CN103789040A - Method for production of high-melting-point petroleum wax - Google Patents
Method for production of high-melting-point petroleum wax Download PDFInfo
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- CN103789040A CN103789040A CN201210433561.1A CN201210433561A CN103789040A CN 103789040 A CN103789040 A CN 103789040A CN 201210433561 A CN201210433561 A CN 201210433561A CN 103789040 A CN103789040 A CN 103789040A
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Abstract
The invention relates to a method for production of high-melting-point petroleum wax. The method comprises the steps of: firstly making a deoiling raw material contact a petroleum wax hydrofining catalyst to undergo refining reaction under a hydrofining condition, subjecting the deoiling raw material undergoing hydrofining to deoiling by a solvent to produce deoiled wax. According to the method provided by the invention, the solvent used in the solvent deoiling process is a mixed solvent of tert-butyl-containing asymmetric ether and C3-C6 aliphatic ketone. Production of high-melting-point petroleum wax by the method provided by the invention can improve the filtration speed of solvent deoiling by 20%-35% and increase the yield of deoiled wax by 1%-3%.
Description
Technical field
The present invention relates to a kind of method of producing high-smelting point petroleum wax, particularly adopt the method for the hydrofining of solvent deoiling raw material and the de-oiling of methylethylketone/Ethyl Tertisry Butyl Ether mixed solvent to produce high-smelting point petroleum wax.High-smelting point petroleum wax of the present invention comprises that fusing point is not less than paraffin and the Microcrystalline Wax of 62 ℃.
Background technology
The de-oiling of petroleum wax mainly contains sweating de-oiling and two kinds of methods of solvent deoiling, and de-oiling raw material comprises the petroleum fractions of cold press dewaxing slack wax, solvent dewaxing slack wax or other high wax content.Sweating de-oiling is only applicable to the raw material that cut is lighter, and can not realize continuous production, industrial less employing at present.Solvent deoiling method is applicable to the raw material of the various cuts such as transformer oil plant, lube stock and bright stock, can realize serialization, long period production, is the main production method of commodity oil wax.
Conventional solvent deoiling method adopts solvent dewaxing and de-oiling joint process, and the dewaxing slack wax that contains 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 improved solvent dewaxing and de-oiling combined technique, the method by de-oiling section filtrate all or major part recycle, can reduce fresh solvent consumption, reduce energy consumption, improve the yield of pressed oil and dewaxed oil.
US4541917 introduces the solvent dewaxing and deoiling combined technique dewaxing after a kind of first de-oiling.The method adds dewaxing agent in dewaxing section, both can improve yield dewaxed oil, has avoided again the pollution of auxiliary agent to wax.
When solvent deoiling is take 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 as raw material production inspissated wax, or take the dewaxing slack wax of bright stock during as raw material production Microcrystalline Wax, routine techniques and above-mentioned two kinds of common shortcomings of improving one's methods are that filtration velocity is slow, filter cloth stops up seriously, 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 overcome the shortcoming of existing solvent deoiling production technology, propose a kind of method take the heavier dewaxing slack wax of cut as raw material production high-smelting point petroleum wax, the method can improve filtration velocity, alleviates the obstruction of filter cloth, improve product yield.
The invention provides a kind of production method of high-smelting point petroleum wax, described method is: first de-oiling raw material contacts with petroleum waxes hydrofining catalytic catalyzer, under hydrofining condition, carry out refining reaction, de-oiling raw material and solvent after hydrofining, obtain high-smelting point petroleum wax through one or more snippets solvent deoiling process, wherein, described solvent is asymmetrical ether and the C containing the tertiary butyl
3～C
6alkenolic mixed solvent.
Described de-oiling raw material is the conventional raw material in this area, can be the heavier vacuum distillate of the cuts such as No. 500 neutral oil plants, No. 650 neutral oil plants, No. 750 neutral oil plants or the dewaxing slack wax of bright stock.Catalyst for refining is take aluminum oxide or aluminum oxide-silicon oxide as carrier component, take group VIB in the periodic table of elements and VIII family metal as active ingredient, and particularly tungsten and nickel, its active component content is WO
325wt%～35wt%, NiO2wt%～8wt%, specific surface area is 160m
2/ g is above, pore volume is 0.3cm
3more than/g.Be WO preferably
329.5wt%～31.5wt%, NiO4.0 wt%～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, 240～350 ℃ of temperature of reaction, hydrogen to oil volume ratio 100～1000.More suitable hydrogenation conditions is: hydrogen dividing potential drop 5.0～15.0MPa, volume space velocity 0.2～1.5h
-1, 260～330 ℃ of temperature of reaction, 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, 260～300 ℃ of temperature of reaction, hydrogen to oil volume ratio 300～500.
Solvent deoiling can adopt the solvent deoiling method of any routine, and primary process is that the mode that adds of solvent can adopt multipoint dilution method by cooling fused raw material and add de-oiling solvent, also can adopt once full dilution process.The mixture of raw material and solvent carries out filtering separation be cooled to de-oiling temperature under whipped state after.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, in solvent deoiling process, solvent used is asymmetrical ether and the C containing 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, preferably 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 a section 4～12 of de-oiling: 1, one section each section 2.0～6.0 afterwards: 1.De-oiling temperature is 5～40 ℃.
Compared with prior art, adopt method in the present invention to produce high-smelting point petroleum wax, can make filtration velocity raising 20%～35%, the dewaxed oil yield of solvent deoiling improve 1%～3%.
Embodiment
The raw material that the embodiment of the present invention and comparative example adopt is No. 650 neutral oil plant dewaxing slack waxs (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%, NiO 4.3wt%, specific surface area 228m
2/ g, pore volume 0.46cm
3/ g.Hydrogenation technique condition 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, have guaranteed 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 respectively with the comparative example comparison of the same terms separately.Embodiment shows, produces the de-oiling raw material of high-smelting point petroleum wax through hydrofining and the de-oiling of methylethylketone/Ethyl Tertisry Butyl Ether mixed solvent, can make filtration velocity raising 20%～35%, the dewaxed oil yield of solvent deoiling improve 1%～3%.
Table 1 feedstock property
| Project | A | B |
| Fusing point, ℃ | 61.0 | ? |
| Melt drop temperature, ℃ | ? | 65.8 |
| Oleaginousness, wt% | 23.11 | 9.75 |
| Kinematic viscosity (100 ℃), mm 2/s | 9.501 | 23.20 |
| Molecular weight | 550 | 691 |
| Density (20 ℃), 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, ℃ | 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, ℃ | 61.0 | 61.0 | 61.5 | 61.5 | ? | ? |
| Melt drop temperature, ℃ | ? | ? | ? | ? | 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, ℃ | 10 | 10 | 20 | 20 | 35 | 35 |
| Relatively consider fast kg/ (m 2·h) | 134.0 | 100.0 | 125.6 | 100.0 | 122.2 | 100.0 |
| Dewaxed oil | ? | ? | ? | ? | ? | ? |
| Fusing point, ℃ | 67.4 | 67.7 | 69.6 | 70.1 | ? | ? |
| Melt drop temperature, ℃ | ? | ? | ? | ? | 79.6 | 80.8 |
| Yield, wt% | 47.6 | 45.3 | 44.0 | 42.6 | 32.8 | 30.0 |
Claims (14)
1. the production method of a high-smelting point petroleum wax, described method is: first de-oiling raw material contacts with petroleum waxes hydrofining catalytic catalyzer, under hydrofining condition, carry out refining reaction, de-oiling raw material and solvent after hydrofining, obtain high-smelting point petroleum wax through one or more snippets solvent deoiling process, it is characterized in that: described solvent is asymmetrical ether and the C containing the tertiary butyl
3～C
6alkenolic mixed solvent.
2. it is characterized in that in accordance with the method for claim 1: 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.
3. it is characterized in that in accordance with the method for claim 1: the C in described solvent
3～C
6aliphatic ketone is acetone, methylethylketone or methyl iso-butyl ketone (MIBK).
4. it is characterized in that in accordance with the method for claim 1: C in described solvent
3～C
6alkenolic content is 50wt%～90wt%.
5. according to the method described in claim 1 or 4, it is characterized in that: C in described solvent
3～C
6alkenolic content is 60wt%～80wt%.
6. it is characterized in that in accordance with the method for claim 1: one section of the weight ratio de-oiling of described solvent and de-oiling raw material be 4～12: 1, one section after each section be 2.0～6.0: 1.
7. it is characterized in that in accordance with the method for claim 1: described de-oiling temperature is 5～40 ℃.
8. it is characterized in that in accordance with the method for claim 1: described de-oiling raw material is the dewaxing slack wax of No. 500 neutral oil plants, No. 650 neutral oil plants, No. 750 neutral oil plants or bright stock.
9. in accordance with the method for claim 1, it is characterized in that: described Hydrobon catalyst is take aluminum oxide or aluminium oxide-silicon oxide as carrier component, take group VIB in the periodic table of elements and VIII family metal as active ingredient.
10. in accordance with the method for claim 9, it is characterized in that: in described Hydrobon catalyst, active ingredient is tungsten and nickel, in metal oxide, content is WO
325wt%～35wt%, NiO2wt%～8wt%, specific surface area is 160m
2/ g is above, pore volume is 0.3cm
3more than/g.
11. in accordance with the method for claim 10, it is characterized in that: the content of described Hydrobon catalyst active ingredient is WO
329.5wt%～31.5wt%, NiO4.0wt%～5.0wt%, specific surface area 200～240m
2/ g, pore volume 0.4～0.6cm
3/ g.
12. in accordance with the method for claim 1, it is characterized in that: the operational condition of described hydrofining reaction is: hydrogen dividing potential drop 4.0～20.0MPa, volume space velocity 0.1～2.0h
-1, 240～350 ℃ of temperature of reaction, hydrogen to oil volume ratio 100～1000.
13. according to the method described in claim 1 or 11, 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, 260～330 ℃ of temperature of reaction, hydrogen to oil volume ratio 300～1000.
14. according to the method described in claim 1 or 11, 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, 260～300 ℃ of temperature of reaction, hydrogen to oil volume ratio 300～500.
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| CN103789040B CN103789040B (en) | 2016-01-20 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105733679A (en) * | 2014-12-28 | 2016-07-06 | 中国石油化工股份有限公司 | Sweating and soap wax and paraffin producing method |
| CN105733681A (en) * | 2014-12-28 | 2016-07-06 | 中国石油化工股份有限公司 | Sweating and microcrystalline wax producing method |
| CN105779000A (en) * | 2014-12-18 | 2016-07-20 | 中国石油化工股份有限公司 | Preparation method of saponated paraffin |
| CN107513411A (en) * | 2016-06-17 | 2017-12-26 | 中国石油化工股份有限公司 | A kind of production method of wax polish |
| CN107523261A (en) * | 2016-06-17 | 2017-12-29 | 中国石油化工股份有限公司 | A kind of method for preparing PUR |
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 |
-
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 |
|---|
| 王士新等: ""脱蜡新溶剂-MTBE"", 《炼油》, no. 2, 31 December 2001 (2001-12-31) * |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105779000A (en) * | 2014-12-18 | 2016-07-20 | 中国石油化工股份有限公司 | Preparation method of saponated paraffin |
| 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 |
| CN105733679A (en) * | 2014-12-28 | 2016-07-06 | 中国石油化工股份有限公司 | Sweating and soap wax and paraffin producing method |
| CN105733681A (en) * | 2014-12-28 | 2016-07-06 | 中国石油化工股份有限公司 | Sweating and microcrystalline wax producing method |
| 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 |
| 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 |
| CN107513411A (en) * | 2016-06-17 | 2017-12-26 | 中国石油化工股份有限公司 | A kind of production method of wax polish |
| CN107523261A (en) * | 2016-06-17 | 2017-12-29 | 中国石油化工股份有限公司 | A kind of method for preparing PUR |
| 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 |
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| CN103789040B (en) | 2016-01-20 |
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