CN106916921B - A method of deoxidier is prepared using waste oil fat hydrogenation catalyst - Google Patents
A method of deoxidier is prepared using waste oil fat hydrogenation catalyst Download PDFInfo
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- CN106916921B CN106916921B CN201510996594.0A CN201510996594A CN106916921B CN 106916921 B CN106916921 B CN 106916921B CN 201510996594 A CN201510996594 A CN 201510996594A CN 106916921 B CN106916921 B CN 106916921B
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- hydrogenation catalyst
- waste oil
- oil fat
- deoxidier
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21C—PROCESSING OF PIG-IRON, e.g. REFINING, MANUFACTURE OF WROUGHT-IRON OR STEEL; TREATMENT IN MOLTEN STATE OF FERROUS ALLOYS
- C21C7/00—Treating molten ferrous alloys, e.g. steel, not covered by groups C21C1/00 - C21C5/00
- C21C7/04—Removing impurities by adding a treating agent
- C21C7/06—Deoxidising, e.g. killing
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21C—PROCESSING OF PIG-IRON, e.g. REFINING, MANUFACTURE OF WROUGHT-IRON OR STEEL; TREATMENT IN MOLTEN STATE OF FERROUS ALLOYS
- C21C2250/00—Specific additives; Means for adding material different from burners or lances
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
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- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
- Fats And Perfumes (AREA)
- Catalysts (AREA)
Abstract
The present invention relates to a kind of methods that recycling waste oil fat hydrogenation catalyst prepares deoxidier.This method uses the carbonate mixture, a small amount of binder and the deionized water that are prepared by waste oil fat hydrogenation catalyst as raw material, is uniformly mixed according to a certain percentage, is prepared into deoxidier after banded extruder forms.Compared with prior art, the present invention is using waste oil fat hydrogenation catalyst as raw material, provide a kind of method for preparing deoxidier of new waste oil fat hydrogenation catalyst, not only realize the recycling of waste oil fat hydrogenation catalyst, and simplify operating procedure, production cost is greatly reduced, while product deoxidier can be made to reach high-precision deoxidation requirement.
Description
Technical field
The present invention relates to it is a kind of roasted using waste oil fat hydrogenation catalyst, acid it is molten after alkaline chemical precipitation, washing, drying after
Add binder and water, the method for extruded moulding deoxidier.
Background technique
Oil hydrogenation is that lower melting-point liquid fat is added hydrogen, is converted it into molten under the action of nickel-base catalyst
The higher solid-state fixed oil of point.The sector generates a large amount of dead catalyst, investigation discovery, domestic more oil hydrogenation devices every year
The dead catalyst generated after HYDROGENATION OF OILS AND FATS is taken as industrial waste accumulation in the factory, not only polluted environment, but also waste resource.
The processing method of waste oil fat hydrogenation catalyst mainly has sour cooking method, and incineration method is saponified sour cooking method and organic extraction
Deng.Xu Delin etc. uses sour cooking method to adding hydrogen dead catalyst to regenerate, since the grease after acid is molten can only be separated by extraction,
Separation not enough will lead to completely also contains grease in sulfate.
The more deoxidier of current application is iron series and manganese systems, and maximum deoxidizing capacity can only achieve ppm grades, and nickel
The maximum deoxidizing capacity of base deoxidier can reach ppb grades, and oxygen capacity is up to 20ml/g.It is found through literature survey, Ni-based deoxidation
The nickel mass fraction of agent is between 20%~43%, and nickel mass fraction exists in the composition of Ni-based waste oil fat hydrogenation catalyst
Between 25%-78%, the composition of chemical deoxidier is complied fully with, therefore, waste oil fat hydrogenation catalyst is passed through into a series of processing
Afterwards as deoxidier carry out using, can make waste oil fat hydrogenation catalyst recycled and make preparation deoxidier reach
To higher oxygen capacity and deoxidation precision.
Summary of the invention
The present invention be it is a kind of roasted using waste oil fat hydrogenation catalyst, acid it is molten after alkaline chemical precipitation, washing, drying after again
Binder and water is added, extruded moulding is the method for deoxidier.This method the specific process is as follows:
(1) waste oil fat hydrogenation catalyst is subjected to elemental analysis, the main content for measuring wherein Ni, Mg, Si.And according to it
In Ni content judge whether the waste oil fat hydrogenation catalyst raw material can reach deoxidier service index after processing.
(2) by waste oil fat hydrogenation catalyst after 300~600 DEG C of roasting temperatures, after being made into the concentration of 20~50wt%
Be added volume fraction 10%~50% acid carry out acid it is molten, add a certain amount of alkali carry out neutralize to pH value be 10~12 after,
After washing, filtering, drying dry powder, be added after binder and water mixed, by banded extruder drying after forming, 300~
Deoxidier is prepared into after roasting at 450 DEG C.
The acid is sulfuric acid, hydrochloric acid.
The alkali is sodium carbonate, potassium carbonate, sodium bicarbonate.
The binder is kaolin, high silicon macropore boehmite, silica solution, cement, white carbon black, low silicon macropore are quasi-
Boehmite, sesbania powder, attapulgite, Na base bentonite, calcium-base bentonite etc. are one such.Content is the dry powder after drying
1~30wt%.
When addition binder and after mixing, the water being added is 40~60wt% of the dry powder after drying.
The advantage of the invention is that the present invention provides a kind of new waste oil using waste oil fat hydrogenation catalyst as raw material
The method of comprehensive utilization of fat hydrogenation catalyst, not only realizes the recycling of waste oil fat hydrogenation catalyst, but also simplifies operation
Technique greatly reduces production cost, while product deoxidier can be made to have reached hyperoxia appearance, the requirement of high deoxidation precision: strong
Degree can reach 100N/cm, and deoxidation capacity reaches as high as 23g/ml, and deoxidation precision can reach 10ppb or less.
Detailed description of the invention
Fig. 1 is embodiment 12 and 13, the XRD spectra under 350 DEG C and 400 DEG C of maturing temperatures.
1 waste oil fat hydrogenation catalyst of table be fired after XRF analysis result
| Title | Content % |
| NiO | 83.23 |
| SiO2 | 11.66 |
| MgO | 3.59 |
| SO3 | 0.69 |
| CoO | 0.38 |
| Al2O3 | 0.09 |
| CaO | 0.07 |
| P2O5 | 0.05 |
| Fe2O3 | 0.02 |
| TiO2 | 71ppm |
| Cl | 0.07 |
The sample carries out inductively-coupled plasma spectrometer (ICP-AES) elemental analysis, and the results are shown in Table 2:
2 waste oil fat hydrogenation catalyst of table be fired after ICP elemental analysis result
| Title | Content |
| Nickel (Ni) | 41.92% |
| Mg | 1.337% |
| Si | 4.799% |
| Co | 1961mg/kg |
| Ca | 237mg/kg |
| Cu | * is not detected |
| Fe | 13mg/kg |
| Pb | * is not detected |
| Sr | 4mg/kg |
| Zn | 18mg/kg |
| Al | 378mg/kg |
| Na | 357mg/kg |
| K | 25mg/kg |
| P | 96mg/kg |
(deoxygenation conditions are that temperature is 400 degree to sample strength, oxygen capacity and deoxidation precision prepared by the different embodiments of table 3
Under, unstripped gas oxygen content is 2013.4ppm, air speed 2000h-1)
Specific embodiment
Give further below by specific embodiment using by the method that waste oil fat hydrogenation catalyst prepares deoxidier
Illustrate, but the present invention is not therefore subject to any restriction.The waste oil fat hydrogenation catalyst (Tables 1 and 2) as described below used
It is middle through ICP detection nickel mass fraction be 41.92%.
Embodiment 1
By waste oil fat hydrogenation catalyst at 400 DEG C after roasting temperature 3 hours, be made into after the concentration of mass concentration 30% plus
Entering the sulfuric acid of mass fraction 30%, to carry out acid molten to PH=2, sodium carbonate is added neutralize to pH value be 10 after, washing, mistake
Dry powder is obtained after filter, drying, after the water of kaolin and dry powder quality 50% that dry powder quality 15% is added is mixed, by extrusion
Machine drying after forming is prepared into deoxidier after roasting 3 hours at 350 DEG C.
Embodiment 2
After roasting temperature 3 hours, matter is added after being made into 10% mass concentration at 350 DEG C in waste oil fat hydrogenation catalyst
Measure score 50% sulfuric acid carry out acid it is molten, add potassium carbonate carry out neutralize to pH value be 10 after, washing, filtering, drying after
Dry powder dries after banded extruder forms after the water of kaolin and dry powder quality 50% that dry powder quality 15% is added is mixed
It is dry, roasted 3 hours at 350 DEG C after be prepared into deoxidier.
Embodiment 3
Waste oil fat hydrogenation catalyst after roasting temperature 2.5 hours, is added at 350 DEG C after being made into 20% mass concentration
It is molten that the sulfuric acid of mass fraction 40% carries out acid, sodium carbonate is added neutralize to pH value be 11 after, after washing, filtering, drying
Dry powder is obtained, after the water of high silicon macropore macropore boehmite and dry powder quality 50% that dry powder quality 15% is added is mixed,
Deoxidier is prepared within 3.5 hours after roasting by banded extruder drying after forming, at 350 DEG C.
Embodiment 4
After roasting temperature 2 hours, matter is added after being made into 10% mass concentration at 350 DEG C in waste oil fat hydrogenation catalyst
Measure score 18% hydrochloric acid carry out acid it is molten, add sodium carbonate carry out neutralize to pH value be 11 after, washing, filtering, drying after
Dry powder, be added dry powder amount 15% cement and dry powder quality 50% water mixed after, by banded extruder drying after forming,
Deoxidier is prepared into after roasting 2 hours at 350 DEG C.
Embodiment 5
After roasting temperature 3 hours, body is added after being made into 30% mass concentration at 400 DEG C in waste oil fat hydrogenation catalyst
It is molten that the hydrochloric acid of fraction 10% carries out acid, sodium carbonate is added neutralize to pH value be 11 after, after washing, filtering, drying
Dry powder, be added dry powder amount 15% kaolin and dry powder quality 50% water mixed after, by banded extruder drying after forming,
Deoxidier is prepared into after roasting 4 hours at 350 DEG C.
Embodiment 6
After roasting temperature 4 hours, matter is added after being made into 30% mass concentration at 500 DEG C in waste oil fat hydrogenation catalyst
Measure score 10% hydrochloric acid carry out acid it is molten, add sodium carbonate carry out neutralize to pH value be 11 after, washing, filtering, drying after
Dry powder, be added dry powder amount 2% silica solution and dry powder quality 40% water mixed after, by banded extruder drying after forming,
Deoxidier is prepared into after roasting 3 hours at 350 DEG C.
Embodiment 7
After roasting temperature 2 hours, matter is added after being made into 40% mass concentration at 600 DEG C in waste oil fat hydrogenation catalyst
Measure score 5% hydrochloric acid carry out acid it is molten, add sodium carbonate carry out neutralize to pH value be 11 after, washing, filtering, drying after must do
Powder, be added dry powder amount 5% kaolin and dry powder quality 40% water mixed after, by banded extruder drying after forming,
Deoxidier is prepared into after roasting 3 hours at 350 DEG C.
Embodiment 8
After roasting temperature 3 hours, matter is added after being made into 50% mass concentration at 600 DEG C in waste oil fat hydrogenation catalyst
Measure score 10% sulfuric acid carry out acid it is molten, add sodium carbonate carry out neutralize to pH value be 11 after, washing, filtering, drying after
Dry powder, be added dry powder amount 15% kaolin and dry powder quality 50% water mixed after, by banded extruder drying after forming,
Deoxidier is prepared into after roasting 2 hours at 450 DEG C.
Embodiment 9
After roasting temperature 3 hours, matter is added after being made into 30% mass concentration at 500 DEG C in waste oil fat hydrogenation catalyst
Measure score 12% hydrochloric acid carry out acid it is molten, add a certain amount of sodium carbonate carry out neutralize to pH value be 11 after, washing, filtering,
After drying dry powder, be added dry powder amount 15% white carbon black and dry powder quality 60% water mixed after, by banded extruder at
After type dry, roasted 2 hours at 450 DEG C after be prepared into deoxidier.
Embodiment 10
After roasting temperature 3 hours, matter is added after being made into 30% mass concentration at 500 DEG C in waste oil fat hydrogenation catalyst
Measure score 12% hydrochloric acid carry out acid it is molten, add a certain amount of sodium carbonate carry out neutralize to pH value be 11 after, washing, filtering,
Dry powder is obtained after drying, after the water of low silicon macropore boehmite and dry powder quality 50% that dry powder amount 15% is added is mixed,
By banded extruder drying after forming, roasted 3 hours at 400 DEG C after be prepared into deoxidier.
Embodiment 11
After roasting temperature 3 hours, matter is added after being made into 30% mass concentration at 500 DEG C in waste oil fat hydrogenation catalyst
Measure score 12% hydrochloric acid carry out acid it is molten, add sodium carbonate carry out neutralize to pH value be 11 after, washing, filtering, drying after
Dry powder, be added dry powder amount 15% sesbania gum and dry powder quality 50% water mixed after, by banded extruder drying after forming,
Deoxidier is prepared into after roasting 3 hours at 450 DEG C.
Embodiment 12
After roasting temperature 3 hours, matter is added after being made into 30% mass concentration at 400 DEG C in waste oil fat hydrogenation catalyst
Measure score 30% sulfuric acid carry out acid it is molten, add sodium carbonate carry out neutralize to pH value be 10 after, washing, filtering, drying after
Dry powder dries after banded extruder forms after the water of attapulgite and dry powder quality 50% that dry powder amount 15% is added is mixed
It is dry, roasted 3 hours at 400 DEG C after be prepared into deoxidier.
Embodiment 13
After roasting temperature 3 hours, matter is added after being made into 30% mass concentration at 400 DEG C in waste oil fat hydrogenation catalyst
Measure score 30% sulfuric acid carry out acid it is molten, add sodium carbonate carry out neutralize to pH value be 10 after, washing, filtering, drying after
Dry powder, after the water of sodium bentonite and dry powder quality 50% that dry powder amount 15% is added is mixed, after banded extruder forms
Drying is prepared into deoxidier after roasting 3 hours at 350 DEG C.
Embodiment 14
After roasting temperature 3 hours, matter is added after being made into 30% mass concentration at 400 DEG C in waste oil fat hydrogenation catalyst
Measure score 30% sulfuric acid carry out acid it is molten, add sodium carbonate carry out neutralize to pH value be 10 after, washing, filtering, drying after
Dry powder, after the water of sodium bentonite and dry powder quality 50% that dry powder amount 15% is added is mixed, after banded extruder forms
Drying is prepared into deoxidier after roasting 3 hours at 350 DEG C.
Embodiment 15
After roasting temperature 3 hours, matter is added after being made into 30% mass concentration at 400 DEG C in waste oil fat hydrogenation catalyst
Measure score 30% sulfuric acid carry out acid it is molten, add sodium carbonate carry out neutralize to pH value be 10 after, washing, filtering, drying after
Dry powder, after the water of sodium bentonite and dry powder quality 60% that dry powder amount 30% is added is mixed, after banded extruder forms
Drying is prepared into deoxidier after roasting 3 hours at 400 DEG C.
Compared with prior art, the present invention is a kind of new using providing using waste oil fat hydrogenation catalyst as raw material
The method of comprehensive utilization of waste oil fat hydrogenation catalyst, not only realizes the recycling of waste oil fat hydrogenation catalyst, but also simplifies
Operating procedure greatly reduces production cost, while product deoxidier can be made to have reached hyperoxia appearance, and high deoxidation precision is wanted
Ask: intensity can reach 100N/cm, and deoxidation capacity reaches as high as 23g/ml, and deoxidation precision can reach 10ppb or less.
Claims (7)
1. a kind of method that the recycling of waste oil fat hydrogenation catalyst prepares deoxidier, it is characterised in that:
By the waste oil fat hydrogenation catalyst containing nickel after 300 ~ 600 DEG C of roastings, waste oil fat hydrogenation catalyst and water after roasting
It is configured to the mixed liquor that catalyst quality percentage is 20% ~ 50%, acid is added into mixed liquor and carries out sour molten, the addition of the acid
Amount be subject to acid it is molten after pH of mixed reach 2 ~ 3；Then alkali is added into mixed liquor again neutralize to liquid pH=10 ~ 12,
Dry powder is obtained after washing, filtering, drying；Be added in dry powder after binder and water mixed, by banded extruder drying after forming,
300 ~ 450 DEG C are prepared into deoxidier after roasting temperature 2.5-4 hours；The acid is sulfuric acid or hydrochloric acid, and the sulfuric acid added is
The aqueous sulfuric acid that sulfuric acid mass percent is 10% ~ 50%, the hydrochloric acid added are the hydrochloric acid that hydrochloric acid mass percent is 8% ~ 18%
Aqueous solution；The molar ratio of acid and waste oil fat hydrogenation catalyst is 1:1.2 ~ 1.5.
2. according to the method described in claim 1, it is characterized by: the waste oil fat hydrogenation catalyst containing nickel is for oil
Nickel-base hydrogenation catalyst after rouge hydrogenation reaction, main active component are nickel, the matter of nickel element in waste oil fat hydrogenation catalyst
Amount percentage is 25%-78%.
3. according to the method described in claim 2, it is characterized by: in waste oil fat hydrogenation catalyst also containing magnesium, silicon, sulphur, cobalt,
Aluminium, calcium, phosphorus, iron or titanium.
4. according to the method described in claim 1, it is characterized by: waste oil fat hydrogenation catalyst calcining time is 2-4 hours.
5. according to the method described in claim 1, it is characterized by: the alkali is sodium carbonate, in potassium carbonate, sodium bicarbonate
It is one or two or more kinds of.
6. according to the method described in claim 1, it is characterized by: the binder is kaolin, high silicon macropore intends thin water
Aluminium stone, silica solution, cement, white carbon black, sesbania powder, attapulgite, Na base bentonite, calcium-base bentonite it is one such or several
Kind, its ratio be 1 ~ 30wt% of the dry powder after drying.
7. according to the method described in claim 1, it is characterized by: the quality of added water is 40 ~ 60 of the dry powder after drying
wt%。
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Citations (3)
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|---|---|---|---|---|
| CN101147865A (en) * | 2006-09-20 | 2008-03-26 | 中国石油化工股份有限公司 | Method for preparing hydrogenation refined catalyst from waste catalyst |
| CN103223341A (en) * | 2013-04-26 | 2013-07-31 | 沈阳三聚凯特催化剂有限公司 | Preparation method of novel hydro-desulfurization catalyst |
| CN104785274A (en) * | 2015-04-13 | 2015-07-22 | 河北工业大学 | Method for preparing bulk Ni-Mo hydrodeoxygenation catalyst with large aperture |
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| US20060183626A1 (en) * | 2005-02-11 | 2006-08-17 | Cavalcanti Fernando Antonio Pe | Process for preparing catalysts and catalysts produced therefrom |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101147865A (en) * | 2006-09-20 | 2008-03-26 | 中国石油化工股份有限公司 | Method for preparing hydrogenation refined catalyst from waste catalyst |
| CN103223341A (en) * | 2013-04-26 | 2013-07-31 | 沈阳三聚凯特催化剂有限公司 | Preparation method of novel hydro-desulfurization catalyst |
| CN104785274A (en) * | 2015-04-13 | 2015-07-22 | 河北工业大学 | Method for preparing bulk Ni-Mo hydrodeoxygenation catalyst with large aperture |
Non-Patent Citations (1)
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| "从失活的油脂加氢催化剂中回收镍";郭宪吉;《工业催化》;20030430;第11 卷(第4 期);第41页左栏第13-18行、右栏第1-3行、右栏倒数第1-3行 |
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