CN107029767A - A kind of catalyst being hydrogenated with for waste mineral oil in the technique of regeneration and its production method - Google Patents
A kind of catalyst being hydrogenated with for waste mineral oil in the technique of regeneration and its production method Download PDFInfo
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Abstract
The invention discloses a kind of catalyst being hydrogenated with for waste mineral oil in the technique of regeneration, its innovative point is：The catalyst is so that alumina support supports active component W, Ni and adjuvant component P, Si and is formed, in terms of the gross mass of the catalyst, WO3 contents are that 20~28%, NiO contents are 7.0~13.0%, P content 4.0~10.5%, Si contents 3.0~6.0%, and surplus is alumina support；The specific surface area of the catalyst is 220~230m2/g, and pore volume is 0.52~0.56ml/g.The present invention's is used for the catalyst that waste mineral oil is hydrogenated with the technique of regeneration, W, Ni two-component metal combination of selection special ratios are used as active component, and auxiliary component Si and P are equipped with, the selection and rational proportion by each component obtain higher high active of hydrogenation catalysis and selectivity.Especially auxiliary agent Si, P introducing, improves the ratio surface of carrier, acidity, improves active metal decentralization, with superhigh specific surface area, large aperture, faintly acid can be hydrogenated with to the full cut of non-mineral oil.
Description
Technical field
The present invention relates to a kind of catalyst being hydrogenated with for waste mineral oil in the technique of regeneration, the invention further relates to a kind of production method for the catalyst being hydrogenated with for waste mineral oil in the technique of regeneration, belong to lubricating oil preparation field.
Background technology
With growing continuously and fast for China's economic, the consumption of lube product is also in cumulative year after year, and China's lubricating oil Apparent con- sumption in 2006 is about 6,800,000 tons, and the waste lubricating oil that about 4,000,000 tons are had accordingly is produced.And the rate of recovery of waste lubricating oil is up to more than 90%, major part therein is used as the oil that makes a fire, and not only pollutes environment, and waste the energy.
With crude oil price rise steadily and petroleum resources increasingly reduction, waste oil regeneration has attracted increasing attention, the particularly recycling of waste lubricating oil, and to saving the energy in terms of the recycling and environmental protection of resource, environmental protection is significant.Research and development are applied to the Social benefit and economic benefit for the hydrogenation catalyst that waste lubricant oil by hydrogenation regenerates significantly, and market potential is huge, will have good promotion prospect.Therefore, the regeneration technology and regenerated catalyst of waste lubricating oil will turn into an important directions of people's research and development from now on.People began to focus on the regeneration of waste lubricating oil in recent years, it is expected that reclaimed oil reaches the level of the basic oil quality of new oil.
Due to various oxidation products are not only existed in waste lubricating oil（Mainly carboxylic acids, carboxylic acid esters, aldehydes, ketone, alcohols, phenols, peroxide etc.）The heavy metal compound and waste lubricating oil that also remaining phenolic additive, sulfur-containing compound, halogen compounds, nitride and additive etc. is brought are in use due to metal of mechanical part of high temperature wear etc., and these undesirable components bring difficulty to the regeneration techniques of waste lubricating oil.
In the regeneration technology of waste lubricating oil, hydrofinishing is important link, the process is mainly feedstock oil and is mixed into reactor with a certain proportion of hydrogen at a certain temperature, under catalyst action, the hetero atoms such as hydrogen and S, N, O in waste oil chemically react, the accessory substances such as H2S, NH3, H2O are correspondingly generated, to remove impurity；Also with a small amount of unsaturated hydrocarbons in waste oil addition reaction occurs for hydrogen, to reach saturation；Hydrogen is also acted on the heavy metal in waste oil, makes heavy metal deposition on the surface of catalyst.In order that waste lubricating oil molecule is chemically reacted in catalyst active center, first, catalyst must possess sufficiently large specific surface area and enough pore volumes and unimpeded duct, be that reactant and product molecule provide preferable reacting environment；Secondly, theoretically, in order to keep the ideal composition of the long side chain lubricating oil of few ring, regenerative process does not allow occur cracking reaction, lube base oil viscosity otherwise will be caused to decline, therefore, catalyst should have as far as possible few solid acid.It is worthy of note that, heavy metal undesirable components content is higher in waste lubricating oil, and this pore structure for being accomplished by catalyst base is sufficiently large relative to conventional carrier, to ensure catalyst long-term operation.And at present in process for regeneration of waste lubricating oil, hydrogenation catalyst used therein is common oil hydrogenation catalyst, due to the particularity of waste lubricating oil composition, existing common hydrogenation catalyst is applied to be difficult to reach preferable hydrofinishing effect when reclaiming waste lubricating oil.Therefore, in order to be able to remove the above-mentioned impurity in waste lubricating oil, the quality of reclaimed oil is lifted, a kind of big pore volume, bigger serface, faintly acid is researched and developed, the catalyst for being exclusively used in process for regeneration of waste lubricating oil undoubtedly has great importance.
The content of the invention
It is an object of the invention to for deficiency of the prior art, a kind of catalyst being hydrogenated with for waste mineral oil in the technique of regeneration is provided, the selectivity and hydrogenation activity of catalyst is enhanced, undesirable components hydrogenation saturation therein can be made, retain ideal composition, obtain properties of product excellent.
In order to solve the above technical problems, the technical solution adopted by the present invention is：A kind of catalyst being hydrogenated with for waste mineral oil in the technique of regeneration, its innovative point is：The catalyst be so that alumina support supports active component W, Ni and adjuvant component P, Si and is formed, in terms of the gross mass of the catalyst, WO3Content is that 20~28%, NiO contents are 7.0~13.0%, P content 4.0~10.5%, Si contents 3.0~6.0%, and surplus is alumina support；The specific surface area of the catalyst is 220~230m2/ g, pore volume is 0.52~0.56ml/g.
On this basis, in terms of the gross mass by the catalyst, WO3Content is that 24%, NiO contents are 9.0%, P content 6.5%, Si contents 4.5%, and surplus is alumina support.
On this basis, the specific surface area of the catalyst is 223~227m2/g。
On this basis, the pore volume of the catalyst is 0.54~0.55ml/g.
It is a further object to provide a kind of production method for the catalyst being hydrogenated with for waste mineral oil in the technique of regeneration, its innovative point is：Comprise the following steps：
（1）Prepare catalyst carrier：Aluminium hydroxide dry powder, ammonium hydrogencarbonate, sesbania powder and nitric acid mixing are weighed successively, and the kneading and compacting that adds water, 3~4h is placed at room temperature and is air-dried, and dries 2~5h at a temperature of 100~110 afterwards, then 1~1.5h is calcined at 500~550 DEG C, alumina support is made；
（2）Prepare co-impregnated solution：The ammonium metatungstate solution for taking mass concentration to be 50~60%, according to every 1ml ammonium metatungstate solutions 0.056~0.063g and 0.06~0.065g ratio, nickelous carbonate and organic acid is separately added into ammonium metatungstate solution, mixed liquor is made in stirring and dissolving, according to mixed liquor：Silicate solution：Phosphoric acid solution=1：0.15~0.3：0.2~0.3, and the content of organic acid is per 3~13 grams in 100ml co-impregnated solutions；
（3）Prepare catalyst：According to 0.6~0.8g of every 1ml co-impregnated solutions ratio, resulting alumina support is immersed in co-impregnated solution, and in impregnating 1h under normal temperature, 3~4h is stood at room temperature again to be air-dried, then it is dried into 1~2h at a temperature of 100~120 DEG C, finally produced in 500~650 DEG C of 1~1.5h of roasting temperature.
On this basis, the organic acid is the mixture of citric acid, glacial acetic acid and malic acid, wherein, the mixed proportion of citric acid, glacial acetic acid and malic acid is 1.5~4.5：2.5~3.5：3~5.
On this basis, the step（1）Middle aluminium hydroxide dry powder, ammonium hydrogencarbonate, the mass ratio of sesbania powder and nitrate mixture are 1.2：0.035~0.046：0.036~0.048.
On this basis, the step（1）Middle aluminium hydroxide dry powder, ammonium hydrogencarbonate, the mass ratio of sesbania powder and nitrate mixture are 1.2：0.037：0.042.
Beneficial effects of the present invention are as follows：
（1）The present invention's is used for the catalyst that waste mineral oil is hydrogenated with the technique of regeneration, W, Ni two-component metal combination of selection special ratios are used as active component, and auxiliary component Si and P are equipped with, the selection and rational proportion by each component obtain higher high active of hydrogenation catalysis and selectivity.Especially auxiliary agent Si, P introducing, improve the ratio surface of carrier, acidity, improve active metal decentralization, with superhigh specific surface area, large aperture, faintly acid, the full cut of non-mineral oil can be hydrogenated with, with very strong removing S, N, O and undesirable components hydrogenation saturability, and with extremely strong demetalization and anti-metal ability, enhance the selectivity and hydrogenation activity of catalyst, undesirable components hydrogenation saturation therein can be made, retain ideal composition, obtain properties of product excellent.
（2）The present invention's is used for the catalyst that waste mineral oil is hydrogenated with the technique of regeneration, regeneration technology is hydrogenated with applied to non-mineral oil, raw material is without pretreatment, it can be directly hydrogenated with, resulting mineral oil base oil, which reconciles, to be combined, and total recovery reaches 100%, not only increase the yield of regeneration oil product, and technological process is simplified, production cost is substantially reduced, and improves economic benefit.
（3）The present invention's is used for the catalyst that waste mineral oil is hydrogenated with the technique of regeneration, pass through the active component and adjuvant component of reasonable selection special ratios content and appropriate catalyst carrier, and appropriate organic acid is added in combination in preparation method, make preparation-obtained catalyst have big pore volume, bigger serface, it is active high the features such as, and preparation flow is short, prepare reproducible, cost is low, can long-term operation.
Embodiment
Technical scheme is elaborated with reference to specific embodiment.
Embodiment 1
It is a kind of for waste mineral oil be hydrogenated with regeneration technique in catalyst, the catalyst be so that alumina support supports active component W, Ni and adjuvant component P, Si and is formed, in terms of the gross mass of the catalyst, WO3Content is that 20%, NiO contents are 7.0%, P content 4.0%, Si contents 3.0%, and surplus is alumina support；The specific surface area of catalyst is 220m2/ g, pore volume is 0.52ml/g.
The production method of this catalyst being hydrogenated with for waste mineral oil in the technique of regeneration, comprises the following steps above：
（1）Prepare catalyst carrier：Aluminium hydroxide dry powder, ammonium hydrogencarbonate, sesbania powder and nitric acid mixing, and the kneading and compacting that adds water are weighed successively, and 3h is placed at room temperature and is air-dried, 2h is dried at a temperature of 100 afterwards, is then calcined 1h at 500 DEG C, alumina support is made；
（2）Prepare co-impregnated solution：The ammonium metatungstate solution for taking mass concentration to be 50%, according to every 1ml ammonium metatungstate solutions 0.056g and 0.06g ratio, nickelous carbonate and organic acid is separately added into ammonium metatungstate solution, mixed liquor is made in stirring and dissolving, according to mixed liquor：Silicate solution：Phosphoric acid solution=1：0.15：0.2, and the content of organic acid is per 3 grams in 100ml co-impregnated solutions；
（3）Prepare catalyst：According to every 1ml co-impregnated solutions 0.6g ratio, resulting alumina support is immersed in co-impregnated solution, and in impregnating 1h under normal temperature, then stands 3~4h at room temperature and air-dried, then by it at a temperature of 100 DEG C drying 1h, finally produced in 500 DEG C of roasting temperature 1h.
Wherein, organic acid is the mixture of citric acid, glacial acetic acid and malic acid, wherein, the mixed proportion of citric acid, glacial acetic acid and malic acid is 1.5：2.5：3.
Step（1）Middle aluminium hydroxide dry powder, ammonium hydrogencarbonate, the mass ratio of sesbania powder and nitrate mixture are 1.2：0.035：0.036.
Embodiment 2
It is a kind of for waste mineral oil be hydrogenated with regeneration technique in catalyst, the catalyst be so that alumina support supports active component W, Ni and adjuvant component P, Si and is formed, in terms of the gross mass of the catalyst, WO3Content is that 28%, NiO contents are 13.0%, P content 10.5%, Si contents 6.0%, and surplus is alumina support；The specific surface area of catalyst is 230m2/ g, pore volume is 0.56ml/g.
The production method of this catalyst being hydrogenated with for waste mineral oil in the technique of regeneration, comprises the following steps above：
（1）Prepare catalyst carrier：Aluminium hydroxide dry powder, ammonium hydrogencarbonate, sesbania powder and nitric acid mixing, and the kneading and compacting that adds water are weighed successively, and 4h is placed at room temperature and is air-dried, 5h is dried at a temperature of 110 afterwards, is then calcined 1.5h at 550 DEG C, alumina support is made；
（2）Prepare co-impregnated solution：The ammonium metatungstate solution for taking mass concentration to be 60%, according to every 1ml ammonium metatungstate solutions 0.063g and 0.065g ratio, nickelous carbonate and organic acid is separately added into ammonium metatungstate solution, mixed liquor is made in stirring and dissolving, according to mixed liquor：Silicate solution：Phosphoric acid solution=1：0.3：0.3, and the content of organic acid is per 13 grams in 100ml co-impregnated solutions；
（3）Prepare catalyst：According to every 1ml co-impregnated solutions 0.8g ratio, resulting alumina support is immersed in co-impregnated solution, and in impregnating 1h under normal temperature, then stands 4h at room temperature and air-dried, then by it at a temperature of 120 DEG C drying 2h, finally produced in 650 DEG C of roasting temperature 1.5h.
Organic acid is the mixture of citric acid, glacial acetic acid and malic acid, wherein, the mixed proportion of citric acid, glacial acetic acid and malic acid is 4.5：3.5：5.
Step（1）Middle aluminium hydroxide dry powder, ammonium hydrogencarbonate, the mass ratio of sesbania powder and nitrate mixture are 1.2：0.037：0.042.
Embodiment 3
It is a kind of for waste mineral oil be hydrogenated with regeneration technique in catalyst, the catalyst be so that alumina support supports active component W, Ni and adjuvant component P, Si and is formed, in terms of the gross mass of the catalyst, WO3Content is that 24%, NiO contents are 9.0%, P content 6.5%, Si contents 4.5%, and surplus is alumina support, and the specific surface area of catalyst is 225m2/ g, the pore volume of catalyst is 0.54.5ml/g.
The production method of this catalyst being hydrogenated with for waste mineral oil in the technique of regeneration, comprises the following steps above：
（1）Prepare catalyst carrier：Aluminium hydroxide dry powder, ammonium hydrogencarbonate, sesbania powder and nitric acid mixing, and the kneading and compacting that adds water are weighed successively, and 3~4h is placed at room temperature and is air-dried, 3h is dried at a temperature of 105 afterwards, is then calcined 1.2h at 530 DEG C, alumina support is made；
（2）Prepare co-impregnated solution：The ammonium metatungstate solution for taking mass concentration to be 55%, according to every 1ml ammonium metatungstate solutions 0.059g and 0.063g ratio, nickelous carbonate and organic acid is separately added into ammonium metatungstate solution, mixed liquor is made in stirring and dissolving, according to mixed liquor：Silicate solution：Phosphoric acid solution=1：0.23：0.25, and the content of organic acid is per 8 grams in 100ml co-impregnated solutions；
（3）Prepare catalyst：According to every 1ml co-impregnated solutions 0.7g ratio, resulting alumina support is immersed in co-impregnated solution, and in impregnating 1h under normal temperature, then stand 3.5h at room temperature and air-dried, then it is dried into 1.5h at a temperature of 110 DEG C, finally produced in 550 DEG C of roasting temperature 1.3h.
Wherein, organic acid is the mixture of citric acid, glacial acetic acid and malic acid, wherein, the mixed proportion of citric acid, glacial acetic acid and malic acid is 2.5：3.0：4.
Step（1）Middle aluminium hydroxide dry powder, ammonium hydrogencarbonate, the mass ratio of sesbania powder and nitrate mixture are 1.2：0.042：0.045.
It is as shown in the table for the main physico-chemical property of catalyst carrier in embodiment 1,2 and 3：
| Project | Embodiment 1 | Embodiment 2 | Embodiment 3 |
| Crushing strength/N.cm-1 | 193 | 196 | 199 |
| Granularity | 1.6x（3~8） | 1.6x（3~8） | 1.6x（3~8） |
| Specific surface area/m2.g-1 | 306 | 303 | 299 |
| Pore volume/ml.g-1 | 0.80 | 0.76 | 0.78 |
| Heap ratio/g.cm-3 | 0.45 | 0.46 | 0.48 |
It is as shown in the table for the main physico-chemical property of catalyst in embodiment 1,2 and 3：
| Project | Embodiment 1 | Embodiment 2 | Embodiment 3 |
| Chemical composition/m% | |||
| WO3 | 20% | 28% | 24% |
| NiO | 7.0% | 13.0% | 9.0% |
| Si | 4.0% | 10.5% | 6.5% |
| P | 3.0% | 6.0% | 4.5% |
| Specific surface area/m2 | 220 | 230 | 225 |
| Pore volume | 0.52 | 0.56 | 0.54.5 |
| Crushing strength | 198 | 199 | 201 |
| Granularity | 1.6x（3~8） | 1.6x（3~8） | 1.6x（3~8） |
The general principle and principal character and advantages of the present invention of the present invention has been shown and described above.It should be understood by those skilled in the art that; the present invention is not limited to the above embodiments; merely illustrating the principles of the invention described in above-described embodiment and specification; without departing from the spirit and scope of the present invention; various changes and modifications of the present invention are possible, and these changes and improvements all fall within the protetion scope of the claimed invention.The scope of the present invention is defined by the appended claims and its equivalents.
Claims (8)
1. a kind of catalyst being hydrogenated with for waste mineral oil in the technique of regeneration, it is characterised in that：The catalyst be so that alumina support supports active component W, Ni and adjuvant component P, Si and is formed, in terms of the gross mass of the catalyst, WO3Content is that 20~28%, NiO contents are 7.0~13.0%, P content 4.0~10.5%, Si contents 3.0~6.0%, and surplus is alumina support；The specific surface area of the catalyst is 220~230m2/ g, pore volume is 0.52~0.56ml/g.
2. the catalyst according to claim 1 being hydrogenated with for waste mineral oil in the technique of regeneration, it is characterised in that：In terms of the gross mass by the catalyst, WO3Content is that 24%, NiO contents are 9.0%, P content 6.5%, Si contents 4.5%, and surplus is alumina support.
3. the catalyst according to claim 1 being hydrogenated with for waste mineral oil in the technique of regeneration, it is characterised in that：The specific surface area of the catalyst is 223~227m2/g。
4. the catalyst according to claim 1 being hydrogenated with for waste mineral oil in the technique of regeneration, it is characterised in that：The pore volume of the catalyst is 0.54~0.55ml/g.
5. it is used for the production method for the catalyst that waste mineral oil is hydrogenated with the technique of regeneration described in a kind of claim 1, it is characterised in that：Comprise the following steps：
（1）Prepare catalyst carrier：Aluminium hydroxide dry powder, ammonium hydrogencarbonate, sesbania powder and nitric acid mixing are weighed successively, and the kneading and compacting that adds water, 3~4h is placed at room temperature and is air-dried, and dries 2~5h at a temperature of 100~110 afterwards, then 1~1.5h is calcined at 500~550 DEG C, alumina support is made；
（2）Prepare co-impregnated solution：The ammonium metatungstate solution for taking mass concentration to be 50~60%, according to every 1ml ammonium metatungstate solutions 0.056~0.063g and 0.06~0.065g ratio, nickelous carbonate and organic acid is separately added into ammonium metatungstate solution, mixed liquor is made in stirring and dissolving, according to mixed liquor：Silicate solution：Phosphoric acid solution=1：0.15~0.3：0.2~0.3, and the content of organic acid is per 3~13 grams in 100ml co-impregnated solutions；
（3）Prepare catalyst：According to 0.6~0.8g of every 1ml co-impregnated solutions ratio, resulting alumina support is immersed in co-impregnated solution, and in impregnating 1h under normal temperature, 3~4h is stood at room temperature again to be air-dried, then it is dried into 1~2h at a temperature of 100~120 DEG C, finally produced in 500~650 DEG C of 1~1.5h of roasting temperature.
6. the production method of the catalyst according to claim 5 being hydrogenated with for waste mineral oil in the technique of regeneration, it is characterised in that：The organic acid is the mixture of citric acid, glacial acetic acid and malic acid, wherein, the mixed proportion of citric acid, glacial acetic acid and malic acid is 1.5~4.5：2.5~3.5：3~5.
7. the production method of the catalyst according to claim 5 being hydrogenated with for waste mineral oil in the technique of regeneration, it is characterised in that：The step（1）Middle aluminium hydroxide dry powder, ammonium hydrogencarbonate, the mass ratio of sesbania powder and nitrate mixture are 1.2：0.035~0.046：0.036~0.048.
8. the production method of the catalyst according to claim 7 being hydrogenated with for waste mineral oil in the technique of regeneration, it is characterised in that：The step（1）Middle aluminium hydroxide dry powder, ammonium hydrogencarbonate, the mass ratio of sesbania powder and nitrate mixture are 1.2：0.037：0.042.
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| CN108130129A (en) * | 2018-02-13 | 2018-06-08 | 新疆聚力环保科技有限公司 | Waste mineral oil two-stage hydrogenation handles regeneration technology and method for preparing catalyst |
| CN108251156A (en) * | 2018-01-31 | 2018-07-06 | 新疆聚力环保科技有限公司 | A kind of method of full fraction waste mineral oil two-stage hydrogenation processing regeneration technology |
| CN114602533A (en) * | 2022-03-14 | 2022-06-10 | 山东久硕环保科技有限公司 | Preparation method of regenerated hydrogenation catalyst for waste lubricating oil |
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| CN101041139A (en) * | 2007-04-30 | 2007-09-26 | 京福马(北京)石油化工高新技术有限公司 | Catalyzer for regenerating the waste lubricant oil by hydrogenation and the preparing method |
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Application publication date: 20170811 |