CN101733132B - Catalyst system for producing diesel oil and method for producing diesel oil by using system - Google Patents
Catalyst system for producing diesel oil and method for producing diesel oil by using system Download PDFInfo
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- CN101733132B CN101733132B CN2008102262855A CN200810226285A CN101733132B CN 101733132 B CN101733132 B CN 101733132B CN 2008102262855 A CN2008102262855 A CN 2008102262855A CN 200810226285 A CN200810226285 A CN 200810226285A CN 101733132 B CN101733132 B CN 101733132B
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- catalyst system
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Abstract
The invention provides a catalyst system for producing high-cleanness diesel oil, which comprises mixed acid of concentrated sulfuric acid and concentrated phosphoric acid, and a mixture dispersed in the mixed acid and consisting of aluminum oxide, magnesium oxide and silicon dioxide. The invention also provides a method for producing the high-cleanness diesel oil, which comprises a step of pre-treating raw materials for the catalyst system of the invention. According to the catalyst system and the method, the high-cleanness diesel oil can be produced. The high-cleanness diesel oil prepared by the method can form synthetic diesel oil meeting the requirement of international GB252-2000 standard through blending. Moreover, the process is relatively simple, does not consume energy, and has low unit production cost.
Description
Technical field
The present invention relates to a kind of catalyst system that is used to produce diesel oil, also relate to a kind of method that adopts this Catalyst Production diesel oil.
Background technology
At present, China all has a large amount of waste used oils, middle coalite tar, heavy oil, wax oil etc. to be used as waste disposal to fall every day, thereby causes the serious waste of resource.
The someone adopts physics method (Fig. 1) that above-mentioned refuse is handled.So-called physics method; Be meant to utilize and be no more than 400 ℃ weighing apparatus constant temperature; Adopt the method for heating, Coal Chemical Industry or the petroleum by-product that will have an oil component obtains the technical process of cut at many carbon alkanes mixture of 120 ℃ to 360 ℃ through the mode of distillation or catalytic pyrolysis.Product after many carbon alkanes mixture is wherein allocated is called high-cleanness diesel oil.But will consume mass energy in the physics method production process, and equipment investment is bigger, so the overall process cost is high, thereby has limited its practical application.
" catalytic pyrolysis " of present technique indication be meant in 360 ℃～380 ℃ temperature ranges, utilizes " fixed-bed catalytic " or directly select for use in present technique to add 1%～3% the aluminium oxide catalytic pyrolysis as the catalyst realization in the raw material.
Therefore, be badly in need of a kind of cost effective method that can effectively utilize above-mentioned raw materials at present.
Summary of the invention
One object of the present invention is to provide a kind of catalyst system that is used for producing at low cost diesel oil.
Another object of the present invention is to provide a kind of method of producing diesel oil at low cost.
According to a first aspect of the invention, a kind of catalyst system that is used to produce diesel oil is provided, it comprises:
(1) mix acid liquor of the concentrated sulfuric acid, SPA;
(2) be scattered in the mixture of forming by aluminium oxide, magnesia, silica in the above-mentioned mix acid liquor.
According to a second aspect of the invention, a kind of method of producing high-cleanness diesel oil is provided, it comprises with catalyst system of the present invention raw material is carried out pretreated step.
Inventor of the present invention is surprised to find very much, can utilize chemical method that waste used oil, washing oil, middle coalite tar, heavy oil, wax oil or its mixture are handled through catalyst of the present invention, produces the high-cleanness diesel oil of National standard.With respect to physical method, the present invention has adopted chemical method to produce diesel oil, and technology is simple relatively, consumes energy not, and unit cost of production expense is low.
Below, the present invention is carried out more detailed description.But these descriptions and the embodiment that provides for purpose of description are not limitation of the present invention.
Description of drawings
Fig. 1 is the process flow diagram that prior art physics method is produced the diesel oil technology;
Fig. 2 is that the chemical treatment method (the non-way of distillation or catalystic pyrolysis) according to a kind of embodiment of the present invention is produced the process flow diagram of high-cleanness diesel oil technology;
Fig. 3 is that the physico-chemical process (the two method that combines) according to another embodiment of the present invention is produced the process flow diagram of high-cleanness diesel oil technology.
The specific embodiment
Among the present invention, unless otherwise indicated, term " high-cleanness diesel oil " is meant the diesel oil that meets relevant national standard (for example GB252-2000).
The invention provides a kind of catalyst system that is used to produce diesel oil, it comprises:
(1) mix acid liquor of the concentrated sulfuric acid, SPA;
(2) be scattered in the mixture of forming by aluminium oxide, magnesia, silica in the above-mentioned mix acid liquor.
A kind of preferred embodiment of catalyst system according to the present invention; Wherein the volume ratio of the concentrated sulfuric acid and SPA is 30-90:70-10, preferred 35-85:65-15, more preferably 40-80:60-20; Further preferred 50-70:50-30, preferred especially 55-65:45-35.
A kind of preferred embodiment of catalyst system according to the present invention, wherein the weight ratio of aluminium oxide, magnesia, silica is: 1-10:1-10:1-10, preferred 2-9:1-7:1-6, more preferably 3-6:4-2:3-2.
A kind of preferred embodiment of catalyst system according to the present invention; In wherein per 1000 milliliters of mix acid liquors, the content of the said mixture of being made up of aluminium oxide, magnesia, silica is the 0.01-40 gram, preferred 0.1-25 gram; Further preferred 1-30 gram; Also further preferred 1.5-20 gram, further preferred 2-10 gram, most preferably 3-8 gram.
Catalyst system of the present invention can adopt following method preparation: at first, the concentrated sulfuric acid, SPA are mixed; Then, predetermined amounts adds the mixture of being made up of aluminium oxide, magnesia, silica in mix acid liquor, and it is mixed.Be prone to more than 5 hours solids and liquid object lamination take place because catalyst system time of repose of the present invention surpasses, thereby should stir once more before the use of the catalyst system after leaving standstill, making it become the uniform mixed liquor of state can use.
When the concentrated sulfuric acid and SPA mix, preferably SPA is slowly added in the concentrated sulfuric acid, slowly stir while adding.So the preparation of catalytic liquid should be carried out in corrosion-resistant containers such as glass container, forbid directly to contact or with other metalware splendid attire with human body.
The preparation of the said mixture of being made up of aluminium oxide, magnesia, silica does not have particular restriction, for example can get aluminium oxide, magnesia, silica normal temperature by predetermined ratio and puddle evenly, can make desired mixt.
Although be reluctant to accept the opinion constraint, the inventor believes that in the catalyst system of the present invention, the said mixture of being made up of aluminium oxide, magnesia, silica is partly dissolved, reacts, and has formed acid salt in mix acid liquor.Therefore, the mixture of the acid salt that catalyst system of the present invention is the concentrated sulfuric acid, SPA, reaction generated, the mixture be made up of aluminium oxide, magnesia, silica comprising solids and liquid object, belongs to the solid-liquid system.The mechanism of catalyst system catalytic reaction of the present invention (chemical reaction mechanism of catalytic reaction agent) maybe be as follows: caltalyst ties up to and plays polymerisation in the microfabricated chemical reactor of chemical treatment raw material and lotus root is closed reaction promoter; Can make the macromolecule carbon generation polymerization in the secondary material of petrochemical industry or Coal Chemical Industry form polymolecular solid carbon particle; Be free on petrochemical industry or Coal Chemical Industry byproduct with the form of polymer and separate thereby make macromolecule carbon or higher carbon compounds molecule form polymolecular group, promptly form so-called oil, slag separates.
The present invention also provides a kind of method of producing diesel oil, and it comprises with above-mentioned catalyst system of the present invention raw material is carried out pretreated step.Preprocessing process is actual to be that the primary raw materials of being selected for use is decoloured, filters.As previously mentioned, should stir once more before the catalyst system of the present invention after leaving standstill uses, make it become the uniform mixed liquor of state and can be used for raw material is carried out preliminary treatment.
According to embodiment preferred, the raw material that per 1000 grams will be handled, the consumption of catalyst system of the present invention are the 1-6 gram, preferred 2-5 gram.Concrete consumption is selected according to raw material and the diesel oil that will produce.
According to embodiment preferred, method of the present invention also comprises adaptation step and optional purification step subsequently.
According to a kind of preferred embodiment of the inventive method, do not adopt physical method (method or the catalytic thermal cracking method that promptly add thermal distillation) in the whole flow process that raw material is handled.The raw material that is applicable to this scheme of the present invention include but not limited to waste old oil, light oil, washing oil, readymade oil, naphtalene oil, the non-standard diesel oil of all kinds of soil refinings, to refine non-standard diesel oil, tar, acid-refined oil, wash oil, machine washing oil, plastics oily.
According to other a kind of preferred embodiment of the inventive method, also comprise before the said pre-treatment step raw material is distilled or the step of catalytic pyrolysis.Add wherein that thermal distillation or catalytic pyrolysis preferably carry out under the steady temperature that is no more than 400 ℃ (preferred 350 ℃～400 ℃), temperature Tai Gaoyi makes many carbon alkanes fractures, produce unwanted gas.According to this scheme, raw material is handled through the physics method earlier, carries out chemical Treatment then.The raw material that is applicable to this scheme of the present invention includes but not limited to middle coalite tar, waste used oil, heavy oil, wax oil.
According to other a kind of preferred embodiment of the inventive method, after chemical Treatment, (comprise after the physics method processing in the physical-chemical process) after perhaps physical-chemical process is handled, adopt atlapulgite that the liquid after handling is further handled.The consumption of atlapulgite is the 2-5 weight % of pending liquid.
After adopting catalyst system of the present invention that raw material is carried out preliminary treatment, can add conventional auxiliary agent (for example catalytic combustion agent, optimization agent) and allocate according to the difference of raw material and the quality index of derv fuel, thus the diesel oil that obtains suiting the requirements.Also can add other high-flash lightweight component oil separately, blend like 200# solvent naphtha or aviation kerosine or low-gravity GB fossil diesel fuel, with its physical and chemical index of further raising.
Below in conjunction with accompanying drawing and embodiment, the present invention is carried out more detailed illustrating.
Embodiment
Embodiment 1:
The preparation of catalyst system: the first step: get 70% (volume ratio) concentrated sulfuric acid, 30% (volume ratio) SPA; Second step: SPA is slowly added in the concentrated sulfuric acid, slowly stir, form mix acid liquor after about 30 minutes while adding; The 3rd step: the mixture of preparing aluminium oxide, magnesia, silica according to the weight ratio of 1:1:1; The 4th step: join the ratio of the mixture of the said aluminium oxide of 6g, magnesia, silica in every 1000ml mix acid liquor, the mixture of said aluminium oxide, magnesia, silica is added in the mix acid liquor, stir while adding, until becoming the micro emulsion shape.
Embodiment 2:
The preparation of catalyst system: the first step: get 30% (volume ratio) concentrated sulfuric acid, 70% (volume ratio) SPA; Second step: SPA is slowly added in the concentrated sulfuric acid, slowly stir, form mix acid liquor after about 30 minutes while adding; The 3rd step: the mixture of preparing aluminium oxide, magnesia, silica according to the weight ratio of 1:10:1; The 4th step: join the ratio of the mixture of the said aluminium oxide of 25g, magnesia, silica in every 1000ml mix acid liquor, the mixture of said aluminium oxide, magnesia, silica is added in the mix acid liquor, stir while adding, until becoming the micro emulsion shape.
Embodiment 3:
The preparation of catalyst system: the first step: get 50% (volume ratio) concentrated sulfuric acid, 50% (volume ratio) SPA; Second step: SPA is slowly added in the concentrated sulfuric acid, slowly stir, form mix acid liquor after about 30 minutes while adding; The 3rd step: the mixture of preparing aluminium oxide, magnesia, silica according to the weight ratio of 10:1:10; The 4th step: join the ratio of the mixture of the said aluminium oxide of 1g, magnesia, silica in every 1000ml mix acid liquor, the mixture of said aluminium oxide, magnesia, silica is added in the mix acid liquor, stir while adding, until becoming the micro emulsion shape.
Embodiment 4:
The preparation of catalyst system: the first step: get 90% (volume ratio) concentrated sulfuric acid, 10% (volume ratio) SPA; Second step: SPA is slowly added in the concentrated sulfuric acid, slowly stir, form mix acid liquor after about 30 minutes while adding; The 3rd step: the mixture of preparing aluminium oxide, magnesia, silica according to the weight ratio of 5:3:2; The 4th step: join the ratio of the mixture of the said aluminium oxide of 3g, magnesia, silica in every 1000ml mix acid liquor, the mixture of said aluminium oxide, magnesia, silica is added in the mix acid liquor, stir while adding, until becoming the micro emulsion shape.
Embodiment 5:
The preliminary treatment of feedstock oil (chemical method):
In 1000 gram washing oil, add the catalyst system of 1 gram embodiment 1, stirred 45 minutes, have the black fine particle to separate out; Staticly settle and be not less than 30 minutes; Isolate sediment then, in surplus liquid, add the 30g atlapulgite, fully stir more than 30 minutes; Obtain the washing oil after the primary treatment, filter then and obtain light yellow certified products.The dark brown defective work that obtains adopts the catalyst system of embodiment 1 to carry out after-treatment with said method.
Embodiment 6:
The preliminary treatment of feedstock oil (chemical method):
In 1000 gram light oil, add the catalyst system of 6 gram embodiment 2, stirred 45 minutes, have the black fine particle to separate out; Staticly settle and be not less than 30 minutes; Isolate sediment then, in surplus liquid, add the 30g atlapulgite, fully stir more than 30 minutes; Obtain the washing oil after the primary treatment, filter then and obtain light yellow certified products.The dark brown defective work that obtains adopts the catalyst system of embodiment 2 to carry out after-treatment with said method.
Embodiment 7:
The preliminary treatment of feedstock oil (chemical method):
In 1000 gram light oil, add the catalyst system of 3 gram embodiment 3, stirred 45 minutes, have the black fine particle to separate out; Staticly settle and be not less than 30 minutes; Isolate sediment then, in surplus liquid, add the 30g atlapulgite, fully stir more than 30 minutes; Obtain the washing oil after the primary treatment, filter then and obtain lurid prefinished products (through mass spectral analysis is C
12-C
24Hydrocarbon).The dark brown defective work that obtains adopts the catalyst system of embodiment 3 to carry out after-treatment with said method.Referring to Fig. 2.
Embodiment 8:
The preliminary treatment of feedstock oil (physics method and chemical method combine):
Get coalite tar as raw material, all or part of coalite tar is added thermal distillation or catalytic pyrolysis 360 ℃～380 ℃ temperature ranges, deliver to the chemical treatment section after the condensation of gas of distilling or catalytic pyrolysis obtains is reclaimed; Adopt the catalyst system of embodiment 4 to carry out preliminary treatment; The residue that stays obtains transparency liquid through filtering behind distillation or the catalytic pyrolysis, treat that transparency liquid deepens brown, black after; Part is delivered to the chemical treatment section and is adopted the catalyst system of embodiment 4 to carry out preliminary treatment; Remainder carries out adding thermal distillation or catalytic pyrolysis the second time, obtains the peony material, conventional filtration; The dark red filtrate that obtains is filtered (consumption of atlapulgite is per 100 gram filtratings, 3 gram atlapulgites) with atlapulgite, and (through mass spectral analysis is C to obtain the prefinished products of buff
12-C
24Hydrocarbon).Referring to Fig. 3.
Embodiment 9:
The allotment of high-cleanness diesel oil:
Adopt following prescription (by weight) to allocate, obtain high-cleanness diesel oil:
The prefinished products 96～99 that obtains among the embodiment 7
Nitric acid isooctyl (playing the effect of optimizing agent) 0.05～2
Diesel pour inhibitor 0.1～10
Barium mahogany sulfonate 0.2～3.
Embodiment 10:
Utilize high-cleanness diesel oil to blend combined diesel oil:
Adopt following prescription (by weight) to allocate, obtain combined diesel oil:
The high-cleanness diesel oil 450～600 that obtains among the embodiment 9
200# solvent naphtha 200～300
Index fossil diesel oil 150～300
Nitric acid isooctyl 0.2～2
Barium mahogany sulfonate 0.1～1.
Claims (10)
1. catalyst system that is used to produce diesel oil, it comprises:
(1) mix acid liquor of the concentrated sulfuric acid, SPA;
(2) be scattered in the mixture of forming by aluminium oxide, magnesia, silica in the above-mentioned mix acid liquor.
2. the catalyst system of claim 1, wherein the volume ratio of the concentrated sulfuric acid and SPA is 30-90: 70-10.
3. the catalyst system of claim 1, wherein the weight ratio of aluminium oxide, magnesia, silica is: 1-10: 1-10: 1-10.
4. the catalyst system of claim 1, in wherein per 1000 milliliters of mix acid liquors, the content of the said mixture of being made up of aluminium oxide, magnesia, silica is the 0.01-25 gram.
5. the catalyst system of claim 4, in wherein per 1000 milliliters of mix acid liquors, the content of the said mixture of being made up of aluminium oxide, magnesia, silica is the 1.5-20 gram.
6. the catalyst system of claim 5, in wherein per 1000 milliliters of mix acid liquors, the content of the said mixture of being made up of aluminium oxide, magnesia, silica is the 2-10 gram.
7. method of producing diesel oil, it comprises that the catalyst system with claim 1 carries out pretreated step to raw material, and said preliminary treatment is meant decolours and filters primary raw materials, and the consumption of wherein said catalyst system is per 1000 gram raw material 1-6 grams.
8. the method for claim 7 also comprises adaptation step subsequently.
9. the method for claim 7 also comprised the step of raw material being distilled or in 360 ℃～380 ℃ temperature ranges, utilizes the fixed-bed catalytic cracking before said pre-treatment step.
10. the method for claim 7, wherein said raw material is selected from waste used oil, washing oil, middle coalite tar, heavy oil, wax oil.
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| CN2008102262855A CN101733132B (en) | 2008-11-12 | 2008-11-12 | Catalyst system for producing diesel oil and method for producing diesel oil by using system |
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| CN2008102262855A CN101733132B (en) | 2008-11-12 | 2008-11-12 | Catalyst system for producing diesel oil and method for producing diesel oil by using system |
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| CN101733132B true CN101733132B (en) | 2012-01-25 |
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Citations (3)
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| CN1522293A (en) * | 2002-03-11 | 2004-08-18 | ��Ԩ��ѧ��ҵ��ʽ���� | Method for producing bio-fuel |
| CN1748019A (en) * | 2002-12-19 | 2006-03-15 | 格雷斯公司 | Process for removal of nitrogen containing contaminants from gas oil feedstreams. |
| CN101029274A (en) * | 2007-04-23 | 2007-09-05 | 肖青山 | Method and apparatus for refining light diesel oil and gasoline from waste mobile oil |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1522293A (en) * | 2002-03-11 | 2004-08-18 | ��Ԩ��ѧ��ҵ��ʽ���� | Method for producing bio-fuel |
| CN1748019A (en) * | 2002-12-19 | 2006-03-15 | 格雷斯公司 | Process for removal of nitrogen containing contaminants from gas oil feedstreams. |
| CN101029274A (en) * | 2007-04-23 | 2007-09-05 | 肖青山 | Method and apparatus for refining light diesel oil and gasoline from waste mobile oil |
Non-Patent Citations (1)
| Title |
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| 董丽旭等.超声波作用下柴油氧化脱硫工艺研究.《化学与黏合》.2007,第29卷(第3期),第216－219页. * |
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Denomination of invention: Catalyst system for producing diesel oil and method for producing diesel oil by using system Effective date of registration: 20121123 Granted publication date: 20120125 Pledgee: Bank of Hangzhou, Limited by Share Ltd, Beijing, Zhongguancun branch Pledgor: Beijing Qingyan Lihua Petroleum Chemical Technology Co., Ltd. Registration number: 2012110000004 |
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Date of cancellation: 20130506 Granted publication date: 20120125 Pledgee: Bank of Hangzhou, Limited by Share Ltd, Beijing, Zhongguancun branch Pledgor: Beijing Qingyan Lihua Petroleum Chemical Technology Co., Ltd. Registration number: 2012110000004 |
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Denomination of invention: Catalyst system for producing diesel oil and method for producing diesel oil by using system Effective date of registration: 20130508 Granted publication date: 20120125 Pledgee: Beijing wisdom industry Co., Ltd. Pledgor: Beijing Qingyan Lihua Petroleum Chemical Technology Co., Ltd. Registration number: 2013990000269 |
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Granted publication date: 20120125 Termination date: 20161112 |