CN103789040B - A kind of method of producing high-smelting point petroleum wax - Google Patents
A kind of method of producing high-smelting point petroleum wax Download PDFInfo
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- CN103789040B CN103789040B CN201210433561.1A CN201210433561A CN103789040B CN 103789040 B CN103789040 B CN 103789040B CN 201210433561 A CN201210433561 A CN 201210433561A CN 103789040 B CN103789040 B CN 103789040B
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Abstract
The present invention relates to a kind of method of producing high-smelting point petroleum wax, described method concrete steps are: de-oiling raw material first with petroleum waxes hydrofining catalytic catalyst exposure, under Hydrofinishing conditions, carry out refining reaction, the de-oiling raw material after hydrofining produces dewaxed oil through solvent deoiling.In the inventive method, solvent used in solvent deoiling process is the asymmetrical ether and the C that contain the tertiary butyl
3~ C
6alkenolic mixed solvent.Adopt the inventive method to produce high-smelting point petroleum wax, the filtration velocity raising 20% ~ 35% of solvent deoiling, dewaxed oil yield raising 1% ~ 3% can be made.
Description
Technical field
The present invention relates to a kind of method of producing high-smelting point petroleum wax, particularly adopt the method for solvent deoiling raw material hydrofining and methylethylketone/Ethyl Tertisry Butyl Ether mixed solvent de-oiling to produce high-smelting point petroleum wax.High-smelting point petroleum wax of the present invention comprises paraffin and the Microcrystalline Wax that fusing point is not less than 62 DEG C.
Background technology
The de-oiling of petroleum wax mainly contains sweating de-oiling and solvent deoiling two kinds of methods, and de-oiling raw material comprises the petroleum fractions of cold press dewaxing slack wax, solvent dewaxing slack wax or other high-content wax amount.Sweating de-oiling is only applicable to the lighter raw material of cut, and can not realize continuous seepage, current industrial less employing.Solvent deoiling method is applicable to the raw material of the various cuts such as transformer oil plant, lube stock and bright stock, and can realize serialization, long-cycle production, be the main production process of commodity oil wax.
Conventional solvent deoiling method adopts solvent dewaxing and de-oiling joint process, and the dewaxing slack wax containing solvent that dewaxing obtains adds solvent cut pulp, intensification de-oiling, filtering separation.This is one section of de-oiling.In most cases, the wax filter cake of one section of de-oiling adds solvent cut pulp, filtering separation again.This is two sections of de-oilings.The wax filter cake of two sections of de-oilings obtains the dewaxed oil of low oil content after steaming and desolventizing.The more employing of de-oiling solvent be the mixture of aliphatic ketone and aromatic hydrocarbons, what adopt at most is methylethylketone/toluene Mixed Solvent.
CN86105061A discloses a kind of solvent dewaxing and de-oiling combined technique of improvement, the method by de-oiling section filtrate all or major part recycle, the yield that can reduce fresh solvent consumption, reduce energy consumption, improve pressed oil and dewaxed oil.
The solvent dewaxing and deoiling combined technique that US4541917 dewaxes after introducing a kind of first de-oiling.The method adds dewaxing agent in dewaxing section, both can improve yield dewaxed oil, and turn avoid the pollution of auxiliary agent to wax.
When solvent deoiling with the dewaxing slack wax of the heavier vacuum distillate of the cuts such as No. 500 neutral oil plants, No. 650 neutral oil plants, No. 750 neutral oil plants for raw material production inspissated wax, or with the dewaxing slack wax of bright stock for raw material production Microcrystalline Wax time, routine techniques and above-mentioned two kinds of common drawback of improving one's methods are that filtration velocity is slow, filter cloth blocking is serious, cause that filter temperature is washed frequently, solvent consumption increases, the reduction of wax yield.
Summary of the invention
The object of the invention is to the shortcoming overcoming existing solvent deoiling production technology, propose a kind of method that dewaxing slack wax heavier with cut is raw material production high-smelting point petroleum wax, the method can improve filtration velocity, alleviates the blocking of filter cloth, improve product yield.
The invention provides a kind of production method of high-smelting point petroleum wax, described method is: de-oiling raw material first with petroleum waxes hydrofining catalytic catalyst exposure, refining reaction is carried out under Hydrofinishing conditions, de-oiling raw material after hydrofining and solvent, high-smelting point petroleum wax is obtained through one or more snippets solvent deoiling process, wherein, described solvent is the asymmetrical ether and the C that contain the tertiary butyl
3~ C
6alkenolic mixed solvent.
Described de-oiling raw material is the conventional raw material in this area, can be the dewaxing slack wax of the heavier vacuum distillate of the cut such as No. 500 neutral oil plants, No. 650 neutral oil plants, No. 750 neutral oil plants or bright stock.Catalyst for refining is with aluminum oxide or aluminum oxide-silicon oxide for carrier component, and with group VIB in the periodic table of elements and VIII race's metal for active ingredient, particularly tungsten and nickel, its active component content is WO
325wt% ~ 35wt%, NiO2wt% ~ 8wt%, specific surface area is 160m
2/ more than g, pore volume are 0.3cm
3/ more than g.Be WO preferably
329.5wt% ~ 31.5wt%, NiO4.0wt% ~ 5.0wt%, specific surface area 200 ~ 240m
2/ g, pore volume 0.4 ~ 0.6cm
3/ g.The operational condition of hydrofining reaction is: hydrogen dividing potential drop 4.0 ~ 20.0MPa, volume space velocity 0.1 ~ 2.0h
-1, temperature of reaction 240 ~ 350 DEG C, hydrogen to oil volume ratio 100 ~ 1000.Comparatively suitable hydrogenation conditions is: hydrogen dividing potential drop 5.0 ~ 15.0MPa, volume space velocity 0.2 ~ 1.5h
-1, temperature of reaction 260 ~ 330 DEG C, hydrogen to oil volume ratio 300 ~ 1000.Best reaction conditions is: hydrogen dividing potential drop 5.0 ~ 10.0MPa, volume space velocity 0.5 ~ 1.5h
-1, temperature of reaction 260 ~ 300 DEG C, hydrogen to oil volume ratio 300 ~ 500.
Solvent deoiling can adopt the solvent deoiling method of any routine, and primary process is cooled by fused raw material and adds de-oiling solvent, and the feed postition of solvent can adopt multipoint dilution method, also can adopt once full dilution process.Filtering separation is carried out after the mixture of raw material and solvent is cooled to de-oiling temperature under whipped state.This is one section of de-oiling.As required, degreasing process can adopt one or more snippets de-oiling.Wax filter cake obtains dewaxed oil after steaming desolventizing.
In the inventive method, solvent used in solvent deoiling process is the asymmetrical ether and the C that contain the tertiary butyl
3~ C
6alkenolic mixture.The asymmetrical ether containing the tertiary butyl in described solvent is methyl tertiary butyl ether, Ethyl Tertisry Butyl Ether, sec.-propyl tertbutyl ether or sec-butyl tertbutyl ether, preferred Ethyl Tertisry Butyl Ether.C in described solvent
3~ C
6aliphatic ketone is acetone, methylethylketone or methyl iso-butyl ketone (MIBK), is preferably methylethylketone.
In the inventive method, C in described solvent
3~ C
6alkenolic weight content is 45% ~ 90%, preferably 55% ~ 80%.More suitable weight of solvent and the ratio of raw material weight are de-oiling one section 4 ~ 12: 1, one section each section 2.0 ~ 6.0: 1 afterwards.De-oiling temperature is 5 ~ 40 DEG C.
Compared with prior art, adopt method in the present invention to produce high-smelting point petroleum wax, the filtration velocity raising 20% ~ 35% of solvent deoiling, dewaxed oil yield raising 1% ~ 3% can be made.
Embodiment
The raw material that the embodiment of the present invention and comparative example adopt is No. 650 neutral oil plants dewaxing slack wax (A) and bright stock dewaxing slack wax (B).Its character is in table 1.
The embodiment of the present invention and comparative example hydrofining adopt fixed bed one stage hydrofining technique, and Hydrobon catalyst is W-Ni/Al
2o
3type catalyst for hydrogen refining of paraffin wax.Catalyst property is: WO
329.8wt%, NiO4.3wt%, specific surface area 228m
2/ g, pore volume 0.46cm
3/ g.Hydrogenation process conditions and the results are shown in Table 2.In embodiment and comparative example, the fusing point of hydrogenation products and oleaginousness remain unchanged, and show substantially to occur without scission reaction, ensure that the characteristic index of petroleum wax is not destroyed.
The embodiment of the present invention and comparative example adopt one section of solvent deoiling technique, and in embodiment, solvent for use is methylethylketone/Ethyl Tertisry Butyl Ether mixed solvent, and content of methyl ethyl ketone is 65wt%.In comparative example, solvent for use is methylethylketone/toluene Mixed Solvent, and content of methyl ethyl ketone is 65wt%.Its processing condition and the results are shown in Table 3.In table 3, paraffin and Microcrystalline Wax compare with the comparative example of respective the same terms respectively.Embodiment shows, the de-oiling raw material producing high-smelting point petroleum wax, through hydrofining and methylethylketone/Ethyl Tertisry Butyl Ether mixed solvent de-oiling, can make the filtration velocity raising 20% ~ 35% of solvent deoiling, dewaxed oil yield raising 1% ~ 3%.
Table 1 feedstock property
| Project | A | B |
| Fusing point, DEG C | 61.0 | |
| Melt drop temperature, DEG C | 65.8 | |
| Oleaginousness, wt% | 23.11 | 9.75 |
| Kinematic viscosity (100 DEG C), mm 2/s | 9.501 | 23.20 |
| Molecular weight | 550 | 691 |
| Density (20 DEG C), kg/m 3 | 850 | 906 |
Table 2 hydrofining technology condition and result
| Project | Embodiment 1 | Comparative example 1 | Embodiment 2 | Comparative example 2 | Embodiment 3 | Comparative example 3 |
| Hydrogenating materials | A | A | A | A | B | B |
| Processing condition | ||||||
| Hydrogen dividing potential drop, MPa | 10.0 | 10.0 | 5.0 | 5.0 | 15.0 | 15.0 |
| Temperature of reaction, DEG C | 260 | 260 | 300 | 300 | 330 | 330 |
| Volume space velocity, h -1 | 0.4 | 0.4 | 1.0 | 1.0 | 1.5 | 1.5 |
| Hydrogen to oil volume ratio | 300 | 300 | 500 | 500 | 800 | 800 |
| Hydrogenation products | A 1 | A 1 | A 2 | A2 | B 3 | B 3 |
| Fusing point, DEG C | 61.0 | 61.0 | 61.5 | 61.5 | ||
| Melt drop temperature, DEG C | 65.5 | 65.5 | ||||
| Oleaginousness, wt% | 23.15 | 23.16 | 23.15 | 23.13 | 9.55 | 9.55 |
Table 3 solvent deoiling processing condition and result
| Project | Embodiment 4 | Comparative example 4 | Embodiment 5 | Comparative example 5 | Embodiment 6 | Comparative example 6 |
| De-oiling raw material | A 1 | A 1 | A 2 | A 2 | B 3 | B 3 |
| Processing condition | ||||||
| Solvent ratio (weight) | 8 | 8 | 5 | 5 | 11 | 11 |
| De-oiling temperature, DEG C | 10 | 10 | 20 | 20 | 35 | 35 |
| Relative worry speed kg/ (m 2·h) | 134.0 | 100.0 | 125.6 | 100.0 | 122.2 | 100.0 |
| Dewaxed oil | ||||||
| Fusing point, DEG C | 67.4 | 67.7 | 69.6 | 70.1 | ||
| Melt drop temperature, DEG C | 79.6 | 80.8 | ||||
| Yield, wt% | 47.6 | 45.3 | 44.0 | 42.6 | 32.8 | 30.0 |
Claims (5)
1. the production method of a high-smelting point petroleum wax, described method is: de-oiling raw material first with petroleum waxes hydrofining catalytic catalyst exposure, refining reaction is carried out under Hydrofinishing conditions, de-oiling raw material after hydrofining and solvent, obtain high-smelting point petroleum wax through one or more snippets solvent deoiling process, it is characterized in that: described solvent is the asymmetrical ether and the C that contain the tertiary butyl
3~ C
6alkenolic mixed solvent, the asymmetrical ether containing the tertiary butyl in described solvent is Ethyl Tertisry Butyl Ether, the C in described solvent
3~ C
6aliphatic ketone is methylethylketone, C in described solvent
3~ C
6alkenolic content is 50wt% ~ 90wt%, and described de-oiling raw material is the dewaxing slack wax of bright stock, and described de-oiling temperature is 5 ~ 40 DEG C, and the operational condition of described hydrofining reaction is: hydrogen dividing potential drop 4.0 ~ 20.0MPa, volume space velocity 0.1 ~ 2.0h
-1, temperature of reaction 240 ~ 350 DEG C, hydrogen to oil volume ratio 100 ~ 1000, described Hydrobon catalyst is W-Ni/Al
2o
3type catalyst for hydrogen refining of paraffin wax, catalyst property is: WO
329.8wt%, NiO4.3wt%, specific surface area is 228m
2/ g, pore volume are 0.46cm
3/ g.
2. in accordance with the method for claim 1, it is characterized in that: C in described solvent
3~ C
6alkenolic content is 60wt% ~ 80wt%.
3. in accordance with the method for claim 1, it is characterized in that: the weight ratio de-oiling one section of described solvent and de-oiling raw material be 4 ~ 12: 1, one section after each section be 2.0 ~ 6.0: 1.
4. in accordance with the method for claim 1, it is characterized in that: described hydrofining reaction operational condition is: hydrogen dividing potential drop 5.0 ~ 15.0MPa, volume space velocity 0.2 ~ 1.5h
-1, temperature of reaction 260 ~ 330 DEG C, hydrogen to oil volume ratio 300 ~ 1000.
5. in accordance with the method for claim 4, it is characterized in that: described hydrofining reaction operational condition is: hydrogen dividing potential drop 5.0 ~ 10.0MPa, volume space velocity 0.5 ~ 1.5h
-1, temperature of reaction 260 ~ 300 DEG C, hydrogen to oil volume ratio 300 ~ 500.
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105779000B (en) * | 2014-12-18 | 2017-11-24 | 中国石油化工股份有限公司 | A kind of preparation method of soap wax |
| CN105733679B (en) * | 2014-12-28 | 2017-11-24 | 中国石油化工股份有限公司 | A kind of sweating and the method for production soap wax and paraffin |
| CN105733681B (en) * | 2014-12-28 | 2017-10-03 | 中国石油化工股份有限公司 | A kind of sweating and the method for producing microwax |
| CN107523261B (en) * | 2016-06-17 | 2019-05-17 | 中国石油化工股份有限公司 | A method of preparing hot melt adhesive |
| CN107513411B (en) * | 2016-06-17 | 2019-06-18 | 中国石油化工股份有限公司 | A kind of production method of wax polish |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4541917A (en) * | 1983-12-19 | 1985-09-17 | Exxon Research And Engineering Co. | Modified deoiling-dewaxing process |
| CN1335372A (en) * | 2000-07-24 | 2002-02-13 | 中国石油化工股份有限公司 | Production process of high-smelting point petroleum wax |
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2012
- 2012-11-05 CN CN201210433561.1A patent/CN103789040B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4541917A (en) * | 1983-12-19 | 1985-09-17 | Exxon Research And Engineering Co. | Modified deoiling-dewaxing process |
| CN1335372A (en) * | 2000-07-24 | 2002-02-13 | 中国石油化工股份有限公司 | Production process of high-smelting point petroleum wax |
Non-Patent Citations (1)
| Title |
|---|
| "脱蜡新溶剂-MTBE";王士新等;《炼油》;20011231(第2期);第1、2、3节 * |
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