CN1118543C - Refining basic oil of lubricating oil by denitrification - Google Patents
Refining basic oil of lubricating oil by denitrification Download PDFInfo
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- CN1118543C CN1118543C CN 99122371 CN99122371A CN1118543C CN 1118543 C CN1118543 C CN 1118543C CN 99122371 CN99122371 CN 99122371 CN 99122371 A CN99122371 A CN 99122371A CN 1118543 C CN1118543 C CN 1118543C
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Abstract
On the basis of the denitrification process for lube base oil, an adsorbent is used in stead of clay so as to overcome the defects of high refining temperature, high energy consumption, need of a heating furnace, etc. which exist in the traditional clay process, thereby reducing refining temperature and saving energy consumption. The present invention saves equipment cost and provides a process for supplementing economical refined lube base oil.
Description
The invention belongs to the refining of petroleum field, relate in particular to the good lube base oil making technology of oxidation stability, its international Patent classificating number is C10M101/00.
As everyone knows, the quality level of lubricating oil should adapt with Development in Machine Industry, continuous increase along with Development in Machine Industry of China and import equipment, requirement to quality of lubrication oil also improves rapidly, at present, the quality of lubrication oil that China produces compared with developed countries, also has certain gap, influenced China's lubricating oil competitive capacity in market at home and abroad, thereby the quality that improves China's lubricating oil is the present task of top priority, improve the quality of lubricating oil, must at first improve the quality of base oil.Aspect the raising quality of lubrication oil, domestic and international many experts have done a lot of work: the essence of EP.0278694 patent is to remove the basic nitrogen compound of solvent in raffinating oil, its denitrogenation method is with solid acid polar adsorbent dealkalize nitrogen, these sorbent materials have silicon-aluminium, aluminium-based porous catalytic cracking agent, zeolite etc., the renovation process of solid adsorbent is high pressure, high temperature hydrogenation, or uses solvent washing.The essence of United States Patent (USP) 4137154 is to adsorb denitrogenation after adsorbing anhydrous acidic gas with solid adsorbent, and solid adsorbent is silica gel, X zeolite, aluminum oxide and composition thereof, and sour gas is hydrogen bromide, hydrogenchloride.United States Patent (USP) 4600502 is to come the bright stock base oil with alkaline adsorbent such as ion exchange resin, IIA family oxide compound and hopcalite as sorbent material, thereby reduces the whipability of lubricant base.EP.053510A2 is with acidic ion exchange resin, silica gel treatment lubricant base, thereby improves the demulsification performance of lubricant base.CN.1130676A handles lubricant base with gac, to improve the quality of lubricant base.CN.1060305: the processing method that provides peculiar smell in a kind of deep removal kerosene fraction, whole process comprises strong oxidizer oxidation, adding assistant catalyzed oxidation and three kinds of different chemical process combinations of solid adsorbent absorption, and product after treatment meets the mineral oil of the supporting odorless of fine chemicals.The essence of above-mentioned patent all is the bad components that itself exist in lubricant base or the kerosene by removing, to improve the performance of oil product.Oxidation stability all directly influences the work-ing life or the high-temperature behavior of lubricating oil with regard to quality of lubrication oil, therefore this character is subjected to people's attention always, lubricant base oxidation stability and its chemical constitution have close getting in touch, in this respect, experts and scholars have carried out many researchs both at home and abroad, result of study shows: it is positive interaction that the existence of the sulfide in the lubricant base has certain restraining effect to oxidation, nitride then is a negative interaction, especially basic nitrogen compound has very strong negative interaction, high outside the comparator of nitrogen sulphur in the crude oil in China, nitride concentrates in the heavier component mostly, so amount of nitrides height in the lube base, and China's lubricant base process for refining can not address this problem well, and clay-filtered technology is carclazyte consumption height not only, poor selectivity, yield is low, operational condition is poor, and environmental issue is outstanding, and nitride can only remove 40-50%; Hydrofining technology dealkalize nitrogen is very low or take off hardly, the decreasing ratio of sulphur is then very high, the high-pressure hydrogenation process investment is huge, the cost height, adopt the producer of this technology very few, Chinese patent (ZL94115190.5) has been invented a kind of high sulfur-preserving and denitrifying agent of lubricant base selectivity that is used for, for the good lubricant base of preparation oxidation stability provides favourable condition.Existing patent 97116286.7 has been invented a kind of refined course of lubricating oil, its process is: at the present dewaxing device of producing lubricant base, the propane deasphalting device, furfural treatment or phenol treating device, in the production process such as hydrogenation or clay-filtered device, add nitrogen rejection facility before or after any one device or the several means combined process, thereby remove the neutral and alkali nitride of lubricant base, improve the oxidation stability of lubricant base, improve the quality of base oil.Still contain traditional clay-filtered device in the technological process of this invention, and it is traditional clay-filtered except carclazyte consumption height, poor selectivity, outside environmental issue is outstanding, also having an important problem is that clay-filtered temperature needs do not wait for 170 ℃-300 ℃, the energy consumption height, heating needs with process furnace (accompanying drawing 1).
Purpose of the present invention is exactly that traditional carclazyte technology is got rid of in the aftertreatment of denitrogenation oil, reduces extraction temperature, the cancellation process furnace.Essence of the present invention is not the bad component that itself exists in order to remove in the lubricant base, but removes lubricant base because of adding residual composition after the denitrfying agent denitrogenation, and it is a kind of post-refining process after the denitrogenation of lubricating oil usefulness denitrfying agent.
The present invention replaces the carclazyte in the clay finishing system in the denitrification process technology with another sorbent material, can satisfy refining base oil requirement fully, after also finding to use sorbent material, adsorption temp can be 20 ℃ to 180 ℃, both reduced extraction temperature, energy efficient also can be cancelled process furnace, saves cost of equipment.
The present invention provides a kind of improved lubricating oil denitrogenation post-refining process, this method comprises, use a kind of effective adsorbent to replace traditional carclazyte, the composition of improved sorbent material is the porousness solid matter, or pressed powder or the particle and the mixture thereof of inorganic salt, mineral alkali, metal oxide.Can be used to implement the present invention, but the explanation example that does not limit the sorbent material of the scope of the invention is: gac, diatomite, molecular sieve and their compound; Improvement also comprises the absorption heat-exchange system in the process system in addition, and available fully common interchanger replaces traditional process furnace, comes the good lubricating base oil of production oxidation stability.
The inventive method see accompanying drawing 2, it is that a kind of residual oil with straight-run gas oil or propane deasphalting passes through solvent treatment as raw material, dewaxing, denitrogenation, refining with adsorbents or repeated hydrogenation and produce lubricant base, it is characterized in that lubricant base (1) and denitrfying agent (2) flow into static mixer (A) at pipe-line blending, enter electric slurry tank (B) behind the thorough mixing, denitrogenation oil (3) flows out from electric slurry tank (B) top and mixes with sorbent material (3b) in pipeline, the sorbent material consumption is the 0.01-5% (weight) of denitrogenation oil, enter interchanger (E) and be heated to normal temperature-180 ℃, enter again that filter (C) is removed sorbent material and the residue that contains and make treated oil (5).
Two of the inventive method is seen accompanying drawing 3, it also is that a kind of residual oil with straight-run gas oil or propane deasphalting passes through solvent treatment as raw material, dewaxing, denitrogenation, refining with adsorbents or repeated hydrogenation and produce lubricant base, it is characterized in that lubricant base (1) and denitrfying agent (2) flow into static mixer (A) at pipe-line blending, enter electric slurry tank (B) behind the thorough mixing, denitrogenation slag (4) is drained from electric slurry tank (B) bottom, denitrogenation oil (3) flows out the fixed-bed adsorber (F) that enters filled with adsorbent (3b) from electric slurry tank (B) top, adsorption temp is a normal temperature-180 ℃, the sorbent material consumption is the 0.001-5% (weight) of denitrogenation oil, and makes treated oil (5).
1. with straight-run gas oil as lubricant base oil fraction, through dewaxing, oil after the furfural treatment or through above-mentioned refining after again the oil of mild hydrogenation through heat exchange to 25 ℃-130 ℃ and denitrfying agent with the ratio (abbreviation agent-oil ratio) 1 of denitrfying agent with oil: 50-1: 500 mix in static mixer, enter electric slurry tank then between strength of electric field 0-3000V/cm, the denitrogenation slag is discharged from the slurry tank bottom, and denitrogenation oil flows out from electrofining slurry tank top, is just preparing oxidation stability good lubricant base after the adsorption treatment through the sorbent material of 0.1%-0.3% under 80 ℃ of-130 ℃ of conditions again.
2. with straight-run gas oil as lubricant base oil fraction, through dewaxing, oil after the furfural treatment or through above-mentioned refining after heat exchange to 25 ℃-130 ℃ and denitrfying agent with agent-oil ratio 1: 50-1: 500 mix in static mixer, enter electric slurry tank then, settlement separate between strength of electric field 0-3000V/cm, the denitrogenation slag is discharged from the slurry tank bottom, and denitrogenation oil flows out from electrofining slurry tank top, just prepares the good lubricant base of oxidation stability through sorbent material adsorption treatment back end hydrogenation under 80 ℃ of-130 ℃ of conditions of 0.1%-0.3% again.
3. with residual oil as lubricant base oil fraction through propane deasphalting, after furfural treatment or the phenol treating or the oil of hydrogenation after heat exchange to 50 ℃-130 ℃ with denitrfying agent thorough mixing in static mixer, enter electric slurry tank then, in strength of electric field is settlement separate between the 0-2000V/cm, the denitrogenation slag is discharged at the bottom of slurry tank, and denitrogenation oil flows out from electrofining slurry tank top, and the sorbent material through 0.5%-2% is just making the good lubricant base of oxidation stability after the adsorption treatment under 100 ℃ of-150 ℃ of conditions again.
4. with residual oil as lubricant base oil fraction through propane deasphalting, oil after furfural treatment or the phenol treating after heat exchange to 50 ℃-180 ℃ with denitrfying agent thorough mixing in static mixer, enter electric slurry tank then, in strength of electric field is settlement separate between the 0-2000V/cm, the denitrogenation slag is discharged at the bottom of slurry tank, and denitrogenation oil all flows out from electrofining sedimentation tank deck, and the sorbent material adsorption treatment back end hydrogenation under 100 ℃ of-150 ℃ of conditions through 0.5%-2% just makes the good lubricant base of oxidation stability again.
For then in said process, reducing dewaxing process with crude oil of low-coagulation production denitrogenation lubricant base.
The effect that the present invention reached is the method that has proposed a kind of new bright stock base oil, both reduced extraction temperature, energy efficient, can also cancel process furnace, save cost of equipment, adopt base oil alkali nitrogen of the present invention to take off to 0-300PPm from 50-1000PPm, and sulphur content decline is very low, generally only about 10%, and other physical and chemical index of denitrogenation lubricant base is constant substantially, but oxidation stability is significantly increased, and grand celebration paraffin base oil 500SN can improve arrival more than 200 minutes from 110 minutes.
Accompanying drawing and explanation thereof:
Fig. 1 is existing process flow diagram
Fig. 2 is first kind of process flow diagram of the present invention
Fig. 3 is second kind of process flow diagram of the present invention
Wherein:
The A-static mixer
B-electricity slurry tank
The C-filter
The D-process furnace
The E-interchanger
The F-fixed-bed adsorber
The 1-lubricant base
The 2-denitrfying agent
3-denitrogenation oil 3a-carclazyte 3b-sorbent material
4-denitrogenation slag
5-purified lubricant base
Grand celebration paraffin base oil 200S N dewaxes denitrogenation through furfural treatment, processes such as adsorbents adsorb, under 1: 250 condition of 70 ℃ of agent-oil ratios, sorbent material consumption 0.1%, 25 ℃ of adsorption temps, alkali nitrogen is reduced to 40PPm from 200PPm, and the rotary oxygen bomb value was brought up to 230 minutes from 110 minutes.Product meets the requirement of HVIS400SN.
Grand celebration paraffinic base 650SN dewaxes through furfural, denitrogenation, and processes such as adsorbents adsorb, under 1: 200 condition of the ratio of 80 ℃ of denitrfying agents and oil, sorbent material consumption 0.5%, 100 ℃ of adsorption temps, alkali nitrogen is reduced to 110ppm from 280ppm.Product meets the requirement of HVIS600SN.
Grand celebration paraffinic base residual oil is through propane deasphalting, dewaxing, furfural treatment, and denitrogenation, processing such as adsorbents adsorb, under 1: 100 condition of 95 ℃ of agent-oil ratios of temperature, sorbent material consumption 5.0%, 180 ℃ of adsorption temps, alkali nitrogen is reduced to 110ppm from 538ppm.Product meets the requirement of HVIS150BS.
The Nanyang intermediate base subtracts third fractional oil through furfural treatment, dewaxing, hydrogenation, denitrogenation, and processes such as adsorbents adsorb, wherein agent-oil ratio is 1: 150, sorbent material consumption 0.1%, 100 ℃ of adsorption temps, alkali nitrogen is reduced to 21ppm from 290ppm.Product meets the requirement of intermediate base industrial white oil.
The Nanyang intermediate base subtracts third fractional oil through furfural treatment, dewaxing, hydrogenation, denitrogenation, and processes such as adsorbents adsorb, hydrogenation, wherein agent-oil ratio is 1: 150, sorbent material consumption 0.2%, 100 ℃ of adsorption temps, alkali nitrogen is reduced to 11ppm from 290ppm.Product meets the requirement of intermediate base industrial white oil.
Embodiment 6
Grand celebration paraffinic base 650SN is through furfural treatment, dewaxing, and denitrogenation, processes such as fixed bed suction, under 1: 200 condition of 80 ℃ of agent-oil ratios, sorbent material is selected granulated active carbon for use, 100 ℃ of adsorption temps, alkali nitrogen is reduced to 92ppm from 280ppm.Product meets the requirement of HVIS650SN.
Embodiment 7
Grand celebration paraffinic base 75SN is after denitrogenation (agent-oil ratio 1: 500), by the adsorber of being filled by sorbent material, 40 ℃ of adsorption temps, the sorbent material consumption is 0.002%, alkali nitrogen is reduced to 2ppm by 60ppm, the ash content of lubricating oil, and colourity all touches the mark and requires also not contain fully the denitrfying agent slag.
Claims (2)
1, a kind of residual oil with perfectly straight wax oil or propane deasphalting passes through solvent treatment as raw material, dewaxing, denitrogenation, refining with adsorbents or repeated hydrogenation and produce lubricant base, it is characterized in that lubricant base (1) and denitrfying agent (2) flow into static mixer (A) at pipe-line blending, enter electric slurry tank (B) behind the thorough mixing, denitrogenation slag (4) is drained from electric slurry tank (B) bottom, denitrogenation oil (3) flow out from the top of electric slurry tank (B) with the sorbent material consumption by weight percentage ratio meter 0.01-5% enter interchanger (E) at pipe-line blending and be heated to normal temperature to 180 ℃, enter again that filter (C) is removed sorbent material and the residue that contains and obtain purified lubricant base (5).
2, a kind of residual oil with perfectly straight wax oil or propane deasphalting passes through solvent treatment as raw material, dewaxing, denitrogenation, refining with adsorbents or repeated hydrogenation and produce lubricant base, it is characterized in that lubricant base (1) and denitrfying agent (2) flow into static mixer (A) at pipe-line blending, enter electric slurry tank (B) behind the thorough mixing, denitrogenation slag (4) is drained from electric slurry tank (B) bottom, denitrogenation oil (3) flows out the fixed-bed adsorber (F) that enters filled with adsorbent (3b) from electric slurry tank (B) top, make denitrogenation oil under normal temperature to 180 ℃ condition, pass through fixed-bed adsorber (F), sorbent material consumption percentage ratio is by weight counted 0.001% to 5% of denitrogenation oil, and makes purified lubricant base (5).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 99122371 CN1118543C (en) | 1999-11-04 | 1999-11-04 | Refining basic oil of lubricating oil by denitrification |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 99122371 CN1118543C (en) | 1999-11-04 | 1999-11-04 | Refining basic oil of lubricating oil by denitrification |
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| Publication Number | Publication Date |
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| CN1253165A CN1253165A (en) | 2000-05-17 |
| CN1118543C true CN1118543C (en) | 2003-08-20 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN 99122371 Expired - Lifetime CN1118543C (en) | 1999-11-04 | 1999-11-04 | Refining basic oil of lubricating oil by denitrification |
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101560330B (en) * | 2009-06-01 | 2010-11-10 | 上海富沃地润滑油有限公司 | Method for producing environment-friendly rubber softening oil |
| CN102485842B (en) * | 2010-12-03 | 2014-01-15 | 中国石油天然气股份有限公司 | Method for processing fixed bed fishing coker gas oil |
| CN102485845B (en) * | 2010-12-03 | 2014-01-15 | 中国石油天然气股份有限公司 | Denitrogenation hydrogenation method for secondary processing diesel oil |
| CN102533319B (en) * | 2010-12-17 | 2014-06-04 | 中国石油天然气股份有限公司 | Method for removing basic nitrogen compounds in oils |
| CN110283620B (en) * | 2019-06-24 | 2021-09-24 | 盘锦北方沥青燃料有限公司 | Method for reducing water content of base oil |
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1999
- 1999-11-04 CN CN 99122371 patent/CN1118543C/en not_active Expired - Lifetime
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| CN1253165A (en) | 2000-05-17 |
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Owner name: CHINA PETROCHEMICAL CORPORATION Free format text: FORMER OWNER: WUHAN PETRO-CHEMICAL PLANT, CHINA PETRO-CHEMICAL CORP. Effective date: 20080328 |
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Effective date of registration: 20080328 Address after: Wuhan City, Hubei province Changqing District Changqing Road, China Petrochemical Plant Wuhan branch Patentee after: China Petrochemical Group Corp. Address before: No. 1, Changqing Road, Qingshan District, Hubei, Wuhan Patentee before: Wuhan Petro-Chemical Plant of China Petro-Chemical Corp. |
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Granted publication date: 20030820 |
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