CN1292049C - Novel tech. for sulfonating of low aromatic solvent oil and its liquid flow injecting sulfonation reacter - Google Patents
Novel tech. for sulfonating of low aromatic solvent oil and its liquid flow injecting sulfonation reacter Download PDFInfo
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- CN1292049C CN1292049C CN 200510039197 CN200510039197A CN1292049C CN 1292049 C CN1292049 C CN 1292049C CN 200510039197 CN200510039197 CN 200510039197 CN 200510039197 A CN200510039197 A CN 200510039197A CN 1292049 C CN1292049 C CN 1292049C
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Abstract
The present invention provides a novel technology for sulphonation of low arene solvent oil, which relates to a refining and purifying technology. The technology of the present invention is characterized in that SO3 is used as a treating agent to carry out sulphonation reaction to remove arene and other impurities in arene base oil; the arene base oil is jetted into a reactor to contact SO3 liquid which is sucked by negative pressure to react, the reaction temperature is from 20 to 50 DEG C, the molar ratio of SO3 to the impurities in the arene base oil is 1 to 1.2:1, and the reaction time is from 5 to 30 hours. The present invention enables jetted liquid flow to contact the SO3 liquid to finish continuous or intermittent sulphonation reaction in a fully enclosed mode, and then, the SO3 sufficiently reacts with the impurities in oil products; thus, the consumption of the SO3 is greatly reduced, the product quality is improved, the environmental pollution in the process of sulphonation is avoided, and good economical and social benefits are obtained.
Description
Technical field
The present invention relates to a kind of refining purifying technique, being meant a kind of is that treatment agent carries out sulfonation reaction and removes the aromatic hydrocarbons in the aromatic hydrocarbon base oil and the technology of other impurity with SO3, and the liquid stream that uses in this technology jet sulfonation reactor also is provided simultaneously.
Technical background
Though the base oil as lube stock is to extract through rectifying, but also contain many detrimental impurity such as aromatic hydrocarbons in it, directly use it in industry or other (as the food medicine etc.) industry lubricated, solvent oil uses cannot, must make with extra care impurity elimination, as Liquid Paraffin (abbreviation white oil) be by the light lubricating oil fraction through oleum repeatedly wash the extracting of (sulfonation) ethanol be refined into colourless, tasteless, do not have and to smell unreactiveness, to the stabile product of light.Oleum method of sulfonation also is traditional process for purification of other aromatic hydrocarbon base oil, and this method SO3 consumes greatly, and efficient is low, and environmental pollution is serious.
Summary of the invention
The present invention is just in order to overcome above-mentioned deficiency, provide that a kind of SO3 consumes less, environmentally safe, sulfonating of low aromatic solvent oil novel process that decon efficient is high, the totally-enclosed liquid stream ejection-type sulfonation reactor that also has this novel process to adopt that provides simultaneously, main innovation is that aromatic hydrocarbon base oil is spurted into reaction tubes finishes sulfonation reaction with the SO3 gas-to-liquid contact that sprays the negative pressure suction that forms, until emitting qualified low aromatic solvent naphtha.Specifically be achieved like this: the sulfonating of low aromatic solvent oil novel process, it is characterized in that aromatic hydrocarbon base oil is through spraying the SO3 gas-liquid contact reaction that sucks with negative pressure in reactor, temperature of reaction is 20-50 ℃, the mol ratio of impurity is 1-1.2 in SO3 and the aromatic hydrocarbon base oil: 1, and the reaction times is 5-30 hour.
This technology can adopt batch production, also can continuous production.In order to obtain satisfied sulfonation effect, technology stage by stage/classification carries out.The number of stages of rhythmic reaction and the progression in the successive reaction are according to aromatic hydrocarbon base oil fractional composition, foreign matter content and treatment capacity decision, each the stage/SO3 addition and temperature of reaction at different levels change in gradient, the molar ratio of impurity level is in the addition of per stage/every grade of SO3 and the aromatic hydrocarbon base oil: 0-0.7: 1.
This technology gas-liquid two-phase carries out violent contact in reactor, release of heat has been quickened reaction process, carries out under the temperature condition of optimum for keeping reaction process, reaction heat will in time shift out through heat-exchanger rig, and this heat-exchanger rig can be coil tube type, shell and tube etc.
If process using rhythmic reaction mode, the temperature of reaction in each stage increases progressively gradually, and the add-on of the SO3 in each time in stage reduces gradually, and reaction does not feed SO3 at last, sprays by fluidic to discharge dissolved SO3 in it.
Best method is to adopt the continuous production method, form by some stage reactor serial connections, aromatic hydrocarbon base oil and SO3 gas flow mode are adverse current, smooth and easy in order to guarantee air-flow adverse current in each stage reactor, vacuum delivery in each stage reactor changes in gradient, and first and last stage pressure difference is controlled between the 1.10Kpa-20.0Kpa.
Some stage reactors of serial connection, the first step is export of finished oil end, SO3 first entrance end, and final stage is aromatic hydrocarbon base oil entrance end, SO3 tail gas exit end, and the addition gradient of temperature of reaction at different levels and SO3 is successively decreased, vacuum tightness increases progressively; First step reactor also can be aromatic hydrocarbon base oil entrance end, SO3 tail gas exit end, and final stage is first entrance end of solvent oil exit end, SO3, and the addition of temperature of reaction at different levels and SO3 then is that gradient increases progressively, vacuum tightness is successively decreased in gradient.
For the SO3 that is dissolved in the liquid stream after the complete reaction is overflowed, solvent fluid stream after the sulfonation reaction can freely overflow SO3 through injection again, be about to liquid after the sulfonation reaction and circulate and finish the work of removing in the injection reactor of the obstructed SO3 air-flow set up, make SO3 contained in the finished product as far as possible little.
The casing that is used for the liquid stream jet sulfonation reactor of sulfonation reaction is built-in with reaction tubes, be furnished with heat exchanger around the reaction tubes, described reaction tubes one end is near bottom half, the other end connects the liquid flow injection head outside casing, bottom half is taper, the tapered bottom mouth is the jetting fluid relief outlet, is equipped with the circulation tube of bleeding between casing top and liquid flow injection head, and the circulation tube of bleeding links to each other with inlet pipe in addition.The liquid jet orifice of flowing through enters the reaction mouth of pipe, spray the negative pressure that forms and suck SO3 gas simultaneously, gas-liquid is the strong collision reaction in reaction tubes, the heat that discharges is discharged by the intravital heat exchanger of case, liquid stream reaction in the pipe is laggard goes in the casing, heat exchanger is except that cooling effect, also play guide functions, make liquid stream in casing, produce collision rotation and the further contact reacts of air-flow, refrigerative liquid stream is extracted out by the tapered bottom mouth, and unreacted SO3 gas comes together in casing top separated space and is inhaled into once more in the liquid flow injection head by the circulation tube of bleeding.
Have material above the sulfonation reactor casing and add mouth and gauge port, have gas phase on the casing of side and extract mouth, liquid phase extraction mouth out and be equipped with liquid level meter, conical lower portion has thief hole, to finish the real-time detection and the reaction conditions of each material in the reactor is controlled.
The present invention utilizes liquid stream to spray the totally enclosed continuously or intermittently sulfonation reaction of finishing with the SO3 gas-to-liquid contact, make SO3 fully and the impurity in the oil product react, greatly reduce the consumption of SO3, improved quality product, avoided in the sulfonation process pollution of environment has been obtained good economic benefit and social benefit.
Description of drawings
The structural representation of Fig. 1 sulfonation reactor of the present invention.
Fig. 2 is an intermittently sulfonating reaction process schema of embodiment 1.
Fig. 3 is embodiment 3 continuous sulfonating reaction process schemas.
Embodiment
Embodiment 1, aromatic hydrocarbon base oil is squeezed in the reaction tubes of liquid stream injection reactor through pump, simultaneously SO3 gas is sucked and carry out the intense mixing reaction, gas-liquid also continues reaction in the reactor casing, and by water conservancy diversion cartridge type coil heat exchanger, reaction heat is taken out of assurance sulfonation reaction at a certain temperature, gas phase SO3 non-reacted parts is overflowed from liquid stream main body and is entered reactor top separated space in reactor, simultaneously for guaranteeing certain SO3, phase concentrations adds the fresh SO3 gas of specified amount in different time sections, fresh SO3 inlet of change and temperature of reaction are carried through to the end sulfonation reaction in the time in stage that is reflected at regulation of going round and beginning again, each time in stage interior reaction temperature gradient increases progressively, SO3 inlet gradient is successively decreased last to zero, the situation of analyzing per sample in time changes operational stage, make sulfonation reaction at the end in the tail gas SO3 content very low.
Process conditions is:
Aromaticity content is 5.8% (WT%) in the raw material
Aromaticity content is 0.5%-1.0% (WT%) in the product
The sulfonation time: 19 hours
Sulfonation temperature 25-50 ℃
The final total molar ratio of SO3 and aromatic hydrocarbon base oil impurity during terminal point: 1.2: 1
The placed in-line continuous sulfonation of embodiment 2, three stills, the first step are export of finished oil end, SO3 first entrance end, and the third stage is aromatic hydrocarbon base oil entrance end, SO3 tail gas exit end, and each inter-stage thermograde is successively decreased, vacuum tightness increases progressively, the SO3 addition successively decreases.Process conditions is:
Aromaticity content is 7.2% (WT%) in the raw material
Aromaticity content is 0.3%-0.7% (WT%) in the product
The sulfonation time: 20 hours
Sulfonation temperature 20-35 ℃
The total molar ratio of SO3 and aromatic hydrocarbon base oil impurity during terminal point: 1.1: 1
The finished product low aromatic solvent naphtha that the first step is come out in this technology also can be put into the liquid stream jet sulfonation reactor of a no SO3 feeding amount, dissolved SO3 in jetting action effusion liquid phase.
Illustrate: according to the foreign matter content of aromatic hydrocarbon base oil, can design the continuous processing flow process that different steps is counted batch technology flow process and different progression, corresponding increase of reaction times or shortening, the general sulfonation time was controlled between 5-30 hour.
Claims (8)
1. sulfonating of low aromatic solvent oil novel process, it is characterized in that aromatic hydrocarbon base oil is through spraying the SO3 gas-liquid contact reaction that sucks with negative pressure in reactor, temperature of reaction is 20-50 ℃, the mol ratio of impurity is 1-1.2 in SO3 and the aromatic hydrocarbon base oil: 1, reaction times is 5-30 hour, with the production of intermittence/continuous processing, each stage/successive reaction of rhythmic reaction SO3 addition and temperature of reaction at different levels changes in gradient, and the molar ratio of impurity level is in the addition of per stage/every grade of SO3 and the aromatic hydrocarbon base oil: 0-0.7: 1.
2. sulfonating of low aromatic solvent oil novel process according to claim 1 is characterized in that the temperature of reaction in each stage increases progressively gradually in the rhythmic reaction, and the add-on of the SO3 in each time in stage reduces gradually.
3. sulfonating of low aromatic solvent oil novel process according to claim 1 is characterized in that successive reaction is formed by some stage reactor serial connections, and aromatic hydrocarbon base oil and SO3 gas flow mode are adverse current.
4. sulfonating of low aromatic solvent oil novel process according to claim 3 is characterized in that the vacuum delivery in each stage reactor changes in gradient, and first and last stage pressure difference is controlled between the 1.10Kpa-20.0Kpa.
5. sulfonating of low aromatic solvent oil novel process according to claim 4, it is characterized in that some stage reactors of being connected in series, the first step is export of finished oil end, SO3 first entrance end, final stage is aromatic hydrocarbon base oil entrance end, SO3 tail gas exit end, and the addition gradient of temperature of reaction at different levels and SO3 is successively decreased, vacuum tightness increases progressively.
6. sulfonating of low aromatic solvent oil novel process according to claim 4, it is characterized in that some stage reactors of being connected in series, the first step is aromatic hydrocarbon base oil entrance end, SO3 tail gas exit end, final stage is first entrance end of solvent oil exit end, SO3, and the addition of temperature of reaction at different levels and SO3 then is that gradient increases progressively, vacuum tightness is successively decreased in gradient.
7. flow jet sulfonation reactor according to the described sulfonating of low aromatic solvent oil novel process of claim 1-6 with liquid, it is characterized in that the reactor casing is built-in with reaction tubes, be furnished with heat exchanger around the reaction tubes, described reaction tubes one end is near bottom half, the other end connects the liquid flow injection head outside casing, bottom half is taper, and the tapered bottom mouth is the jetting fluid relief outlet, be equipped with the circulation tube of bleeding between casing top and liquid flow injection head, the circulation tube of bleeding links to each other with inlet pipe in addition.
8. liquid stream jet sulfonation reactor according to claim 7, it is characterized in that sulfonation reactor casing top has material and adds mouth and gauge port, have gas phase on the casing of side and extract mouth, liquid phase extraction mouth out and be equipped with liquid level meter, conical lower portion has thief hole.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510039197 CN1292049C (en) | 2005-04-30 | 2005-04-30 | Novel tech. for sulfonating of low aromatic solvent oil and its liquid flow injecting sulfonation reacter |
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| Application Number | Priority Date | Filing Date | Title |
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| CN 200510039197 CN1292049C (en) | 2005-04-30 | 2005-04-30 | Novel tech. for sulfonating of low aromatic solvent oil and its liquid flow injecting sulfonation reacter |
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| CN1693422A CN1693422A (en) | 2005-11-09 |
| CN1292049C true CN1292049C (en) | 2006-12-27 |
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| CN 200510039197 Expired - Fee Related CN1292049C (en) | 2005-04-30 | 2005-04-30 | Novel tech. for sulfonating of low aromatic solvent oil and its liquid flow injecting sulfonation reacter |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101654627B (en) * | 2009-09-15 | 2012-06-27 | 江苏高科石化股份有限公司 | Production method of organic silicon solvent |
| CN105254542A (en) * | 2015-10-30 | 2016-01-20 | 浙江赞宇科技股份有限公司 | Method and device for producing leather fatliquoring agent by liquid SO3 sulfonation |
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