CN103468305B - Solvent dewaxing method for low waxy hydrocarbon oil - Google Patents
Solvent dewaxing method for low waxy hydrocarbon oil Download PDFInfo
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Abstract
The invention relates to a solvent dewaxing method for low waxy hydrocarbon oil. The method includes mixing raw oil of a crude oil vacuum distillate fraction section, petroleum microcrystalline wax and a dewaxing solvent, cooling the mixture to a filtering temperature, filtering to obtain filtrate and cerate, and removing the solvent from the filtrate to obtain dewaxed oil, wherein the drop melting point of the petroleum microcrystalline wax is 67 DEG C to 92 DEG C, the mass ratio of the petroleum microcrystalline wax to the raw oil ranges from 0.005:1 to 0.2:1. Though use of the solvent dewaxing method, wax in the low waxy hydrocarbon oil can be more effectively removed, the dewaxing temperature difference can be reduced and the filtering speed can be increased.
Description
Technical field
The invention belongs to the process for dewaxing of hydrocarbon ils.Specifically, the present invention relates to the solvent-dewaxing method of the low content of wax hydrocarbon oil crude material of a kind of oil reduced pressure distillate section.
Background technology
In order to keep the low-temperature fluidity of lubricating oil, wax contained in stock oil must be removed in the production process of lubricant base, to reduce condensation point or the pour point of lubricant base.The product of wax after de-oiling is divided into paraffin and Microcrystalline Wax, and paraffin is based on normal paraffin and a certain amount of isoparaffin, and Microcrystalline Wax then containing normal paraffin, isoparaffin and alkyl naphthene, and contains a certain amount of alkylaromatic hydrocarbon.The method of lubricating oil dewaxing has a variety of, and wherein the most frequently used is solvent dewaxing process.The principle of solvent dewaxing be exactly by stock oil and dewaxing solvent miscible, then progressively cool, utilize insoluble to wax the component at low temperatures or oligodynamical of solvent and characteristic to other components dissolved, make wax crystallization in dewaxed solution, finally filter, oil is separated with wax.
Solvent dewaxing technology not only may be used for the wax removed in lube stock, also may be used for the component being separated different zero pour in other oil products.For different oil products, due to the wax content of stock oil and the difference of wax molecular structure and product different to the requirement of pour point, its solvent dewaxing process has larger difference.Such as: producing in the process of environment-friendly rubber extending oil with furfural extract oil, first must remove the wax extracted out in oil, then just can it can be used as the raw materials for production of environment-friendly rubber extending oil.But the wax removed in furfural extract oil with the solvent dewaxing process of routine is very difficult.
The criteria for classifying that the height of hydrocarbon ils wax content is ununified.For lubricant base is produced, it is generally acknowledged that the lube stock oil obtained by paraffinic crude is high-content wax stock oil, the lube stock oil obtained by naphthenic base crude is low waxy feeds oil, the wax content of the lube stock oil obtained by intermediate base crude oil is between the two above-mentioned, more be partial to naphthenic base crude, wax content is lower, and the isoparaffin in wax component, with the naphthenic hydrocarbon of long side chain or aromatic hydrocarbons more, adopt conventional solvent-dewaxing method to reduce the pour point of waxy oil more difficult.The content of wax hydrocarbon ils obtained after the content of wax hydrocarbon ils obtained by crude oil time processing or secondary processing, when the wax content of hydrocarbon ils low to a certain extent time, conventional solvent-dewaxing method cannot be adopted to produce the pressed oil meeting pour point and require, this class hydrocarbon ils is just called low content of wax hydrocarbon ils.
Summary of the invention
The invention provides a kind of solvent-dewaxing method of low content of wax hydrocarbon ils, the method more effectively can remove the wax in the low content of wax hydrocarbon oil crude material of oil reduced pressure distillate section, reduces dewaxing differential, improves filtration velocity.
A solvent-dewaxing method for low content of wax hydrocarbon ils, comprising: the stock oil of oil reduced pressure distillate section, oil Microcrystalline Wax and dewaxing solvent are mixed, be cooled to filtration temperature, filters and obtains filtrate and slack wax, after filtrate desolvation, obtain pressed oil; The melt drop temperature of oil Microcrystalline Wax is between 67 DEG C ~ 92 DEG C; The mass ratio of oil Microcrystalline Wax and stock oil is 0.005: 1 to 0.2: 1.
The mass ratio of oil Microcrystalline Wax and stock oil is preferably 0.008: 1 to 0.15: 1, is more preferably 0.01: 1 to 0.12: 1.
The melt drop temperature scope of described oil Microcrystalline Wax preferably between 67 DEG C ~ 92 DEG C, more preferably between 75 DEG C ~ 84 DEG C.The oleaginousness of described oil Microcrystalline Wax preferably between 0.4% ~ 5%, more preferably between 1% ~ 3%.
" the low content of wax " in the present invention refer to the lower and naphthenic hydrocarbon with long side chain in wax of the wax content of oil reduced pressure distillate section hydrocarbon oil crude material or aromatic hydrocarbons more, conventional solvent-dewaxing method cannot be adopted to produce the pressed oil meeting pour point and require.
The solvent-refined oil that the stock oil of reduced pressure distillate section can be the vacuum distillate of crude oil, vacuum distillate obtains through solvent treatment and solvent treatment extract oil out, extracted out hydrotreatment oil that oil obtains through hydrotreatment by above-mentioned vacuum distillate, solvent-refined oil and solvent treatment in one or more.Described vacuum distillate preferably subtracts three line distillates or subtracts four line distillates.
Stock oil pour point of the present invention preferably between 5 DEG C ~ 40 DEG C, more preferably between 10 DEG C ~ 35 DEG C.
In preferred situation, first oil Microcrystalline Wax is dissolved in stock oil, and then adds dewaxing solvent.Temperature oil Microcrystalline Wax being dissolved in stock oil is preferably 70 DEG C ~ 110 DEG C, is more preferably 80 DEG C ~ 100 DEG C.
Filtration temperature in hydrodewaxing step is preferably-25 DEG C ~ 0 DEG C, is more preferably-20 DEG C ~-10 DEG C.
Described dewaxing solvent is the mixture of ketone and aromatic hydrocarbons, and ketone is wherein preferably acetone and/or butanone, and aromatic hydrocarbons is preferably benzene and/or toluene; More preferably adopt little to wax solubleness and to this dewaxing solvent all dissolved of oil base, as the mixture of butanone and toluene.
When adopting the mixture of butanone and toluene as dewaxing solvent, with the cumulative volume of butanone-toluene Mixed Solvent for benchmark, the volume content of butanone is 40% to being less than 100%, preferably 50% to 95%.
When adopting the mixture of butanone and toluene as dewaxing solvent, the mass ratio of butanone-toluene Mixed Solvent and stock oil is 1: 1 to 8: 1, is preferably 2: 1 to 6: 1.
In the present invention, dewaxing solvent can disposablely add, and also can add several times, preferably divides and adds for 3 or 4 times.
According to the ratio of solvent and low waxy feeds oil, those skilled in the art easily can determine the additional proportion of each point diluting solvent.
According to the viscosity of material in process of cooling, what those skilled in the art easily can determine each point diluting solvent adds temperature.
The present invention once can dewax after hydrodewaxing step again, and second time dewaxing filtration temperature is between the scope of first time dewaxing filtration temperature to low 5 DEG C than it.Second time dewaxing can be filtered the diluting solvent that the filtrate obtained is used as first time dewaxing by the present invention, is preferably used as the secondary in first time dewaxing, three times or four diluting solvents.
The present invention also comprises, and by slack wax desolvation, obtains gatch.
In described separating filtrate and slack wax, the method for solvent is well known in the art, and such as respectively material is sent into solvent recovery tower except desolventizing, recovered solvent recycles.In the present invention, the solvent after recovery can containing a small amount of stock oil component.
Allly in the present invention relate in the step of different components mixing, preferably adopt mixing tank enhancing mixed effect.Described mixing tank belongs to prior art, and the present invention can adopt the liquid mixer of this area routine.
When the wax content of the stock oil of reduced pressure distillate section is to a certain extent low, during the pressed oil that conventional solvent-dewaxing method cannot be adopted to produce meet pour point to require, just method of the present invention can be adopted produce the pressed oil meeting pour point requirement.
The wax removed in oil reduced pressure distillate section low content of wax hydrocarbon ils with the solvent dewaxing process of routine is very difficult, and major cause is: the wax content 1. in low content of wax hydrocarbon oil crude material is lower, and high melting point component content is few, causes the wax recovery concentration in mixed solution lower; 2. the more important thing is, wax major part in low content of wax hydrocarbon oil crude material is naphthenic hydrocarbon with long side chain or aromatic hydrocarbons, and the wax crystalline substance formed in solvent dewaxing process is more tiny, and little wax crystalline substance easily penetrates filter cloth, enter in pressed oil, cause dewaxing differential increase, dewaxing effect reduction; 3. in addition, slightly large wax crystalline substance is easily stuck in filter cloth duct, and blocking filtration channel, reduces the permeability energy of filter cloth, and dewaxing filtration velocity reduces and the temperature increasing filter cloth washes the frequency.Compared with the solvent dewaxing technology of routine, the present invention with the addition of high melt drop temperature oil Microcrystalline Wax in low content of wax hydrocarbon ils, more effectively can remove the wax in the low content of wax hydrocarbon ils of oil reduced pressure distillate section, reduces dewaxing differential, improves filtration velocity.
Accompanying drawing explanation
Accompanying drawing is block diagram of the present invention.
Embodiment
Below in conjunction with accompanying drawing, a kind of preferred implementation of the present invention is described.
Stock oil mixes with the oil Microcrystalline Wax from pipeline 2 through pipeline 1, heat in well heater 4 through pipeline 3, mix further in mixing tank 6 through pipeline 5, in water cooler 10, be cooled to filtration temperature through pipeline 9 through pipeline 7 and the dewaxing solvent from pipeline 8, enter strainer 12 through pipeline 11 and filter; Dewaxed filtrate, through pipeline 13 desolventizing recovery tower 14 desolvation, obtains pressed oil through pipeline 15, does not mark the trend of recycling design in figure; Dewaxing slack wax, through pipeline 16 desolventizing recovery tower 17 desolvation, obtains gatch through pipeline 18, does not mark the trend of desolvation in figure.
Further illustrate the present invention by the following examples.
Embodiment 1
To subtract three extraction oil for raw material, its character is in table 1.The melt drop temperature of Microcrystalline Wax is 75 DEG C, and Microcrystalline Wax oleaginousness is 2%, and the mass ratio of Microcrystalline Wax and stock oil is 0.12: 1; Dewaxing solvent is butanone-toluene Mixed Solvent, and the volume content of butanone is 95%; Adopt multipoint dilution technique, total diluent oil is than 2: 1.Prepare pressed oil by the flow process of accompanying drawing 1, detailed process is as follows:
Oil Microcrystalline Wax is joined in stock oil, is heated to 80 DEG C, fully melt and after mixing, add each diluting solvent successively.Be cooled to-10 DEG C, obtain dewaxed filtrate and dewaxing slack wax after filtration, obtain pressed oil after filtrate desolvation, after slack wax desolvation, obtain gatch.Dewaxing results is in table 2.
Comparative example 1
Stock oil is identical with embodiment 1.Except not adding except oil Microcrystalline Wax in stock oil, all the other operations are all identical with embodiment 1 with test conditions.Dewaxing results is in table 2.
Embodiment 2
To subtract three distillates for raw material, its character is in table 1.The melt drop temperature of Microcrystalline Wax is 84 DEG C, and Microcrystalline Wax oleaginousness is 1%, and the mass ratio of Microcrystalline Wax and stock oil is 0.07: 1; Dewaxing solvent is butanone-toluene Mixed Solvent, and the volume content of butanone is 70%, and adopt multipoint dilution technique, total diluent oil is than 3.5: 1.Prepare pressed oil by the flow process of accompanying drawing 1, detailed process is as follows:
Oil Microcrystalline Wax is joined in stock oil, is heated to 100 DEG C, fully melt and after mixing, add each diluting solvent successively.Be cooled to-15 DEG C, obtain dewaxed filtrate and dewaxing slack wax after filtration, obtain pressed oil after filtrate desolvation, after slack wax desolvation, obtain gatch.Dewaxing results is in table 2.
Comparative example 2
Stock oil is identical with embodiment 2.Except not adding except oil Microcrystalline Wax in stock oil, all the other operations are all identical with embodiment 2 with test conditions.Dewaxing results is in table 2.
Embodiment 3
To subtract four hydrotreatment oil for raw material, its character is in table 1.The melt drop temperature of Microcrystalline Wax is 80 DEG C, and the oleaginousness of Microcrystalline Wax is 3%, and the mass ratio of Microcrystalline Wax and stock oil is 0.01: 1; Dewaxing solvent is butanone-toluene Mixed Solvent, and the volume content of butanone is 50%, and adopt multipoint dilution technique, total diluent oil is than 6: 1.Prepare pressed oil by the flow process of accompanying drawing 1, detailed process is as follows:
Oil Microcrystalline Wax is joined in stock oil, is heated to 90 DEG C, fully melt and after mixing, add each diluting solvent successively.Be cooled to-20 DEG C, obtain dewaxed filtrate and dewaxing slack wax after filtration, obtain pressed oil after filtrate desolvation, after slack wax desolvation, obtain gatch.Dewaxing results is in table 2.
Comparative example 3
Stock oil is identical with embodiment 3.Except not adding except oil Microcrystalline Wax in stock oil, all the other operations are all identical with embodiment 3 with test conditions.Dewaxing results is in table 2.
Table 1
| Subtract three extraction oil | Subtract three distillates | Subtract four hydrotreatment oil | |
| Pour point/DEG C | 15 | 24 | 33 |
| 100 DEG C of viscosity/(mm 2/s) | 27.91 | 8.991 | 10.31 |
| 20 DEG C of density/(kg/m 3) | 985.5 | 911.1 | 869.9 |
| Carbon residue/% | 0.48 | 0.1 | ＜0.05 |
| Flash-point/DEG C | / | 234 | 262 |
| Boiling range/DEG C | |||
| 10％ | / | 440 | 475 |
| 30％ | / | 449 | 489 |
| 50％ | / | 464 | 499 |
| 70％ | / | 490 | 515 |
Table 2
As can be seen from the solvent dewaxing result of each embodiment and corresponding comparative example, its corresponding comparative example is compared, and is added in stock oil by oil Microcrystalline Wax and carries out solvent dewaxing, and dewaxing filtration velocity all significantly improves, and dewaxing differential reduces.
As can be seen from the solvent dewaxing result of embodiment 1,2 and 3, be no matter extract oil out as raw material using the low content of wax, or using low wax-containing distillate or hydrotreatment oil as raw material, dewaxing filtration velocity can be improved through the inventive method, reduce dewaxing differential.
Claims (17)
1. a solvent-dewaxing method for low content of wax hydrocarbon ils, comprising: the stock oil of oil reduced pressure distillate section, oil Microcrystalline Wax and dewaxing solvent are mixed, be cooled to filtration temperature, filters and obtains filtrate and slack wax, after filtrate desolvation, obtain pressed oil; The melt drop temperature of described oil Microcrystalline Wax is between 67 DEG C ~ 92 DEG C; The mass ratio of oil Microcrystalline Wax and stock oil is 0.005: 1 to 0.2: 1; The solvent-refined oil that the stock oil of described reduced pressure distillate section is the vacuum distillate of crude oil, vacuum distillate obtains through solvent treatment and solvent treatment extract oil out, extracted out hydrotreatment oil that oil obtains through hydrotreatment by above-mentioned vacuum distillate, solvent-refined oil and solvent treatment in one or more, described vacuum distillate is for subtracting three line distillates or subtracting four line distillates.
2. in accordance with the method for claim 1, it is characterized in that, the mass ratio of oil Microcrystalline Wax and stock oil is 0.008: 1 to 0.15: 1.
3. in accordance with the method for claim 2, it is characterized in that, the mass ratio of oil Microcrystalline Wax and stock oil is 0.01: 1 to 0.12: 1.
4. in accordance with the method for claim 1, it is characterized in that, the melt drop temperature scope of described oil Microcrystalline Wax is between 67 DEG C ~ 92 DEG C.
5. in accordance with the method for claim 4, it is characterized in that, the melt drop temperature scope of described oil Microcrystalline Wax is between 75 DEG C ~ 84 DEG C.
6. in accordance with the method for claim 1, it is characterized in that, stock oil pour point is between 5 DEG C ~ 40 DEG C.
7. in accordance with the method for claim 6, it is characterized in that, stock oil pour point is between 10 DEG C ~ 35 DEG C.
8. in accordance with the method for claim 1, it is characterized in that, first oil Microcrystalline Wax is dissolved in stock oil, and then adds dewaxing solvent, temperature oil Microcrystalline Wax being dissolved in stock oil is 70 DEG C ~ 110 DEG C.
9. in accordance with the method for claim 8, it is characterized in that, temperature oil Microcrystalline Wax being dissolved in stock oil is 80 DEG C ~ 100 DEG C.
10. in accordance with the method for claim 1, it is characterized in that, described dewaxing solvent is the mixture of ketone and aromatic hydrocarbons.
11. in accordance with the method for claim 10, it is characterized in that, described ketone is acetone and/or butanone, and described aromatic hydrocarbons is benzene and/or toluene.
12. in accordance with the method for claim 11, it is characterized in that, described dewaxing solvent is butanone and toluene, and with the cumulative volume of butanone-toluene Mixed Solvent for benchmark, the volume content of butanone is 40% to being less than 100%.
13. in accordance with the method for claim 12, it is characterized in that, with the cumulative volume of butanone-toluene Mixed Solvent for benchmark, the volume content of butanone is 50% to 95%.
14. in accordance with the method for claim 12, it is characterized in that, the mass ratio of dewaxing solvent and stock oil is 1: 1 to 8: 1.
15. in accordance with the method for claim 14, it is characterized in that, the mass ratio of dewaxing solvent and stock oil is 2: 1 to 6: 1.
16. in accordance with the method for claim 1, it is characterized in that, by slack wax desolvation, obtains gatch.
17. in accordance with the method for claim 1, it is characterized in that, after hydrodewaxing step, the slack wax obtained that dewaxes for the first time is dewaxed again, filtration temperature dewaxing for the second time between the scope of first time dewaxing filtration temperature to low 5 DEG C than it, being used as filtering the filtrate obtained for the second time the diluting solvent dewaxed for the first time.
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3576735A (en) * | 1969-10-29 | 1971-04-27 | Gulf Research Development Co | Paraffinic slack wax as a dewaxing aid for lubricating oils |
| SU1675322A1 (en) * | 1989-05-03 | 1991-09-07 | Московский Институт Нефти И Газа Им.И.М.Губкина | Method of producing solid hydrocarbons |
| CN1648216A (en) * | 2004-01-19 | 2005-08-03 | 中国石油化工股份有限公司 | Solvent dewaxing method |
| CN102952571A (en) * | 2011-08-25 | 2013-03-06 | 中国石油化工股份有限公司 | Solvent dewaxing method of low-wax content heavy hydrocarbon oil |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3576735A (en) * | 1969-10-29 | 1971-04-27 | Gulf Research Development Co | Paraffinic slack wax as a dewaxing aid for lubricating oils |
| SU1675322A1 (en) * | 1989-05-03 | 1991-09-07 | Московский Институт Нефти И Газа Им.И.М.Губкина | Method of producing solid hydrocarbons |
| CN1648216A (en) * | 2004-01-19 | 2005-08-03 | 中国石油化工股份有限公司 | Solvent dewaxing method |
| CN102952571A (en) * | 2011-08-25 | 2013-03-06 | 中国石油化工股份有限公司 | Solvent dewaxing method of low-wax content heavy hydrocarbon oil |
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