure, the problems such as technique is cumbersome.What and for example CN105502455A was provided is " a kind of
The method for preparing ammonia-alum using kaolin ore dressing acid waste water ", it is many using kaolin ore dressing acid waste water and kaolin
Secondary circulation and make to be dissolved in aluminum sulfate therein and reach saturation, then reacted with ammonium sulfate, crystallize twice, obtain ammonia-alum,
The patent application scheme realizes the recycling of ore dressing waste acid water, but equally exists operating procedure is more, and technique is cumbersome etc.
Problem.Therefore aluminium is contained by what the petrochemical industry as mentioned above of solid waste containing aluminium was produced in process of production for exploration simple process
Dead catalyst, which prepares ammonia-alum, has positive effect.
The content of the invention
The task of the present invention is a kind of method that ammonia-alum is prepared by raw material of dead catalyst of offer, and this method can be with letter
Experienced processing step makes the aluminium element in the dead catalyst containing aluminium that petroleum chemical industry is produced be fully used and mitigate oil
The three-protection design cost of chemical industry and using economizes on resources, environmental protection and embody recycling economy spirit.
What the task of the present invention was performed by, a kind of method that ammonia-alum is prepared by raw material of dead catalyst, including
Following steps：
A) prepare and sulfuric acid is added in the thick liquid of aluminum sulfate, the dead catalyst containing aluminium produced in process of production to petrochemical industry and is soaked
Bubble, after immersion terminates in container of the input with agitating device and heater and in unlatching agitating device and the shape of heater
Reaction is stirred under state, stirring reaction is transferred to centrifugal separating device centrifugation, obtains the thick liquid of aluminum sulfate after terminating；
B the thick liquid of alum) is prepared, to step A）Concentrated ammonia liquor is added in the obtained thick liquid of aluminum sulfate, in stirring and heated condition
Lower carry out neutralization reaction, and control agitator mixing speed, control heater heating-up temperature, control neutralization reaction when
Between and control reaction system pH value, obtain the thick liquid of alum；
C thick ammonia-alum filter cake) is prepared, first will be by step B）The obtained thick liquid of alum is transferred to crystallizing pond and carries out crystallization reaction simultaneously
And temperature and the time of control crystallization reaction of control crystallization reaction, then press filtration is carried out, obtain thick ammonia-alum filter cake；
D finished product) is prepared, to by step C）Obtained thick ammonia-alum filter cake elution and Non-leaching degree, through drying, are obtained into
Product ammonia-alum.
In the specific embodiment of the present invention, step A）Described in dead catalyst containing aluminium in aluminium quality %
Content is 10-50%, and the quality % specific concentrations of the sulfuric acid are 25-45%.
In another specific embodiment of the present invention, step A）Described in time for soaking be one week.
In another specific embodiment of the present invention, step A）Described in agitating device mixing speed be 100-
4000 rpm, the time of the stirring reaction is 6-24h, and the heating-up temperature of the heater is 80-120 DEG C.
In another specific embodiment of the present invention, step B）Described in control agitator mixing speed be to stir
Speed control is mixed for 100-4000 rpm；The described heating-up temperature for controlling heater be by heating and temperature control be 80-85 DEG C；
It is described control neutralization reaction time be by time control be 25-35min；The pH value of described control reaction system is by pH value
Control as 1.8-2.2.
In the also specific embodiment of the present invention, step B）Described in concentrated ammonia liquor and the thick liquid of the aluminum sulfate
Mass ratio be 0.05-0.5：1.
In a still more specific embodiment of the invention, the quality % specific concentrations of the concentrated ammonia liquor are 25-28%.
The present invention's and then in a specific embodiment, step C）Described in control crystallization reaction temperature be by
The temperature control of crystallization reaction is 5-15 DEG C；The described time for controlling crystallization reaction is to be by the time control of crystallization reaction
40-60min。
Step D in yet a further embodiment of the present invention）Described in elution be to be eluted with cold water；It is described
Non-leaching degree refer to elution it is colourless to filtrate；Described dries to dry naturally.
In the present invention again and then in a specific embodiment, the temperature of described cold water is 5-15 DEG C.
One of technique effect of technical scheme that the present invention is provided, due to the equipment that processing step is simple and need not be harsh
And technical factor, thus preparation of industrialization requirement can be met；Two, due to raw material be derived from petrochemical industry production process produce
Dead catalyst containing aluminium and the aluminium element in dead catalyst containing aluminium can be made full use of, thus can significantly mitigate petrochemical industry to containing
The three-protection design cost of aluminium dead catalyst, can both economize on resources, environmental protection, and can embody the recycling economy essence turned waste into wealth
God；Three, it is only necessary to thick ammonia-alum filter cake elution i.e. can obtain the preferable finished product ammonia-alum of purity.
Brief description of the drawings
Fig. 1 is the process chart of the inventive method.
Embodiment
Embodiment 1：
The step of flow prepares ammonia-alum by raw material of dead catalyst as shown in Figure 1 is as follows：
A the thick liquid of aluminum sulfate) is prepared, to petrochemical industry in process of production such as the matter of aluminium produced during petroleum catalytic cracking
Measure the sulfuric acid that addition quality % specific concentrations are 25% in the dead catalyst containing aluminium that % contents are 30% and soak one week, specifically, future
From in foregoing industry（Petroleum chemical industry）The input of dead catalyst containing aluminium fill in the fermentation vat of sulfuric acid and flooded with sulfuric acid and contain
Aluminium dead catalyst is advisable, and immersion is pulled out and put into from fermentation vat after terminating and carries（It is furnished with）The appearance of agitating device and heater
Reaction, the stirring speed of agitating device are stirred in device such as reactor and in the state of agitating device and heater is opened
Degree control is 2100rpm, and the time control of stirring reaction is 15h, and the temperature control of heater is 80 DEG C, and stirring reaction terminates
After be transferred to centrifugal separating device centrifugation, obtain the thick liquid of aluminum sulfate；
B the thick liquid of alum) is prepared, in the reaction vessel such as reactor equipped with agitator and heater, to step A）Obtain
The thick liquid of aluminum sulfate in add the concentrated ammonia liquor that quality % specific concentrations are 28%, neutralization reaction is carried out under stirring and heated condition, is stirred
The mixing speed control for mixing device is 100rpm, and the heating and temperature control of heater is 85 DEG C, and the time control of neutralization reaction is
35min, it is 1.8 to control the pH value of reaction system by increasing and decreasing the amount of concentrated ammonia liquor, the mass ratio of concentrated ammonia liquor and the thick liquid of aluminum sulfate
Control for 0.3: 1, to obtain the thick liquid of alum；
C thick ammonia-alum filter cake) is prepared, first will be by step B）The obtained thick liquid of alum is transferred to crystallizing pond and carries out crystallization reaction,
The temperature control of crystallization reaction is 10 DEG C, and the time control of crystallization reaction is 50min, then by filter-pressing device such as filter press press filtration,
Obtain thick ammonia-alum filter cake；
D finished product) is prepared, to by step C）Obtained thick ammonia-alum filter cake is eluted to the colourless journey of filtrate with the cold water of 5 DEG C of temperature
Degree, then through drying naturally, obtain the finished product ammonia-alum that purity is more than 99.5%.
Embodiment 2：
Only by step A）In dead catalyst containing aluminium in the quality % contents of aluminium be changed to 10%, the quality % specific concentrations of sulfuric acid are changed
For 30%, the mixing speed of agitating device is changed to 100rpm, the time of stirring reaction is changed to 6h, be reaction by heating-up temperature
Temperature is changed to 120 DEG C；By step B）In mixing speed be changed to 4000rpm, be that reaction temperature is changed to 80 DEG C by heating-up temperature, will
Reaction time is changed to 35min, the mass ratio of concentrated ammonia liquor and the thick liquid of aluminum sulfate is changed into 0.05: 1, by the quality % of concentrated ammonia liquor than dense
Degree is changed to 27%；By step C）In crystallization reaction temperature be changed to 15 DEG C, the time of crystallization reaction is changed to 40min；By step D）
In cold water temperature be changed to 15 DEG C, remaining is with the description to embodiment 1.
Embodiment 3：
Only by step A）In dead catalyst containing aluminium in the quality % contents of aluminium be changed to 50%, the quality % specific concentrations of sulfuric acid are changed
For 40%, the mixing speed of agitating device is changed to 4000rpm, the time of stirring reaction is changed to 20h, is anti-by heating-up temperature
Temperature is answered to be changed to 110 DEG C；By step B）In mixing speed be changed to 2000rpm, be that reaction temperature is changed to 82 DEG C by heating-up temperature,
Reaction time 32min will be changed to, and the mass ratio of concentrated ammonia liquor and the thick liquid of aluminum sulfate will be changed to 0.5: 1, by the quality % of concentrated ammonia liquor than dense
Degree is changed to 26%；By step C）In crystallization reaction temperature be changed to 12 DEG C, the time of crystallization reaction is changed to 60min；By step D）
In cold water temperature be changed to 10 DEG C, remaining is with the description to embodiment 1.
Embodiment 4：
Only by step A）In dead catalyst containing aluminium in the quality % contents of aluminium be changed to 40%, the quality % specific concentrations of sulfuric acid are changed
For 45%, the mixing speed of agitating device is changed to 3000rpm, the time of stirring reaction is changed to 18h, is anti-by heating-up temperature
Temperature is answered to be changed to 90 DEG C；By step B）In mixing speed be changed to 3000rpm, be that reaction temperature is changed to 85 DEG C by heating-up temperature,
Reaction time 30min will be changed to, and the mass ratio of concentrated ammonia liquor and the thick liquid of aluminum sulfate will be changed to 0.1: 1, by the quality % of concentrated ammonia liquor than dense
Degree is changed to 25%；By step C）In crystallization reaction temperature be changed to 5 DEG C, the time of crystallization reaction is changed to 55min；By step D）
In cold water temperature be changed to 8 DEG C, remaining is with the description to embodiment 1.
Embodiment 5：
Only by step A）In dead catalyst containing aluminium in the quality % contents of aluminium be changed to 20%, the quality % specific concentrations of sulfuric acid are changed
For 35%, the mixing speed of agitating device is changed to 2500rpm, the time of stirring reaction is changed to 24h, is anti-by heating-up temperature
Temperature is answered to be changed to 100 DEG C；By step B）In mixing speed be changed to 1000rpm, be that reaction temperature is changed to 83 DEG C by heating-up temperature,
Reaction time 28min will be changed to, and the mass ratio of concentrated ammonia liquor and the thick liquid of aluminum sulfate will be changed to 0.2: 1, by the quality % of concentrated ammonia liquor than dense
Degree is changed to 28%；By step C）In crystallization reaction temperature be changed to 8 DEG C, the time of crystallization reaction is changed to 45min；By step D）
In cold water temperature be changed to 6 DEG C, remaining is with the description to embodiment 1.
Claims (10)
1. a kind of method that ammonia-alum is prepared by raw material of dead catalyst, it is characterised in that comprise the following steps：
A) prepare and sulfuric acid is added in the thick liquid of aluminum sulfate, the dead catalyst containing aluminium produced in process of production to petrochemical industry and is soaked
Bubble, after immersion terminates in container of the input with agitating device and heater and in unlatching agitating device and the shape of heater
Reaction is stirred under state, stirring reaction is transferred to centrifugal separating device centrifugation, obtains the thick liquid of aluminum sulfate after terminating；
B the thick liquid of alum) is prepared, to step A）Concentrated ammonia liquor is added in the obtained thick liquid of aluminum sulfate, in stirring and heated condition
Lower carry out neutralization reaction, and control agitator mixing speed, control heater heating-up temperature, control neutralization reaction when
Between and control reaction system pH value, obtain the thick liquid of alum；
C thick ammonia-alum filter cake) is prepared, first will be by step B）The obtained thick liquid of alum is transferred to crystallizing pond and carries out crystallization reaction simultaneously
And temperature and the time of control crystallization reaction of control crystallization reaction, then press filtration is carried out, obtain thick ammonia-alum filter cake；
D finished product) is prepared, to by step C）Obtained thick ammonia-alum filter cake elution and Non-leaching degree, through drying, are obtained into
Product ammonia-alum.
2. the method according to claim 1 that ammonia-alum is prepared by raw material of dead catalyst, it is characterised in that step A）In
The quality % contents of aluminium in described dead catalyst containing aluminium are 10-50%, and the quality % specific concentrations of the sulfuric acid are 25-45%.
3. the method according to claim 1 that ammonia-alum is prepared by raw material of dead catalyst, it is characterised in that step A）In
The time of the immersion is one week.
4. the method according to claim 1 that ammonia-alum is prepared by raw material of dead catalyst, it is characterised in that step A）In
The mixing speed of the agitating device is 100-4000 rpm, and the time of the stirring reaction is 6-24h, the heater
Heating-up temperature is 80-120 DEG C.
5. the method according to claim 1 that ammonia-alum is prepared by raw material of dead catalyst, it is characterised in that step B）In
It is described control agitator mixing speed be by mixing speed control be 100-4000 rpm；The heating of described control heater
Temperature be by heating and temperature control be 80-85 DEG C；It is described control neutralization reaction time be by time control be 25-35min；Institute
That states controls the pH value of reaction system to be to control pH value to be 1.8-2.2.
6. the method according to claim 1 that ammonia-alum is prepared by raw material of dead catalyst, it is characterised in that step B）In
The mass ratio of described concentrated ammonia liquor and the thick liquid of the aluminum sulfate is 0.05-0.5：1.
7. the method that ammonia-alum is prepared by raw material of dead catalyst according to claim 1 or 6, it is characterised in that described dense
The quality % specific concentrations of ammoniacal liquor are 25-28%.
8. the method according to claim 1 that ammonia-alum is prepared by raw material of dead catalyst, it is characterised in that step C）In
The described temperature for controlling crystallization reaction be by the temperature control of crystallization reaction be 5-15 DEG C；Described control crystallization reaction when
Between be by the time control of crystallization reaction be 40-60min.
9. the method according to claim 1 that ammonia-alum is prepared by raw material of dead catalyst, it is characterised in that step D）In
The elution is eluted with cold water；Described Non-leaching degree refers to that elution is colourless to filtrate；Described dries to dry in the air naturally
It is dry.
10. the method that ammonia-alum is prepared by raw material of dead catalyst according to claim 1 or 9, it is characterised in that described
Cold water temperature be 5-15 DEG C.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710299511.1A CN107055583A (en) | 2017-05-02 | 2017-05-02 | The method that ammonia-alum is prepared by raw material of dead catalyst |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108328638A (en) * | 2018-03-26 | 2018-07-27 | 武汉理工大学 | A method of preparing alum from FCC dead catalyst |
| CN109455747A (en) * | 2018-11-28 | 2019-03-12 | 陕西好化工科技有限公司 | A method of aluminium oxide is prepared using methanol-to-olefins dead catalyst and containing phosphatic manure |
| CN111573703A (en) * | 2020-05-29 | 2020-08-25 | 贵州锂电新能源科技有限公司 | Method for preparing ammonium alum by using sulfuric acid method lithium extraction leaching solution |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108328638A (en) * | 2018-03-26 | 2018-07-27 | 武汉理工大学 | A method of preparing alum from FCC dead catalyst |
| CN109455747A (en) * | 2018-11-28 | 2019-03-12 | 陕西好化工科技有限公司 | A method of aluminium oxide is prepared using methanol-to-olefins dead catalyst and containing phosphatic manure |
| CN109455747B (en) * | 2018-11-28 | 2021-01-05 | 陕西好一化工科技有限公司 | Method for preparing alumina and phosphorus-containing fertilizer by using methanol-to-olefin waste catalyst |
| CN111573703A (en) * | 2020-05-29 | 2020-08-25 | 贵州锂电新能源科技有限公司 | Method for preparing ammonium alum by using sulfuric acid method lithium extraction leaching solution |
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