CN207376099U - A kind of dead catalyst utilization system - Google Patents
A kind of dead catalyst utilization system Download PDFInfo
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- CN207376099U CN207376099U CN201721478680.3U CN201721478680U CN207376099U CN 207376099 U CN207376099 U CN 207376099U CN 201721478680 U CN201721478680 U CN 201721478680U CN 207376099 U CN207376099 U CN 207376099U
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- rotary kiln
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- centrifuge
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Abstract
The utility model discloses a kind of dead catalyst utilization systems, which is characterized in that including desizer, rotary kiln, four-stage counter-current device, agitator tank I, flame filter press I, settling tank I, flame filter press II, agitator tank II, centrifuge I, ion exchange resin, extraction equipment, it is stripped device, settling tank II, centrifuge II and washing tank.The process costs of the utility model are low, it is environmentally protective, Efficient Cycle utilizes the useful component in residual hydrogenation dead catalyst, obtain the products such as industrial steam, nickel aluminium powder, ammonium metavanadate, high-purity molybdic acid, anhydrous sodium sulfate and distilled water, and 99.9% can be reached with regard to high-purity molybdic acid, purity can be obtained without separating for several times process.
Description
Technical field
The utility model is related to a kind of dead catalyst utilization systems.
Background technology
Dead catalyst is generally acknowledged environmental contaminants, into environment before must be converted to innocuous substance.Residual hydrogenation, which gives up, urges
Containing rare metals such as molybdenum vanadium in agent, there is very high economic value.But since the chemistry common of molybdenum and vanadium is more, separation
It is more difficult.
At present, existing separating technology includes：1) using sodium carbonate roasting technique, the auxiliary material of addition is Na2CO3,
NaOH, NaCl or Na2SO4 etc., product of roasting is leached with hot water, and the molybdenum and vanadium in solution enter solution with soluble sodium salt form
In, afterwards, carry out ammonium salt precipitation and the extraction of molybdenum；2) use Ore Leaching or directly oxidation reinforced dose of leaching of use acid, molybdenum, vanadium
And nickel, iron, aluminium and the cobalt in catalyst enter solution, high temperature and pressure alkali leaching processing dead catalyst, alkali immersion liquid acid adding is handled
To the acid solution containing molybdenum and vanadium, molybdenum and vanadium separation method have extraction separation method, sulfide precipitation partition method and ammonium in acid solution
Salt separation by precipitation.But the molybdenum that is obtained by current separating technology, the purity of vanadium is not high, it is necessary to by separating for several times mistake
Cheng Caineng obtains the molybdenum and vanadium of high-purity, with high costs.
It is similary to have also containing other components in residual hydrogenation dead catalyst in addition to containing the rare metals such as molybdenum and vanadium
There is economic value.It is of far-reaching significance for the relatively low China of per capita resources owning rate.Therefore, a kind of new useless catalysis is developed
Agent utilization system, to recycling with definite meaning for residual hydrogenation dead catalyst.
Utility model content
According to the technical issues of set forth above, and provide a kind of dead catalyst utilization system.The utility model uses
Technological means it is as follows：
A kind of dead catalyst utilization system, the desizer including being used for residual hydrogenation dead catalyst deoiling treatment are right
The de-oiling material obtained through the desizer carries out the rotary kiln of sodium roasting, and the sodium material obtained through the rotary kiln is soaked
Go out the four-stage counter-current device of reaction, for the molybdenum vanadium liquid and pure cerium hydroxide sodium or pure cerium hydroxide obtained through the four-stage counter-current device
The agitator tank I of calcium reaction, to the flame filter press I that the liquid obtained through the agitator tank I cleans, to through the sheet frame mistake
The net liquid that filter I obtains carries out the settling tank I of precipitation reaction, and the solidliquid mixture obtained through the settling tank I is filtered
Flame filter press II, for obtained through the flame filter press II solid particle and water mixing agitator tank II, to through institute
State the centrifuge I that the solidliquid mixture that agitator tank II obtains carries out separation of solid and liquid, the filter to being obtained through the flame filter press II
The ion exchange resin that liquid and the mother liquor I obtained through the centrifuge I are filtered, to what is obtained through the ion exchange resin
The extraction equipment that liquid containing molybdenum is extracted, the back extraction being stripped to the saturated organic phase containing molybdenum obtained through the extraction equipment
Device is taken, for the sodium molybdate aqueous solution and the settling tank II of strong sulfuric acid response obtained through the back extraction device, to described in warp
Solidliquid mixture that settling tank II obtains carry out separation of solid and liquid centrifuge II and to through the molybdic acid that the centrifuge II obtains into
The washing tank of row washing.
The desizer has the industrial steam collecting pipe being connected with industrial steam collection device.
The rotary kiln includes cylinder of rotary kiln and burner；The burner is arranged at cylinder of rotary kiln outlet
End；
The cylinder of rotary kiln arrival end is connected with the discharge port of the desizer；The cylinder of rotary kiln port of export bulb
It is connected with ball head connecting piece；The ball head connecting piece is provided centrally with perforative through hole；The burner is fired including natural gas
Burner, combustion tube, burner, burner arm and moving cart；Described combustion tube one end is connected with neat gas burner outlet,
The through hole of the other end through ball head connecting piece is extend into inside cylinder of rotary kiln, is inserted into the end of tube body inside cylinder of rotary kiln
It is threaded with burner；The burner arm is hydraulically extensible cylinder, and moving cart upper end is fixed in bottom；The natural gas
It is hinged at the top of the telescopic rod of burner base and burner arm；Gases at high pressure injection device is provided in the moving cart,
The output pipe of gases at high pressure injection device is connected with combustion tube, and the output pipe of gases at high pressure injection device is band control valve
Pipeline；Control panel is provided in the moving cart, and control panel integrates moving cart control button, neat gas burner
Control button, gases at high pressure injection device control button and burner arm extension and contraction control button；The cylinder of rotary kiln goes out
Mouth end is additionally provided with combustion-supporting hot wind injection device；
The cylinder of rotary kiln port of export is connected with the feed inlet of the four-stage counter-current device.
A kind of dead catalyst utilization system, which further includes, steams the raffinate obtained through the extraction equipment
The condenser that the triple effect evaporator of crystallization and the steam to being obtained through the triple effect evaporator are condensed is sent out, through the centrifuge
II obtained mother liquor II enters the ion exchange resin together with mother liquor I.
Residual hydrogenation dead catalyst is comprehensively utilized using a kind of dead catalyst utilization system described above
Method have following steps：
S1, residual hydrogenation dead catalyst carry out deoiling treatment by desizer, obtain industrial steam and de-oiling material；
S2, de-oiling material and pure cerium hydroxide sodium are mixed, and sodium roasting processing is carried out by rotary kiln, obtain sodium material；
S3, sodium material carry out Leach reaction by four-stage counter-current device, isolate nickel aluminium powder and molybdenum vanadium liquid；
S4, pure cerium hydroxide sodium or pure cerium hydroxide calcium are added in into molybdenum vanadium liquid, and pours into agitator tank I and be mixed, afterwards,
Calcium, aluminium, silicon, phosphorus are removed by flame filter press I, obtain net liquid；
S5, ammonium sulfate is added in into net liquid, it is 8.3~9.0 to adjust pH value, pours into settling tank I and is mixed afterwards, it
Afterwards, solid particle and filtrate being obtained by filtration by flame filter press II, solid particle and water are mixed in agitator tank II, it
Afterwards, separated by centrifuge I, obtain ammonium metavanadate and mother liquor I, filtrate and mother liquor mixing filter out filter by ion exchange resin
Remaining vanadium in liquid and mother liquor, obtains liquid containing molybdenum；
S6, liquid containing molybdenum are poured into the extraction equipment for having been loaded with pure water and organic extractant, and the density of organic extractant is less than
The density of pure water, afterwards, stirring, molybdenum are entered in organic extractant, obtain saturated organic phase containing molybdenum and raffinate, the raffinate
Liquid obtains anhydrous sodium sulfate and steam by triple effect evaporator evaporative crystallization, and the steam is condensed into distilled water by condenser；
S7, saturated organic phase containing molybdenum, which pour into, to be had been loaded in the back extraction device of sodium hydrate aqueous solution, and stirring, molybdenum enters hydrogen
Aqueous solution of sodium oxide is reacted with sodium hydroxide, obtains sodium molybdate aqueous solution；
S8, sodium molybdate aqueous solution pour into settling tank II, then add in the concentrated sulfuric acid into settling tank II, are mixed, afterwards, from
Scheming II separates, and obtains molybdic acid and mother liquor II, and mother liquor II is mixed with the mother liquor I in step S5, completes subsequent step；
S9, molybdic acid are washed by washing tank, obtain high-purity molybdic acid.
The process costs of the utility model are low, environmentally protective, and Efficient Cycle utilizes useful in residual hydrogenation dead catalyst
Ingredient obtains the products such as industrial steam, nickel aluminium powder, ammonium metavanadate, high-purity molybdic acid, anhydrous sodium sulfate and distilled water, and need not
Separating for several times process can reach 99.9% with regard to that can obtain high-purity molybdic acid, purity.
The utility model can be widely popularized in the fields of grade that recycle of chemical waste for the foregoing reasons.
Description of the drawings
It in order to illustrate the embodiment of the utility model or the technical proposal in the existing technology more clearly, below will be to embodiment
Or attached drawing needed to be used in the description of the prior art does simply to introduce, it should be apparent that, the accompanying drawings in the following description is
Some embodiments of the utility model, for those of ordinary skill in the art, in the premise of not making the creative labor property
Under, it can also be obtained according to these attached drawings other attached drawings.
Fig. 1 is a kind of connection diagram of dead catalyst utilization system in specific embodiment of the present utility model.
Fig. 2 be in specific embodiment of the present utility model four-stage counter-current device material stream to schematic diagram.
Fig. 3 is the structure diagram of rotary kiln in specific embodiment of the present utility model.
Specific embodiment
It is new below in conjunction with this practicality to make the purpose, technical scheme and advantage of the utility model embodiment clearer
Attached drawing in type embodiment, the technical scheme in the utility model embodiment is clearly and completely described, it is clear that is retouched
The embodiment stated is the utility model part of the embodiment, instead of all the embodiments.Based on the implementation in the utility model
Example, those of ordinary skill in the art's all other embodiments obtained without making creative work, belongs to
The scope of the utility model protection.
As shown in FIG. 1 to 3, a kind of dead catalyst utilization system, including being used for residual hydrogenation dead catalyst de-oiling
The desizer 1 of processing carries out the de-oiling material obtained through the desizer 1 in the rotary kiln 2 of sodium roasting, to through the rotary kiln
2 obtained sodium material carry out the four-stage counter-current device 3 of Leach reaction, for the molybdenum vanadium liquid obtained through the four-stage counter-current device 3
The agitator tank I 4 reacted with pure cerium hydroxide sodium or pure cerium hydroxide calcium, the plate to clean to the liquid obtained through the agitator tank I 4
Frame filter I 5 carries out the net liquid obtained through the flame filter press I 5 the settling tank I 6 of precipitation reaction, to through the precipitation
The flame filter press II 7 that the solidliquid mixture that tank I 6 obtains is filtered, for the solid obtained through the flame filter press II 7
Particle and the agitator tank II 8 of water mixing carry out the solidliquid mixture obtained through the agitator tank II 8 in the centrifuge of separation of solid and liquid
I 9, the ion that the filtrate obtained through the flame filter press II 7 and the mother liquor I obtained through the centrifuge I 9 are filtered is handed over
Resin 10 is changed, to the extraction equipment 11 that the liquid containing molybdenum obtained through the ion exchange resin 10 is extracted, to through the extraction
The back extraction device 12 that the saturated organic phase containing molybdenum that device 11 obtains is stripped, for being obtained through the back extraction device 12
Sodium molybdate aqueous solution and strong sulfuric acid response settling tank II 13, the solidliquid mixture that is obtained through the settling tank II 13 is carried out
The washing tank 15 that the centrifuge II 14 of separation of solid and liquid and the molybdic acid to being obtained through the centrifuge II 14 are washed.
The desizer 1 has the industrial steam collecting pipe being connected with industrial steam collection device.
The rotary kiln 2 includes cylinder of rotary kiln 2.1 and burner；The burner 2.2 is arranged at rotary kiln cylinder
2.1 port of export of body；
2.1 arrival end of cylinder of rotary kiln is connected with the discharge port of the desizer 1；The cylinder of rotary kiln 2.1 goes out
Mouth end bulb is connected with ball head connecting piece 2.11；The ball head connecting piece 2.11 is provided centrally with perforative through hole；The burning
Device 2.2 includes neat gas burner 2.21, combustion tube 2.22, burner 2.23, burner arm 2.24 and moving cart
2.25；Described 2.22 one end of combustion tube is connected with the outlet of neat gas burner 2.21, and the other end passes through ball head connecting piece 2.11
Through hole is extend into inside cylinder of rotary kiln 2.1, and the end thread for being inserted into 2.1 inside tube body of cylinder of rotary kiln is connected with burner
2.23；The burner arm 2.24 is hydraulically extensible cylinder, and 2.25 upper end of moving cart is fixed in bottom；The combustion of natural gas
2.21 bottom of device at the top of the telescopic rod of burner arm 2.24 with being hinged；Gases at high pressure note is provided in the moving cart 2.25
Enter device 2.26, the output pipe of gases at high pressure injection device 2.26 is connected with combustion tube 2.22, and gases at high pressure injection device
2.26 output pipe is band control valve pipeline；Control panel 2.3, and control panel are provided in the moving cart 2.25
2.3 2.25 control buttons of integrated moving cart, 2.21 control button of neat gas burner, gases at high pressure injection device 2.26 control
2.24 extension and contraction control button of button and burner arm；2.1 port of export of cylinder of rotary kiln is additionally provided with combustion-supporting hot wind note
Enter device 2.4；
2.1 port of export of cylinder of rotary kiln is connected with the feed inlet of the four-stage counter-current device 3.
A kind of dead catalyst utilization system, which further includes, carries out the raffinate obtained through the extraction equipment 11
The condenser 17 that the triple effect evaporator 16 of evaporative crystallization and the steam to being obtained through the triple effect evaporator 16 are condensed, through institute
It states the mother liquor II that centrifuge II 14 obtains and enters the ion exchange resin 10 together with mother liquor I.
As shown in Fig. 2, 3 substance of the four-stage counter-current device flow direction sequentially enters level-one backflow device, two level for sodium material
Backflow device, three-level backflow device and four-stage counter-current device, water sequentially enter four-stage counter-current device, three-level backflow device, two level
Backflow device and the cleaning of level-one backflow device are inverse into four-stage counter-current device, three-level backflow device, two level backflow device and level-one
Flow the sodium material in device.
Finally it should be noted that：Various embodiments above is only to illustrate the technical solution of the utility model rather than it is limited
System；Although the utility model is described in detail with reference to foregoing embodiments, those of ordinary skill in the art should
Understand：It can still modify to the technical solution recorded in foregoing embodiments either to which part or whole
Technical characteristic carries out equivalent substitution；And these modifications or replacement, the essence of appropriate technical solution is not made to depart from this practicality newly
The scope of each embodiment technical solution of type.
Claims (4)
1. a kind of dead catalyst utilization system, which is characterized in that including being used for residual hydrogenation dead catalyst deoiling treatment
Desizer carries out the de-oiling material obtained through the desizer in the rotary kiln of sodium roasting, to the sodium obtained through the rotary kiln
Material carries out the four-stage counter-current device of Leach reaction, for the molybdenum vanadium liquid and pure cerium hydroxide sodium obtained through the four-stage counter-current device
Or the agitator tank I of pure cerium hydroxide calcium reaction, to the flame filter press I that the liquid obtained through the agitator tank I cleans, to warp
The net liquid that the flame filter press I obtains carries out the settling tank I of precipitation reaction, and the solid-liquid obtained through the settling tank I is mixed
The flame filter press II that object is filtered, for the agitator tank of solid particle and the water mixing obtained through the flame filter press II
II, the centrifuge I of separation of solid and liquid is carried out to the solidliquid mixture obtained through the agitator tank II, to through the flame filter press II
The ion exchange resin that obtained filtrate and the mother liquor I obtained through the centrifuge I are filtered, to through the amberlite
The extraction equipment that the liquid containing molybdenum that fat obtains is extracted is stripped the saturated organic phase containing molybdenum obtained through the extraction equipment
The back extraction device taken, for the settling tank II through the obtained sodium molybdate aqueous solution of back extraction device and strong sulfuric acid response,
The centrifuge II of separation of solid and liquid is carried out and to being obtained through the centrifuge II to the solidliquid mixture obtained through the settling tank II
The washing tank that is washed of molybdic acid.
2. a kind of dead catalyst utilization system according to claim 1, it is characterised in that：The desizer have with
The industrial steam collecting pipe of industrial steam collection device connection.
3. a kind of dead catalyst utilization system according to claim 1, it is characterised in that：The rotary kiln includes back
Rotary kiln cylinder and burner；The burner is arranged at the cylinder of rotary kiln port of export；The cylinder of rotary kiln arrival end with
The discharge port connection of the desizer；The cylinder of rotary kiln port of export bulb is connected with ball head connecting piece；The bulb connection
Part is provided centrally with perforative through hole；The burner includes neat gas burner, combustion tube, burner, burner arm
And moving cart；Described combustion tube one end is connected with neat gas burner outlet, and the through hole of the other end through ball head connecting piece is stretched
Enter to inside cylinder of rotary kiln, the end thread for being inserted into tube body inside cylinder of rotary kiln is connected with burner；The burner
Stent is hydraulically extensible cylinder, and moving cart upper end is fixed in bottom；The neat gas burner bottom and burner arm are stretched
It is hinged at the top of contracting bar；Gases at high pressure injection device, the output pipe of gases at high pressure injection device are provided in the moving cart
It is connected with combustion tube, and the output pipe of gases at high pressure injection device is band control valve pipeline；It is provided in the moving cart
Control panel, and control panel integrates moving cart control button, neat gas burner control button, gases at high pressure injection device
Control button and burner arm extension and contraction control button；The cylinder of rotary kiln port of export is additionally provided with combustion-supporting hot wind injection dress
It puts；
The cylinder of rotary kiln port of export is connected with the feed inlet of the four-stage counter-current device.
4. a kind of dead catalyst utilization system according to claim 1, it is characterised in that：A kind of dead catalyst
Utilization system further includes triple effect evaporator that crystallization is evaporated to the raffinate obtained through the extraction equipment and to warp
The condenser that the steam that the triple effect evaporator obtains is condensed, the mother liquor II obtained through the centrifuge II and mother liquor I 1
It is same to enter the ion exchange resin.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201721478680.3U CN207376099U (en) | 2017-11-08 | 2017-11-08 | A kind of dead catalyst utilization system |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201721478680.3U CN207376099U (en) | 2017-11-08 | 2017-11-08 | A kind of dead catalyst utilization system |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111014247A (en) * | 2019-12-24 | 2020-04-17 | 青岛大学 | High-value utilization process of heavy oil suspension bed hydrogenation solid waste |
| CN112111295A (en) * | 2020-09-23 | 2020-12-22 | 铁岭贵鑫环保科技发展有限公司 | Low-temperature pyrolysis method and system for residual oil hydrogenation waste catalyst |
| CN114107702A (en) * | 2021-12-03 | 2022-03-01 | 万循材料科技有限公司 | Cleaning treatment method of waste petroleum catalyst |
-
2017
- 2017-11-08 CN CN201721478680.3U patent/CN207376099U/en active Active
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111014247A (en) * | 2019-12-24 | 2020-04-17 | 青岛大学 | High-value utilization process of heavy oil suspension bed hydrogenation solid waste |
| CN111014247B (en) * | 2019-12-24 | 2021-04-02 | 青岛大学 | High-value utilization process of heavy oil suspension bed hydrogenation solid waste |
| CN112111295A (en) * | 2020-09-23 | 2020-12-22 | 铁岭贵鑫环保科技发展有限公司 | Low-temperature pyrolysis method and system for residual oil hydrogenation waste catalyst |
| CN112111295B (en) * | 2020-09-23 | 2022-03-29 | 铁岭贵鑫环保科技发展有限公司 | Low-temperature pyrolysis method and system for residual oil hydrogenation waste catalyst |
| CN114107702A (en) * | 2021-12-03 | 2022-03-01 | 万循材料科技有限公司 | Cleaning treatment method of waste petroleum catalyst |
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