CN104611008A - Equipment and method for producing environment-friendly rubber filling oil - Google Patents
Equipment and method for producing environment-friendly rubber filling oil Download PDFInfo
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- CN104611008A CN104611008A CN201510024673.5A CN201510024673A CN104611008A CN 104611008 A CN104611008 A CN 104611008A CN 201510024673 A CN201510024673 A CN 201510024673A CN 104611008 A CN104611008 A CN 104611008A
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G53/00—Treatment of hydrocarbon oils, in the absence of hydrogen, by two or more refining processes
- C10G53/02—Treatment of hydrocarbon oils, in the absence of hydrogen, by two or more refining processes plural serial stages only
- C10G53/04—Treatment of hydrocarbon oils, in the absence of hydrogen, by two or more refining processes plural serial stages only including at least one extraction step
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K5/00—Use of organic ingredients
- C08K5/01—Hydrocarbons
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L21/00—Compositions of unspecified rubbers
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Abstract
The invention provides equipment and a method for producing environment-friendly rubber filling oil. The equipment for producing the environment-friendly rubber filling oil comprises an extraction tower, an extract oil refining tank, a raffinate stripping tower and an environment-friendly rubber filling oil tank, wherein an extract oil raffinate pipeline is arranged between the extract oil refining tank and the extraction tower and comprises an extract oil raffinate outlet and an extract oil raffinate inlet, the extract oil raffinate outlet is arranged at the top of the extract oil refining tank, the extract oil raffinate inlet is arranged on the extraction tower and has the highest position and the lowest position, the highest position is located between a solvent inlet and a raw oil inlet, the distance between the highest position and the solvent inlet is twice that between the highest position and the raw oil inlet, and the lowest position is the position where the raw oil inlet is located. The content of environment-friendly monocyclic and dicyclic aromatic hydrocarbon in the refined oil produced by the equipment with the method can be increased, that is, the quality of the produced environment-friendly rubber filling oil can be improved, and meanwhile, the yield of the environment-friendly rubber filling oil is increased.
Description
Technical field
The invention belongs to technical field of petrochemical industry, be specifically related to a kind of apparatus and method for producing environment-friendly rubber extending oil.
Background technology
In the process of manufacture of the rubber items such as tire, for improving the processing characteristics of sizing material, usually need to add a certain amount of rubber filling oil.Rubber filling oil is one of important raw and processed materials of Rubber processing, be divided into aromatic hydrocarbons type, cycloalkanes type and alkane type, wherein to have density large for aromatic hydrocarbons type oil, viscosity is large, affinity is good, the feature that processing characteristics is excellent, there is the consistency good with rubber and the high-performances such as the good anti-slippery of tire can be given, such oil with the extraction oil (DAE) of lubricating oil solvent for representative, wherein containing a large amount of polycyclic arene compounds, polycyclic aromatic hydrocarbons has carcinogenic, the toxics such as damage reproductive system, thus used by some developed countries limitation, European Union has issued 2005/69/EC instruction on December 9th, 2005, require from 1 day January in 2010, all enter EU market tire and rubber item in, the 8 kinds of harmful polycyclic aromatic hydrocarbons total amounts every kilogram be listed in the extending oil used can not more than 10 milligrams, wherein benzopyrene (BaP) content every kilogram can not more than 1 milligram.
Environment-friendly rubber extending oil mainly contains following three kinds: TDAE (process aromatic hydrocarbon oil), MES (also known as shallow oil pumping) and NAP (naphthenic oil) both at home and abroad at present.TDAE be to lubricating oil solvent extract out oil re-refine removing poisonous polycyclic aromatic hydrocarbons after produce; MES forms by dewaxing after the either shallow solvent treatment of paraffinic crude distillate or hydrofining again; NAP is formed through solvent treatment or hydrofining by naphthenic base crude distillate.The composition of TDAE is extracted oils rubber filling oil composition out with lubricating oil solvent and is differed little, and aromaticity content is high, good with rubber compatibility; In the composition of MES and NAP, total aromaticity content is relatively low, with rubber compatibility difference.
With regard to domestic market, along with the continuous increase of auto output, tire output is also always in very fast ascendant trend.Along with the increase that the well-known tire enterprise in the world is invested at home, the trend of the increase of domestic large-lot producer radial export volume and the Green Product of development environment close friend, substitute aromatic hydrocarbon oil and must cause great concern as the environment-friendly rubber extending oil being applied to oil extend rubber and tire production, its demand also can increase.
In the production of environment-friendly rubber extending oil, propose some production methods both at home and abroad, the Chinese invention patent application being CN101597512A as publication number discloses a kind of method of producing environment-friendly rubber extending oil, the method comprises the steps: l) to subtract three line distillates for stock oil, carry out furfural extraction, once extracted out oil; 2) by step l) the once extraction oil that obtains carries out the extracting of furfural secondary, and the secondary fine liquefaction obtained is environment-friendly rubber extending oil.Publication number is that the Chinese invention patent application of CN101597513A discloses a kind of environment-friendly rubber extending oil and preparation method thereof, the method of what this invention provided prepare environment-friendly rubber extending oil, comprise the steps: l) to subtract three line distillates for stock oil, carry out furfural extraction, obtain primary purification oil; 2) by step l) the primary purification oil that obtains carries out the extracting of furfural secondary, and the secondary obtained is extracted oil out and is environment-friendly rubber extending oil.Above two patents are that TDAE class environment-friendly rubber extending oil produced by stock oil with distillate, do not illustrate how to produce NAP class environment-friendly rubber extending oil, also do not illustrate with general lubricating oil solvent extraction oil as how stock oil produces TDAE class environment-friendly rubber extending oil.
Adopt existing solvent treatment technology, if make Ppolynuclear aromatic hydrocarbon (PCA) content of treated oil and 8 kinds of harmful aromatics total contents meet the requirement of European Council Regulation 2005/69/EC environmental protection index, then treated oil virtue carbon content is low, can not meet the requirement of tyre industry to environment-friendly rubber extending oil use properties; If make treated oil virtue carbon content meet the requirement of tyre industry to environment-friendly rubber extending oil use properties, then Ppolynuclear aromatic hydrocarbon (PCA) content of treated oil and 8 kinds of harmful aromatics total contents cannot meet the requirement of European Council Regulation 2005/69/EC environmental protection index.Therefore, urgent expectation a kind of tire environment-friendly rubber extending oil of exploitation and working method thereof.
Summary of the invention
The object of the invention is on prior art basis, realize few ring environment-friendly aromatic that can retain a great deal of, poisonous polycyclic aromatic hydrocarbons can be removed to the utmost again, produce the apparatus and method for of the environment-friendly rubber extending oil meeting European Council Regulation requirement.
The invention provides a kind of equipment producing environment-friendly rubber extending oil, comprise extraction tower, extract oil refining tank, raffinate stripping tower and environment-friendly rubber out and fill oil tank, described extraction tower comprises the stock oil entrance being arranged at its underpart, the colvent inlet being arranged at its top, the raffinate outlet that is arranged at an Extract outlet bottom it, is arranged at its top, described extraction oil refining tank comprises an Extract entrance in portion disposed therein, and described Extract outlet is connected with a described Extract entrance, described raffinate stripping tower comprises the raffinate entrance being arranged at its underpart and the environment-friendly rubber extending oil outlet be arranged at bottom it, and described raffinate outlet is connected with described raffinate entrance, described environment-friendly rubber filling oil tank exports with described environment-friendly rubber extending oil and is connected, wherein, there is between described extraction oil refining tank and described extraction tower an extraction oil raffinate pipeline, described extraction oily raffinate pipeline comprises to be extracted the outlet of oily raffinate out and extracts oily raffinate entrance out, the outlet of described extraction oily raffinate is arranged at the top of described extraction oil refining tank, described extraction oily raffinate entrance to be arranged on described extraction tower and to have extreme higher position and extreme lower position, described extreme higher position is between described colvent inlet and described feed(raw material)inlet, and the distance of described extreme higher position and described colvent inlet is the twice of the distance of described extreme higher position and described stock oil entrance, described extreme lower position is the position at described stock oil entrance place.
The equipment of above-mentioned production environment-friendly rubber extending oil, wherein, also comprise solvent seasoning tower, wet solvent entrance and solvent outlet after being arranged at bottom it drying after described solvent seasoning tower comprises the stripping being arranged at its top, described raffinate stripping tower also comprises the first wet solvent outlet being arranged at its top, described first wet solvent outlet is connected with wet solvent entrance after described stripping, and after described drying, solvent outlet is connected with described colvent inlet.
The equipment of above-mentioned production environment-friendly rubber extending oil, wherein, also comprise secondary Extract evaporator tower, described secondary Extract evaporator tower comprises the secondary Extract entrance being arranged at its underpart, solvent outlet and secondary Extract outlet after being arranged at bottom it evaporation after being arranged at the evaporation at its top, described solvent seasoning tower comprises colvent inlet after the evaporation in portion disposed therein, described extraction oil refining tank also comprises the secondary Extract outlet be arranged at bottom it, described secondary Extract outlet is connected with described secondary Extract entrance, after described evaporation, the outlet of secondary Extract is connected with a described Extract entrance, after described evaporation, solvent outlet is connected with colvent inlet after described evaporation.
The equipment of above-mentioned production environment-friendly rubber extending oil, wherein, also comprise secondary extract stripper and secondary extraction oil tank, after described secondary extract stripper comprises the evaporation being arranged at its underpart, secondary Extract entrance and the secondary be arranged at bottom it extract oil export out, after described evaporation, the outlet of secondary Extract is connected with secondary Extract entrance after described evaporation, and described secondary extraction oil export is extracted oil tank out with described secondary and is connected.
The equipment of above-mentioned production environment-friendly rubber extending oil, wherein, described secondary extract stripper also comprises the second wet solvent outlet being arranged at its top, and described second wet solvent outlet is connected with wet solvent entrance after described stripping.
The equipment of above-mentioned production environment-friendly rubber extending oil, wherein, described secondary is extracted oil export out and is connected with a described Extract entrance.
The present invention also provides a kind of method of producing environment-friendly rubber extending oil, wherein, adopts the equipment of above-mentioned production environment-friendly rubber extending oil to refine, comprises the steps:
Solvent enters described extraction tower from the top of described extraction tower, stock oil enters described extraction tower from the bottom of described extraction tower and carries out countercurrent extraction, the Extract that extracting obtains enters described extraction oil refining tank and refines, the refining extraction oil raffinate obtained is back to described extraction tower by described extraction oily raffinate pipeline, the raffinate that in described extraction tower, extracting obtains enters described raffinate stripping tower, and the environment-friendly rubber extending oil that raffinate obtains after carrying out stripping desolvation enters described environment-friendly rubber and fills oil tank.
The method of above-mentioned production environment-friendly rubber extending oil, wherein, the wet solvent that described raffinate stripping tower stripping goes out enters described solvent seasoning tower through condensation and carries out drying, and the dried described solvent of described solvent seasoning tower bottom enters described extraction tower and recycles.
The method of above-mentioned production environment-friendly rubber extending oil, wherein, in described extraction oil refining tank, the refining secondary Extract obtained obtains the secondary Extract containing a small amount of solvent after pervaporation, and the secondary Extract containing a small amount of solvent obtains secondary and extracts oil out after stripping.
The method of above-mentioned production environment-friendly rubber extending oil, wherein, part secondary extracts oil out or part mixes with the Extract that described extraction tower extracting obtains through the secondary Extract of evaporation containing a small amount of solvent, enters described extraction oil refining tank and refines.
The method of above-mentioned production environment-friendly rubber extending oil, wherein, the solvent removed during the evaporation of secondary Extract and the wet solvent removed when evaporation contains the secondary Extract stripping of a small amount of solvent enter described solvent seasoning tower respectively and carry out drying.
The method of above-mentioned production environment-friendly rubber extending oil, wherein, the operational condition of described extraction oil refining tank is: the secondary mixed with Extract extracts oil out or through evaporate the amount of secondary Extract that contains a small amount of solvent and the mass ratio of stock oil is 0.2-1.5:1, the temperature of extracting oil refining tank out is 40 DEG C-50 DEG C, and the residence time that Extract stays in described extraction oil refining tank is 50-120 minutes; The residence time that the mixed solution that part secondary extraction oil or part obtain after the secondary Extract of evaporation containing a small amount of solvent mixes with an Extract stays in described extraction oil refining tank is 50-120 minutes.
The method of above-mentioned production environment-friendly rubber extending oil, wherein, described stock oil is lubricating oil distillate or solvent-extracted oil, and described solvent is furfural.
The method of above-mentioned production environment-friendly rubber extending oil, wherein, the open flash point of described lubricating oil distillate or described solvent-extracted oil is not less than 200 DEG C, and 100 DEG C of kinematic viscosity are not less than 13.0mm
2/ s, C
avalue is not less than 13.0%, and zero pour is not higher than 30 DEG C, if zero pour is higher than 30 DEG C, carries out dewaxing treatment.
The method of above-mentioned production environment-friendly rubber extending oil, wherein, described furfural extraction condition is, described extraction tower tower top temperature 60 DEG C-90 DEG C, described extraction tower column bottom temperature is 40 DEG C-60 DEG C, and the mass ratio of described furfural and described lubricating oil distillate or described solvent-extracted oil is 1.0-2.5:1.
The present invention is by carrying out secondary refining to once extracting oil out, few Polycyclic aromatic hydrocarbons of once extracting out in oil is reclaimed and makes it return extraction tower, compare with usual vehicle extracting like this, the content of the few ring environment-friendly aromatic in the treated oil obtained can increase, the quality of the environment-friendly rubber extending oil namely obtained can improve, and improves the yield of environment-friendly rubber extending oil simultaneously.
Describe the present invention below in conjunction with the drawings and specific embodiments, but not as a limitation of the invention.
Accompanying drawing explanation
Fig. 1 is a kind of structure diagram producing the equipment of environment-friendly rubber extending oil of the present invention;
Fig. 2 is a kind of process flow sheet producing the method for environment-friendly rubber extending oil of the present invention.
Wherein, Reference numeral
100 extraction towers
110 stock oil entrances
120 colvent inlets
130 Extract outlets
140 raffinate outlets
200 extract oil refining tank out
210 Extract entrances
220 2 Extract outlets
300 raffinate stripping towers
310 raffinate entrances
320 environment-friendly rubber extending oil outlets
330 first wet solvent outlets
400 environment-friendly rubbers fill oil tank
500 extract oily raffinate pipeline out
510 extract the outlet of oily raffinate out
520 extract oily raffinate entrance out
600 solvent seasoning towers
Wet solvent entrance after 610 strippings
620 dry rear solvent outlet
Colvent inlet after 630 evaporations
700 2 Extract evaporator towers
710 2 Extract entrances
Solvent outlet after 720 evaporations
Secondary Extract outlet after 730 evaporations
800 2 extract strippers
Secondary Extract entrance after 810 evaporations
Extract oil export out 820 2 times
830 second wet solvent outlets
Extract oil tank out 900 2 times
4 raffinates
5 Extracts
7 extract oily raffinate out
8 two Extracts
10 solvents removed
11,12,13 containing the secondary Extract of a small amount of solvent
14, oil is extracted out 16,17 2 times
15, the wet solvent that goes out of 18 strippings
19 environment-friendly rubber extending oils
Embodiment
Below in conjunction with the drawings and specific embodiments, technical solution of the present invention is described in detail, further to understand object of the present invention, scheme and effect, but not as the restriction of claims protection domain of the present invention.
The present invention with lubricating oil distillate or its hydrogenation deacidification oil or solvent-extracted oil for raw material, carry out in counter-current extraction tower, use furfural is solvent, solvent enters extraction tower from the top of extraction tower, stock oil enters extraction tower from the bottom of extraction tower, adopt part secondary to extract oil out or mix with the Extract flowed out bottom extraction tower through the secondary Extract of evaporation containing a small amount of solvent, enter extraction oil refining tank to refine, the raffinate extracting oil refining tank top out returns extraction tower, extract the secondary Extract of oil refining pot bottom out through evaporation, obtain secondary after stripping recycling design and extract oil out, the raffinate at extraction tower top obtains solvent-refined oil and is environment-friendly rubber extending oil after stripping recycling design.
This invention takes and carry out secondary refining to once extracting oil out, the extraction obtained oil raffinate is returned the way of extraction tower, solvent extraction with routine is compared, few Polycyclic aromatic hydrocarbons of extracting out in oil is equivalent to reclaim, simultaneously because the composition extracting oily raffinate out is special, it returns in extraction tower and makes the extracting of extraction tower inside create useful effect, the yield of the i.e. environment-friendly rubber extending oil of raffinating oil can be improved under the same conditions further, secondary extracts the yield reduction of oil out simultaneously, few ring content that secondary is extracted out in oil is lower, polycyclic aromatic hydrocarbon content is higher, namely the environmental protection component in raw material obtains sufficient recovery (environmental protection component enters in treated oil mostly), improve the content of aromatic hydrocarbons in environment-friendly rubber extending oil simultaneously further, adopt the method to compare with Conventional solvents is refining, ensureing that under the condition that environmental protection index is qualified, the yield of environment-friendly rubber extending oil is improved largely, namely adopt the efficiency the method increasing solvent extraction, be equivalent to the selectivity that improve solvent.
Particularly, consult Fig. 1, the equipment of production environment-friendly rubber extending oil of the present invention comprises extraction tower 100, extraction oil refining tank 200, raffinate stripping tower 300, environment-friendly rubber filling oil tank 400 and extracts oily raffinate pipeline 500 out.Extraction tower 100 comprises: be arranged at the stock oil entrance 110 of the bottom of extraction tower 100, be arranged at the colvent inlet 120 on extraction tower 100 top, be arranged at an Extract outlet 130 bottom extraction tower 100 and be arranged at the raffinate outlet 140 at extraction tower 100 top.Extract oil refining tank 200 out to comprise: be arranged at the Extract entrance 210 extracted out in the middle part of oil refining tank 200, wherein, an Extract outlet 130 on extraction tower 100 is connected with the Extract entrance 210 extracted out on oil refining tank 200.Raffinate stripping tower 300 comprises: the raffinate entrance 310 being arranged at raffinate stripping tower 300 bottom and the environment-friendly rubber extending oil outlet 320 be arranged at bottom raffinate stripping tower 300, wherein, the raffinate outlet 140 on extraction tower 100 is connected with the raffinate entrance 310 on raffinate stripping tower 300; Environment-friendly rubber filling oil tank 400 exports 320 with the environment-friendly rubber extending oil on raffinate stripping tower 300 and is connected.Extract oily raffinate pipeline 500 out to be arranged between extraction oil refining tank 200 and extraction tower 100, the setting of extracting oily raffinate pipeline 500 out can improve the content of few Polycyclic aromatic hydrocarbons in treated oil, improves yield and the quality of product.
Extract oily raffinate pipeline 500 out comprise the oily raffinate outlet 510 of extraction and extract oily raffinate entrance 520 out, extract oily raffinate outlet 510 out and be arranged at the top of extracting oil refining tank 200 out, extract oily raffinate entrance 520 out to be arranged on extraction tower 100 and there is an extreme higher position, extreme higher position is between colvent inlet 120 and stock oil entrance 110, and the distance of extreme higher position and colvent inlet 120 is twices of the distance of extreme higher position and stock oil entrance 110.
Extract oily raffinate entrance 520 out and also have an extreme lower position, extreme lower position is the position at stock oil entrance 110 place.
Extract yield, C that position that oily raffinate returns extraction tower can affect environment-friendly rubber extending oil out
avalue and the environmental-protecting performance of product, extract out oily raffinate more than described extreme higher position and below extreme lower position time, affect the environmental-protecting performance of product or yield, the C of product
athe increase rate of value diminishes, and therefore the best position returning extraction tower is between described extreme higher position and extreme lower position, comprises extreme higher position and extreme lower position.
As shown in Figure 1, the equipment of production environment-friendly rubber extending oil of the present invention also comprises solvent seasoning tower 600, secondary Extract evaporator tower 700, secondary extract stripper 800 and secondary extraction oil tank 900.
Solvent seasoning tower 600 comprises: wet solvent entrance 610 and solvent outlet 620 after being arranged at bottom solvent seasoning tower 600 drying after being arranged at the stripping on solvent seasoning tower 600 top.Raffinate stripping tower 300 also comprises: the first wet solvent outlet 330 being arranged at raffinate stripping tower 300 top, the first wet solvent outlet 330 on raffinate stripping tower 300 is connected with wet solvent entrance 610 after the stripping on solvent seasoning tower 600, and after the drying on solvent seasoning tower 600, solvent outlet 620 is connected with the colvent inlet 120 on extraction tower 100.
Secondary Extract evaporator tower 700 comprises: the secondary Extract entrance 710 being arranged at secondary Extract evaporator tower 700 bottom, be arranged at secondary Extract evaporator tower 700 top evaporation after solvent outlet 720 and secondary Extract outlet 730 after being arranged at bottom secondary Extract evaporator tower 700 evaporation.Solvent seasoning tower 600 also comprises: be arranged at colvent inlet 630 after the evaporation in the middle part of solvent seasoning tower 600.Extract oil refining tank 200 out also to comprise: be arranged at the secondary Extract outlet 220 of extracting out bottom oil refining tank 200, the secondary Extract outlet 220 of extracting out on oil refining tank 200 is connected with the secondary Extract entrance 710 on secondary Extract evaporator tower 700, after evaporation on secondary Extract evaporator tower 700, secondary Extract outlet 730 is connected with the Extract entrance 210 extracted out on oil refining tank 200, and after the evaporation on secondary Extract evaporator tower 700, solvent outlet 720 is connected with colvent inlet 630 after the evaporation on solvent seasoning tower 600.
Secondary extract stripper 800 comprises: after being arranged at the evaporation of secondary extract stripper 800 bottom, secondary Extract entrance 810 and the secondary be arranged at bottom secondary extract stripper 800 extract oil export 820 out, after evaporation on secondary Extract evaporator tower 700, secondary Extract outlet 730 is connected with secondary Extract entrance 810 after the evaporation on secondary extract stripper 800, and the secondary extraction oil export 820 on extract stripper 800 is extracted oil tank 900 out with secondary and is connected.
Secondary extract stripper 800 also comprises: the second wet solvent outlet 830 being arranged at secondary extract stripper 800 top, and the second wet solvent outlet 830 on secondary extract stripper 800 is connected with wet solvent entrance 610 after the stripping on solvent seasoning tower 600.
Secondary on secondary extract stripper 800 is extracted oil export 820 out and is connected with the Extract entrance 210 extracted out on oil refining tank 200.
The concrete enforcement of the method for production environment-friendly rubber extending oil of the present invention is as shown in Figure 2: stock oil adopts lubricating oil distillate or its hydrogenation deacidification oil or solvent-extracted oil and enters extraction tower 100 from the stock oil entrance 110 of extraction tower 100 bottom, solvent adopts furfural and enters extraction tower 100 from the colvent inlet 120 on extraction tower 100 top, stock oil in extraction tower 100 after solvent treatment, the Extract 5 flowed out bottom extraction tower 100, extract the secondary Extract 8 flowed out bottom oil refining tank 200 out and remove most of solvent through secondary Extract evaporator tower 700, the solvent 10 removed enters the middle part of solvent seasoning tower 600, the secondary Extract 11 containing a small amount of solvent flowed out bottom secondary Extract evaporator tower 700 is divided into two portions 12 and 13, the Extract 5 flowed out bottom the secondary Extract 12 of a part containing a small amount of solvent and extraction tower 100 is mixed into extracts oil refining tank 200 out, the extraction oil raffinate 7 that the top of extracting oil refining tank 200 out is flowed out returns extraction tower 100 by extracting oily raffinate pipeline 500 out, the secondary Extract 13 containing a small amount of solvent flowed out bottom secondary Extract evaporator tower 700 enters secondary extract stripper 800, the wet solvent 15 that stripping goes out enters solvent seasoning tower 600 top through condensation removes moisture as top backflow, dry solvent bottom solvent seasoning tower 600 enters extraction tower 100 to recycle.The raffinate 4 at extraction tower 100 top enters raffinate stripping tower 300, the wet solvent 18 that stripping goes out enters solvent seasoning tower 600 top through condensation removes moisture as top backflow, dry solvent bottom solvent seasoning tower 600 recycles, and flows out environment-friendly rubber extending oil 19 bottom raffinate stripping tower 300.Bottom secondary extract stripper 800, secondary is extracted oil out and 14 is divided into two portions 16 and 17, and a part of secondary is extracted oil 16 out and entered secondary as byproduct and extract oil tank 900 out, and a part of secondary is extracted oil 17 out and once extracted oily 5 and be mixed into and extract oil refining tank 200 out.
Lubricating oil distillate of the present invention or its hydrogenation deacidification oil or solvent-extracted oil, meet open flash point and be not less than 200 DEG C, 100 DEG C of kinematic viscosity are not less than 13.0mm
2/ s, C
avalue is not less than 13.0%, and zero pour is not higher than 30 DEG C, if zero pour is higher than 30 DEG C, need carry out dewaxing treatment.
The opening for feed extracting oil refining tank 200 out can establish feed distributor, extracting out in oil refining tank 200 can be that component is not established in slack tank and inside, or inside increases by one to three layers of sieve plate for preventing back-mixing, extract oil refining tank 200 preferably sleeping tank out, it is 50-120 minutes that the volume extracting oil refining tank 200 out meets the mixed solution residence time wherein that an Extract and secondary extract oil out, time extracted oily raffinate out lower than 50 minutes and is separated not exclusively with Extract, time more than 120 minutes under identical purification condition, the yield of raffinate no longer increases, illustrate that extracting oily raffinate out is fully separated with Extract.
About the operational condition of furfural treating tower, the top temperature of extraction tower 100 is lower than 60 DEG C, and the operation easier of extraction tower 100 increases, and higher than 90 DEG C, the selectivity of solvent declines, and can affect the yield of product; The environmental protection index that solvent ratio is less than 1.0 products is sometimes defective, and solvent ratio is difficult to produce high C higher than 2.5
athe product of value, also can reduce the yield of environment-friendly rubber extending oil simultaneously.Preferred furfural extraction condition is, extraction tower 100 tower top temperature 60 DEG C-90 DEG C, and column bottom temperature is 40 DEG C-60 DEG C, and the mass ratio of solvent and stock oil is 1.0-2.5:1;
About the operational condition of extracting oil refining tank out, secondary extract out oil or secondary Extract through amount that the secondary Extract of evaporation containing a small amount of solvent mixes with Extract and stock oil mass ratio lower than 0.2 and higher than 1.5 time, to the C of environment-friendly rubber extending oil
avalue and the raising of yield not obvious, so the operational condition of extracting oil refining tank 200 out is: the mass ratio that secondary extracts amount that oil or secondary Extract contain a small amount of solvent secondary Extract through evaporation mixes with Extract and stock oil out is 0.2-1.5:1; About the temperature of extracting oil refining tank 200 out, temperature, lower than 40 DEG C, is extracted oil out and is raffinated oil excessively slow with the velocity of separation of solvent, higher than 50 DEG C, can affect the yield extracted oil out and raffinate oil, so the temperature of extracting oil refining tank 200 out is 40 DEG C-50 DEG C.
Embodiment 1
The furfural extract oil of four line cut pressed oils is subtracted for stock oil with paraffinic base, character sees attached list 1, purification condition is: the tower top temperature of extraction tower 100 is 65 DEG C, column bottom temperature is 40 DEG C, the mass ratio of solvent furfural and stock oil is 1.0:1.0, the operational condition of extracting oil refining tank 200 out is: temperature is 40 DEG C, being mixed into what extract oil refining tank 200 out with Extract is 1:1 through evaporating containing the secondary Extract of a small amount of solvent and the mass ratio of stock oil, the residence time is 80 minutes, the extraction oil raffinate 7 that the top of extracting oil refining tank 200 out is flowed out enters extraction tower 100 from the stock oil entrance 110 (namely described extreme lower position) of extraction tower 100, environment-friendly rubber extending oil is obtained after the raffinate 4 that extraction tower 100 top is flowed out enters raffinate stripping tower 300 desolvation, character sees attached list 1.
Comparative example 1
Adopt stock oil, extraction process condition and the extraction tower identical with embodiment 1, namely tower top temperature is 65 DEG C, column bottom temperature is 40 DEG C, the mass ratio of solvent furfural and stock oil is 1.0:1.0, obtain after an Extract recycling design extracting oil out, obtain environment-friendly rubber extending oil after raffinate recycling design, character sees attached list 1.
Embodiment 2
Three hydrogenation deacidification oil are subtracted for stock oil with cycloalkyl, character sees attached list 2, purification condition is: the tower top temperature of extraction tower 100 is 70 DEG C, column bottom temperature is 40 DEG C, the mass ratio of solvent furfural and stock oil is 1.5:1.0, the operational condition of extracting oil refining tank 200 out is: temperature is 40 DEG C, being mixed into what extract oil refining tank 20 out with Extract is 0.5:1 through evaporating containing the secondary Extract of a small amount of solvent and the mass ratio of stock oil, the residence time is 50 minutes, the distance of position and described colvent inlet that the extraction oil raffinate 7 that the top of extracting oil refining tank 200 out is flowed out enters extraction tower 100 is the twice (i.e. described extreme higher position) of this position and described stock oil entrance distance, environment-friendly rubber extending oil is obtained after the raffinate 4 that extraction tower 100 top is flowed out enters raffinate stripping tower 300 desolvation, character sees attached list 2.
Comparative example 2
Adopt stock oil, extraction process condition and the extraction tower identical with embodiment 1, namely tower top temperature is 70 DEG C, column bottom temperature is 40 DEG C, the mass ratio of solvent furfural and stock oil is 1.5:1.0, obtain after an Extract recycling design extracting oil out, obtain environment-friendly rubber oil after raffinate recycling design, character sees attached list 2.
Embodiment 3
Three line furfural extract oils are subtracted for stock oil with cycloalkyl, character sees attached list 3, purification condition is: the tower top temperature of extraction tower 100 is 60 DEG C, column bottom temperature is 40 DEG C, the mass ratio of solvent furfural and stock oil is 2.0:1.0, the operational condition of extracting oil refining tank 200 out is: temperature is 40 DEG C, being mixed into what extract oil refining tank 200 out with Extract is 1.5:1 through evaporating containing the secondary Extract of a small amount of solvent and the mass ratio of stock oil, the residence time is 120 minutes, the distance of position and described colvent inlet that the extraction oil raffinate 7 that the top of extracting oil refining tank 200 out is flowed out enters extraction tower 100 is 5 times (i.e. centres of described extreme higher position and extreme lower position) of this position and described stock oil entrance distance, environment-friendly rubber extending oil is obtained after the raffinate 4 that extraction tower 100 top is flowed out enters raffinate stripping tower 300 desolvation, character sees attached list 3.
Comparative example 3
Adopt stock oil, extraction process condition and the extraction tower identical with embodiment 3, namely tower top temperature is 60 DEG C, column bottom temperature is 40 DEG C, the mass ratio of solvent furfural and stock oil is 2.0:1.0, obtain after an Extract recycling design extracting oil out, obtain environment-friendly rubber extending oil after raffinate recycling design, character sees attached list 3.
Embodiment 4
Four lines are subtracted for stock oil with cycloalkyl, character sees attached list 4, purification condition is: the tower top temperature of extraction tower 100 is 90 DEG C, column bottom temperature is 60 DEG C, the mass ratio of solvent furfural and stock oil is 2.5:1.0, the operational condition of extracting oil refining tank 200 out is: temperature is 50 DEG C, being mixed into what extract oil refining tank 200 out with Extract is 0.2:1 through evaporating containing the secondary Extract of a small amount of solvent and the mass ratio of stock oil, the residence time is 70 minutes, the extraction oil raffinate 7 that flows out of the top of extracting oil refining tank 200 out enters extraction tower 100 from the region between extreme lower position as described in the extreme higher position as described in example 2 of extraction tower 100 and example 1, environment-friendly rubber extending oil is obtained after the raffinate 4 that extraction tower 100 top is flowed out enters raffinate stripping tower 300 desolvation, character sees attached list 4.
Comparative example 4
Adopt stock oil, extraction process condition and the extraction tower identical with embodiment 1, namely tower top temperature is 90 DEG C, column bottom temperature is 60 DEG C, the mass ratio of solvent furfural and stock oil is 2.5:1.0, obtain after an Extract recycling design extracting oil out, obtain environment-friendly rubber extending oil after raffinate recycling design, character sees attached list 4.
Subordinate list 1 embodiment 1 stock oil and environment-friendly rubber extending oil character
Subordinate list 2 embodiment 2 stock oil and environment-friendly rubber extending oil character
Subordinate list 3 embodiment 3 stock oil and environment-friendly rubber extending oil character
Subordinate list 4 embodiment 4 stock oil and environment-friendly rubber extending oil character
As can be seen from product yield and the character of subordinate list 1-4 embodiment 1-4 and comparative example 1-4, present method takes carries out secondary refining to extraction oil, the raffinate of the extraction oil obtained is returned the way of extraction tower, solvent extraction with routine is compared, and can improve yield and the C of product under the same conditions
avalue.
Therefore, adopt lubricating oil distillate or lubricating oil solvent extraction oil to be less than 1mg/kg for stock oil all can produce benzopyrene (BaP) through present method, PCA is less than the environment-friendly rubber extending oil product that 3%, 8 kinds of harmful aromatic hydrocarbons total contents are less than 10mg/kg.
It should be noted that, publication number is that the extraction oil of the high aromaticity content that the Chinese invention patent application of CN101597512A obtains with furfural extraction carries out secondary furfural extraction for raw material, obtain high-arene environment-friendly rubber extending oil, its essence is with furfural extract oil to be that raw material carries out furfural extraction, its treated oil is only the rubber oil of high aromaticity content; Be that raw material carries out furfural treatment with distillate, its treated oil is the rubber oil of low arene content, and the aromaticity content that is in object product environment-friendly rubber oil depends on the aromaticity content in raw material.The object of the invention is with distillate or extract oil out for raw material and adopt furfural extraction method of the present invention to improve the aromaticity content of treated oil and environment-friendly rubber extending oil, be in a production process to the improvement of furfural extraction method to improve treated oil aromaticity content, instead of stock oil is carried out secondary extracting to improve the aromaticity content of rubber oil.
Certainly; the present invention also can have other various embodiments; when not deviating from the present invention's spirit and essence thereof; those of ordinary skill in the art are when making various corresponding change and distortion according to the present invention, but these change accordingly and are out of shape the protection domain that all should belong to the claim appended by the present invention.
Claims (15)
1. produce the equipment of environment-friendly rubber extending oil for one kind, it is characterized in that, comprise extraction tower, extract oil refining tank, raffinate stripping tower and environment-friendly rubber out and fill oil tank, described extraction tower comprises the stock oil entrance being arranged at its underpart, the colvent inlet being arranged at its top, the raffinate outlet that is arranged at an Extract outlet bottom it, is arranged at its top, described extraction oil refining tank comprises an Extract entrance in portion disposed therein, and described Extract outlet is connected with a described Extract entrance, described raffinate stripping tower comprises the raffinate entrance being arranged at its underpart and the environment-friendly rubber extending oil outlet be arranged at bottom it, and described raffinate outlet is connected with described raffinate entrance, described environment-friendly rubber filling oil tank exports with described environment-friendly rubber extending oil and is connected, there is between described extraction oil refining tank and described extraction tower an extraction oil raffinate pipeline, described extraction oily raffinate pipeline comprises to be extracted the outlet of oily raffinate out and extracts oily raffinate entrance out, the outlet of described extraction oily raffinate is arranged at the top of described extraction oil refining tank, described extraction oily raffinate entrance to be arranged on described extraction tower and to have extreme higher position and extreme lower position, described extreme higher position is between described colvent inlet and described feed(raw material)inlet, and the distance of described extreme higher position and described colvent inlet is the twice of the distance of described extreme higher position and described stock oil entrance, described extreme lower position is the position at described stock oil entrance place.
2. the equipment of production environment-friendly rubber extending oil according to claim 1, it is characterized in that, also comprise solvent seasoning tower, wet solvent entrance and solvent outlet after being arranged at bottom it drying after described solvent seasoning tower comprises the stripping being arranged at its top, described raffinate stripping tower also comprises the first wet solvent outlet being arranged at its top, described first wet solvent outlet is connected with wet solvent entrance after described stripping, and after described drying, solvent outlet is connected with described colvent inlet.
3. the equipment of production environment-friendly rubber extending oil according to claim 2, it is characterized in that, also comprise secondary Extract evaporator tower, described secondary Extract evaporator tower comprises the secondary Extract entrance being arranged at its underpart, solvent outlet and secondary Extract outlet after being arranged at bottom it evaporation after being arranged at the evaporation at its top, described solvent seasoning tower comprises colvent inlet after the evaporation in portion disposed therein, described extraction oil refining tank also comprises the secondary Extract outlet be arranged at bottom it, described secondary Extract outlet is connected with described secondary Extract entrance, after described evaporation, the outlet of secondary Extract is connected with a described Extract entrance, after described evaporation, solvent outlet is connected with colvent inlet after described evaporation.
4. the equipment of production environment-friendly rubber extending oil according to claim 3, it is characterized in that, also comprise secondary extract stripper and secondary extraction oil tank, after described secondary extract stripper comprises the evaporation being arranged at its underpart, secondary Extract entrance and the secondary be arranged at bottom it extract oil export out, after described evaporation, the outlet of secondary Extract is connected with secondary Extract entrance after described evaporation, and described secondary extraction oil export is extracted oil tank out with described secondary and is connected.
5. the equipment of production environment-friendly rubber extending oil according to claim 4, it is characterized in that, described secondary extract stripper also comprises the second wet solvent outlet being arranged at its top, and described second wet solvent outlet is connected with wet solvent entrance after described stripping.
6. the equipment of production environment-friendly rubber extending oil according to claim 4, is characterized in that, described secondary is extracted oil export out and is connected with a described Extract entrance.
7. produce a method for environment-friendly rubber extending oil, it is characterized in that, adopt the equipment of production environment-friendly rubber extending oil according to claim 1 to refine, comprise the steps:
Solvent enters described extraction tower from the top of described extraction tower, stock oil enters described extraction tower from the bottom of described extraction tower and carries out extracting, the Extract that extracting obtains enters described extraction oil refining tank and refines, the refining extraction oil raffinate obtained is back to described extraction tower by described extraction oily raffinate pipeline, the raffinate that in described extraction tower, extracting obtains enters described raffinate stripping tower, and the environment-friendly rubber extending oil that raffinate obtains after carrying out stripping desolvation enters described environment-friendly rubber and fills oil tank.
8. the method for production environment-friendly rubber extending oil according to claim 7, it is characterized in that, the wet solvent that described raffinate stripping tower stripping goes out enters described solvent seasoning tower through condensation and carries out drying, and the dried described solvent of described solvent seasoning tower bottom enters described extraction tower and recycles.
9. the method for production environment-friendly rubber extending oil according to claim 8, it is characterized in that, in described extraction oil refining tank, the refining secondary Extract obtained obtains the secondary Extract containing a small amount of solvent after pervaporation, and the secondary Extract containing a small amount of solvent obtains secondary and extracts oil out after stripping.
10. the method for production environment-friendly rubber extending oil according to claim 9, it is characterized in that, part secondary extracts oil out or part mixes with the Extract that described extraction tower extracting obtains through the secondary Extract of evaporation containing a small amount of solvent, enters described extraction oil refining tank and refines.
The method of 11. production environment-friendly rubber extending oils according to claim 9, it is characterized in that, the solvent removed during the evaporation of secondary Extract and the wet solvent removed when evaporation contains the secondary Extract stripping of a small amount of solvent enter described solvent seasoning tower respectively and carry out drying.
The method of 12. production environment-friendly rubber extending oils according to claim 10, it is characterized in that, the operational condition of described extraction oil refining tank is: the secondary mixed with Extract extracts oil out or through evaporate the amount of secondary Extract that contains a small amount of solvent and the mass ratio of stock oil is 0.2-1.5:1, the temperature of extracting oil refining tank out is 40 DEG C-50 DEG C, and the residence time that Extract stays in described extraction oil refining tank is 50-120 minutes; The residence time that the mixed solution that part secondary extraction oil or part obtain after the secondary Extract of evaporation containing a small amount of solvent mixes with an Extract stays in described extraction oil refining tank is 50-120 minutes.
The method of 13. production environment-friendly rubber extending oils according to claim 7, it is characterized in that, described stock oil is lubricating oil distillate or solvent-extracted oil, and described solvent is furfural.
The method of 14. production environment-friendly rubber extending oils according to claim 13, it is characterized in that, the open flash point of described lubricating oil distillate or described solvent-extracted oil is not less than 200 DEG C, and 100 DEG C of kinematic viscosity are not less than 13.0mm
2/ s, C
avalue is not less than 13.0%, and zero pour is not higher than 30 DEG C, if zero pour is higher than 30 DEG C, carries out dewaxing treatment.
The method of 15. production environment-friendly rubber extending oils according to claim 13, it is characterized in that, described furfural extraction condition is, described extraction tower tower top temperature 60 DEG C-90 DEG C, described extraction tower column bottom temperature is 40 DEG C-60 DEG C, and the mass ratio of described furfural and described lubricating oil distillate or described solvent-extracted oil is 1.0-2.5:1.
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| CN101386687A (en) * | 2008-10-24 | 2009-03-18 | 中国海洋石油总公司 | Aromatic rubber oil and producing method thereof |
| CN101684185A (en) * | 2008-09-27 | 2010-03-31 | 中国石油天然气股份有限公司 | Method for producing high-arene environment-friendly rubber oil |
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| CN101684185A (en) * | 2008-09-27 | 2010-03-31 | 中国石油天然气股份有限公司 | Method for producing high-arene environment-friendly rubber oil |
| CN101386687A (en) * | 2008-10-24 | 2009-03-18 | 中国海洋石油总公司 | Aromatic rubber oil and producing method thereof |
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