CN108913196A - A kind of intelligence oil desulfurization equipment - Google Patents
A kind of intelligence oil desulfurization equipment Download PDFInfo
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- CN108913196A CN108913196A CN201810899301.0A CN201810899301A CN108913196A CN 108913196 A CN108913196 A CN 108913196A CN 201810899301 A CN201810899301 A CN 201810899301A CN 108913196 A CN108913196 A CN 108913196A
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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
- C10G31/00—Refining of hydrocarbon oils, in the absence of hydrogen, by methods not otherwise provided for
- C10G31/11—Refining of hydrocarbon oils, in the absence of hydrogen, by methods not otherwise provided for by dialysis
-
- 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
- C10G32/00—Refining of hydrocarbon oils by electric or magnetic means, by irradiation, or by using microorganisms
-
- 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
-
- 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
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/20—Characteristics of the feedstock or the products
- C10G2300/201—Impurities
- C10G2300/202—Heteroatoms content, i.e. S, N, O, P
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- Chemical & Material Sciences (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Engineering & Computer Science (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Microbiology (AREA)
- Production Of Liquid Hydrocarbon Mixture For Refining Petroleum (AREA)
Abstract
The present invention provides a kind of intelligent oil desulfurization equipment, and specifically, the intelligence oil desulfurization equipment includes membrane reactor, intelligence oil desulfurization equipment provided by the invention without chemical reaction, loss of octane number is small, hydrogen consumption is small；It is more highly selective, can deep desulfuration；Low operation temperature, pressure difference are small, low energy consumption, process is simple, free from environmental pollution；Can modularized design, be easy to amplify dilatation and built with other equipment；It is reliable for operation, convenient for safeguarding, it is suitable for a variety of industrial scenes.
Description
Technical field
The present invention relates to petroleum sweetening field, a kind of particularly intelligent oil desulfurization equipment.
Background technique
There are hundreds of sulfur-bearing hydrocarbon in petroleum, has verified that at present and determine structure just has more than 200, these sulfur-bearing hydro carbons exist
It is distributed in each distillate to some extent in petroleum refining process.In view of oil product answering in production and life extensively
With the sulphur for removing wherein harmfulness is very important production practices.
It is industrial at present mainly to use non-hydrodesulfurizationprocess process, acid-alkali refining, solvent extraction and adsorb desulfurization, it is above-mentioned several
All there is defects and deficiency for sulfur method.Wherein acid-alkali refining has a large amount of spent acid spent lye to generate, and will cause serious ring
Border pollution；Energy consumption is high for solvent extraction sweetening process, and oil product yield is low；The adsorbance of adsorbent is small in absorption method, and needs often again
It is raw.
Other non-hydrodesulfurizations are also in experimental stage, wherein biological desulphurization, oxidation sweetening and light and plasma
The application prospect of body desulfurization is very tempting, is the effective ways realizing the following clean fuel oil and producing, but not due to the above method
Stablize, do not there is large-scale industrial production so far, reducing the sulfur content in fuel oil, reducing atmosphere pollution is a complicated mistake
Journey, therefore it is considered as various factors when implementation, the reliability to develop skill, to obtain optimal economic benefit and environmental benefit.
With to sulfur crude processing amount increase and heavy oil catalytic cracking it is universal, oil product sulfur content is exceeded and stability
Bad phenomenon is also increasingly severe.Due to limitation of the hydrodesulfurization in fund and hydrogen source, for centering little refinery plant into
The research of row non-hydrogenation has great importance, and the present invention provides a kind of intelligent oil desulfurization equipment, without adding hydrogen, environment
It is friendly.
Summary of the invention
In order to solve the above technical problem, the present invention provides a kind of intelligent oil desulfurization equipment.
The present invention is realized with following technical solution：
A kind of intelligence oil desulfurization equipment, the intelligence oil desulfurization equipment includes membrane reactor.
Further, the intelligent oil desulfurization equipment further includes crude stream, and the crude stream is defeated by feed pump
It is sent into filter, is provided with intellectual analysis instrument at the crude stream, the filter is connected with the first membrane reactor, described
Membrane reactor is connected with the first vacuum pump, and first membrane reactor is also connected with the second membrane reactor, second film reaction
Device is connected with the second vacuum pump, is provided in first membrane reactor and the second membrane reactor multiple mutual along vertical axis
The plate and frame module separated, the first membrane reactor are connect with fractional condensaion equipment respectively with the second membrane reactor, fractional condensaion
The sulphur products of the different sulfurs of permeability and separation are condensed respectively and are transported in corresponding recycling can by equipment, the conveying of high-sulfur product
To high-sulfur Product recycling tank, low sulfur product is delivered to low sulfur product recycling can, passes through the purified product quilt of two-stage membrane reactor
It is delivered in biological desulphurization reactor, product tank is delivered to after biological desulphurization reactor reaction, intellectual analysis instrument passes through
The quantity of membrane module needed for calculating the detection of crude stream.
Further, the plate and frame module is made of deep desulfuration permeable membrane；
Further, the specific production step of the deep desulfuration permeable membrane is：
Step 1: 20g ZrOCl 8H2O is dissolved in 100ml dehydrated alcohol by sol-gel method for preparing Zr O2 colloidal sol, it
Obtained solution is vigorously mixed at room temperature for 5h afterwards, whipping process is added dropwise concentrated hydrochloric acid and above-mentioned solution is adjusted to pH2, will
Obtained mixed solution continues to stir 10h until obtaining clear solution, and placement 24, which as a child obtains, stablizes ZrO2 colloidal sol；
Step 2: porous fibrous material is taken to immerse in ZrO2 colloidal sol 25 seconds, and it is 2 days dry at 60 DEG C later, later in 400 DEG C of items
It is calcined 4 hours in part oxygen atmosphere, heating rate is 2 DEG C/min, until forming ZrO2 thin layer on porous fibrous material；
Step 3: prepare deep desulfuration permeable membrane, zirconium chloride is taken, H2BDC-NH2, distilled water, acetic acid, dimethylformamide, on
Stating component molar ratio is 1:1:1:180:500, specifically, zirconium chloride is taken, H2BDC-NH2 is dissolved in equivalent dimethylformamide respectively
In and be ultrasonically treated 15 minutes, two kinds of solution are mixed and acetic acid aqueous solution be added in mixed solution, the solution of acquisition is existed
45 minutes acquisition mother liquors are stirred at room temperature；
Step 4: being transferred to mother liquor in the reaction kettle with teflon lined, it is covered with what is obtained in step 2
The porous fibrous material of ZrO2 thin layer is disposed vertically in reaction kettle, and reaction kettle is placed in 120 DEG C of convection oven 48 hours, to
After permeating membrane crystallization, rinsed for several times with 75% ethyl alcohol, it is finally dry to obtain deep desulfuration permeable membrane for 24 hours（ZrO2- BDC-NH2）.
There are mainly two types of existence forms for sulphur in fuel oil：The sulfide that usually can directly react with metal is known as
" active sulfur ", including elemental sulfur, hydrogen sulfide and mercaptan；Sulfide without directly reacting with metal is known as " nonactive
Sulphur ", including thioether, disulphide, thiophene etc..For gasoline fraction, sulfur-bearing hydro carbons is with mercaptan, sulfide and monocycle thiophene
Based on, it is mainly derived from catalytic cracking（Abbreviation FCC）Gasoline.
Therefore, for the index that gasoline meets low-sulphur oil must carry out pretreatment to FCC gasoline raw material or to FCC gasoline
Product is post-processed.And the sulfur-bearing hydro carbons in diesel oil distillate has mercaptan, sulfide, thiophene, benzothiophene and dibenzothiophenes
Deng, wherein the 4 of dibenzothiophenes, in the presence of 6 alkyl, due to alkyl steric hindrance and keep desulfurization extremely difficult, Er Qiesui
The raising of petroleum distillate boiling point, the structure of sulfur-containing compound also become increasingly complex.
Intelligence oil desulfurization equipment provided by the invention is suitable for without chemical reaction, loss of octane number is small, hydrogen consumption is small；
It is more highly selective, can deep desulfuration；Low operation temperature, pressure difference are small, low energy consumption, process is simple, free from environmental pollution；Can modularization set
It counts, be easy to amplify dilatation and built with other equipment；It is reliable for operation, convenient for safeguarding, it is suitable for a variety of industrial scenes.
Detailed description of the invention
Fig. 1 is the schematic diagram of intelligent oil desulfurization equipment of the present invention；
Wherein, 1- crude stream, 11- intellectual analysis instrument, 2- feed pump, 3- filter, the first membrane reactor of 4-, the second film of 5-
Reactor, 6- fractional condensaion equipment, 7- high-sulfur Product recycling tank, 8- low sulfur product recycling can, 9- biological desulphurization reactor, 10-
Product tank.
Specific embodiment
To make the object, technical solutions and advantages of the present invention clearer, the present invention will be made below further detailed
Description.
Embodiment 1：
The present invention is more particularly directed to a kind of UF membrane-biological desulphurizations to couple FCC gasoline desulfurization of raw material equipment, as shown in Figure 1, the original
Oily desulphurization plant includes crude stream 1, and the crude stream is conveyed into filter 3 by feed pump 2, at the crude stream 1
It is provided with intellectual analysis instrument 11, the filter 3 is connected with the first membrane reactor 4, and first membrane reactor 4 is connected with
One vacuum pump, first membrane reactor 4 are also connected with the second membrane reactor 5, and it is true that second membrane reactor 5 is connected with second
Sky pumps, and is provided in first membrane reactor 4 and the second membrane reactor 5 multiple along vertical axis plate and frame spaced apart from each other
Membrane module, the first membrane reactor 4 are connect with 6 equipment of fractional condensaion respectively with the second membrane reactor 5, and fractional condensaion equipment 6 will seep
The sulphur products of the different sulfurs separated thoroughly are condensed respectively and are transported in corresponding recycling can, and high-sulfur product is delivered to high-sulfur production
Product recycling can 7, low sulfur product are delivered to low sulfur product recycling can 8, are transported to by the purified product of two-stage membrane reactor
In biological desulphurization reactor 9, it is delivered to product tank 10 after the reaction of biological desulphurization reactor 9, intellectual analysis instrument 11 passes through
The quantity of membrane module needed for calculating the detection of crude stream 1, Fig. 1 are only used as schematic diagram to indicate connection relationship, not instruction dress
The size set or spatial position.
Embodiment 2：
Membrane reactor provided by the invention includes that plate and frame module is made in deep desulfuration permeable membrane, can be according to original in actual production
Oil processing demand can obtain required membrane area, the deep desulfuration infiltration by the installation of infiltration direction by concatenated mode
The dissolution diffusivity of film at different conditions is different, during infiltration evaporation according to permeation flux difference to recovery product into
Row selects, and the sulfur-containing compound in middle fraction and heavy distillat gasoline is mainly thiophene and derivatives, and the present invention specifically provides
A kind of deep desulfuration permeable membrane for thiophene and derivatives, it is preferable that it is for removal sulfur in gasoline ether, curing
Object, thiophenes have excellent effect, and the specific production step of the deep desulfuration permeable membrane is：
Step 21 passes through sol-gel method for preparing Zr O220g ZrOCl8H2O is dissolved in 100ml dehydrated alcohol by colloidal sol,
Obtained solution is vigorously mixed at room temperature for 5h later, whipping process is added dropwise concentrated hydrochloric acid and above-mentioned solution is adjusted to pH2,
Continue obtained mixed solution to stir 10h until obtaining clear solution, placement 24, which as a child obtains, stablizes ZrO2Colloidal sol；
Step 22 takes porous fibrous material to immerse ZrO2It is 2 days dry at 60 DEG C later 25 seconds in colloidal sol, later in 400 DEG C of items
It is calcined 4 hours in part oxygen atmosphere, heating rate is 2 DEG C/min, until forming ZrO on porous fibrous material2Thin layer；
Step 23 prepares deep desulfuration permeable membrane, takes zirconium chloride, H2BDC-NH2, distilled water, acetic acid, dimethylformamide, on
Stating component molar ratio is 1:1:1:180:500, specifically, take zirconium chloride, H2BDC-NH2It is dissolved in equivalent dimethylformamide respectively
In and be ultrasonically treated 15 minutes, two kinds of solution are mixed and acetic acid aqueous solution be added in mixed solution, the solution of acquisition is existed
45 minutes acquisition mother liquors are stirred at room temperature；
Mother liquor is transferred in the reaction kettle with teflon lined by step 24, is covered with what is obtained in step 22
ZrO2The porous fibrous material of thin layer is disposed vertically in reaction kettle, and reaction kettle is placed in 120 DEG C of convection oven 48 hours, to
After permeating membrane crystallization, rinsed for several times with 75% ethyl alcohol, it is finally dry to obtain deep desulfuration permeable membrane for 24 hours（ZrO2- BDC-NH2）.
Embodiment 3：
Bioreactor is prepared, the core reaction element of the bioreactor is that polyacrylamide gel embeds active microorganism
Immobilized cell particle, the making step of the immobilized cell particle is as follows：
Step 31, the rhodococcus erythropolis (Rhodococcus erythropolis) for taking proper proportion, Thiobacillus thioxidans
（Thiobacillus thiooxidans）, grate sulfur thiobacillus（Thiobacill usthioparus）, Thiobacillus ferrooxidans
（Thiobacillus ferrooxidans）And thiobacillus denitrificans（Thiobacillus denitrificans）Culture,
Ratio is 10:2:1:1:1, above-mentioned strain is commercially available strain；
Plastc ring is dissolved in sterile water by step 32, and plastc ring total cell amount is made to reach 50g/L, is mixed to 1L
65.5g/L acrylamide is added in bacterium solution, the 2.5g/L BIS of 200ml is added, adds the 20ml/L APS and four of 200ml
Methyl ethylenediamine 2 drips, and ice bath 30 minutes, obtains immobilized cell particle；
Step 33 is loaded on immobilized cell particle stationary in bioreactor, adjusts temperature, pH value, oxygen-supply quantity, logical
Crossing periodically spray culture solution makes immobilized microorganism rejuvenation and promotes desulphurizing ability.
Embodiment 4：
With 50% crude oil+50%（Toluene, normal octane, quinoline, thiophene）The simulated system of composition carries out intelligent oil desulfurization equipment
Desulfurization performance test, test show that total permeation flux of the first membrane reactor is up to 4578g/ at 150 DEG C of operation temperature
(m2* h), the sulfur-rich factor is 8.5, and through testing, operation temperature is during a grade is increased to 215 DEG C, to rise with 5 DEG C from 115 DEG C
When the beginning, the micro-Brownian movement of deep desulfuration permeable membrane is accelerated, and permeation flux increases, and with selectivity decline, works as operation temperature
When being 135-155 DEG C, permeation flux and selectivity reach zone of reasonableness, and after tested, this equipment can be disposably by the sulphur of crude oil
Content is reduced to 19.8% or less.
The above disclosure is only the preferred embodiments of the present invention, cannot limit the right model of the present invention with this certainly
It encloses, therefore equivalent changes made in accordance with the claims of the present invention, is still within the scope of the present invention.
Claims (4)
1. a kind of intelligence oil desulfurization equipment, which is characterized in that the intelligence oil desulfurization equipment includes membrane reactor.
2. equipment according to claim 1, which is characterized in that the intelligence oil desulfurization equipment further includes crude stream, institute
It states crude stream and filter is conveyed by feed pump, intellectual analysis instrument, the filter are provided at the crude stream
It is connected with the first membrane reactor, the membrane reactor is connected with the first vacuum pump, and first membrane reactor is also connected with second
Membrane reactor, second membrane reactor are connected with the second vacuum pump, in first membrane reactor and the second membrane reactor
Be provided with it is multiple along vertical axis plate and frame module spaced apart from each other, the first membrane reactor and the second membrane reactor respectively with point
The sulphur products of the different sulfurs of permeability and separation are condensed respectively and are transported to corresponding by grade condensing plant connection, fractional condensaion equipment
Recycling can in, high-sulfur product is delivered to high-sulfur Product recycling tank, and low sulfur product is delivered to low sulfur product recycling can, passes through two-stage
The purified product of membrane reactor is transported in biological desulphurization reactor, and production is delivered to after biological desulphurization reactor reaction
Object tank, the quantity of membrane module needed for intellectual analysis instrument is calculated by the detection to crude stream.
3. equipment according to claim 2, which is characterized in that the plate and frame module is made of deep desulfuration permeable membrane.
4. equipment according to claim 3, which is characterized in that the specific production step of the deep desulfuration permeable membrane is：
Step 1: passing through sol-gel method for preparing Zr O220g ZrOCl8H2O is dissolved in 100ml dehydrated alcohol by colloidal sol, it
Obtained solution is vigorously mixed at room temperature for 5h afterwards, whipping process is added dropwise concentrated hydrochloric acid and above-mentioned solution is adjusted to pH2, will
Obtained mixed solution continues to stir 10h until obtaining clear solution, and placement 24, which as a child obtains, stablizes ZrO2Colloidal sol；
Step 2: porous fibrous material is taken to immerse ZrO2It is 2 days dry at 60 DEG C later 25 seconds in colloidal sol, later in 400 DEG C of items
It is calcined 4 hours in part oxygen atmosphere, heating rate is 2 DEG C/min, until forming ZrO on porous fibrous material2Thin layer；
Step 3: preparing deep desulfuration permeable membrane, zirconium chloride, H are taken2BDC-NH2, distilled water, acetic acid, dimethylformamide is above-mentioned
Component molar ratio is 1:1:1:180:500, specifically, take zirconium chloride, H2BDC-NH2It is dissolved in equivalent dimethylformamide respectively
And be ultrasonically treated 15 minutes, two kinds of solution are mixed and acetic acid aqueous solution is added in mixed solution, by the solution of acquisition in room
Temperature is lower to stir 45 minutes acquisition mother liquors；
Step 4: being transferred to mother liquor in the reaction kettle with teflon lined, ZrO is covered with by what is obtained in step 22
The porous fibrous material of thin layer is disposed vertically in reaction kettle, and reaction kettle is placed in 120 DEG C of convection oven 48 hours, to be infiltrated
After membrane crystallization, rinsed for several times with 75% ethyl alcohol, it is finally dry to obtain deep desulfuration permeable membrane for 24 hours（ZrO2- BDC-NH2）.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN201610422U (en) * | 2009-12-05 | 2010-10-20 | 中国石油大学(华东) | Deep gasoline desulfurization device adopting membrane method |
| CN101927130A (en) * | 2009-04-16 | 2010-12-29 | 济南开发区星火科学技术研究院 | Method for removing sulfur-containing compounds from oil by utilizing membrane process |
| CN103463999A (en) * | 2013-09-06 | 2013-12-25 | 烟台绿水赋膜材料有限公司 | Preparation method of novel ultrathin salt-cutting separation membrane |
| CN103894074A (en) * | 2012-12-28 | 2014-07-02 | 中国科学院上海高等研究院 | Novel hybrid membrane as well as preparation method and application thereof |
| CN105873667A (en) * | 2013-12-30 | 2016-08-17 | 3M创新有限公司 | Composite membranes and methods of use |
| CN108031303A (en) * | 2017-11-24 | 2018-05-15 | 大连理工大学 | A kind of preparation method of infiltration evaporation metal organic framework UiO-66 series gasoline desulfurizing films |
-
2018
- 2018-08-08 CN CN201810899301.0A patent/CN108913196A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101927130A (en) * | 2009-04-16 | 2010-12-29 | 济南开发区星火科学技术研究院 | Method for removing sulfur-containing compounds from oil by utilizing membrane process |
| CN201610422U (en) * | 2009-12-05 | 2010-10-20 | 中国石油大学(华东) | Deep gasoline desulfurization device adopting membrane method |
| CN103894074A (en) * | 2012-12-28 | 2014-07-02 | 中国科学院上海高等研究院 | Novel hybrid membrane as well as preparation method and application thereof |
| CN103463999A (en) * | 2013-09-06 | 2013-12-25 | 烟台绿水赋膜材料有限公司 | Preparation method of novel ultrathin salt-cutting separation membrane |
| CN105873667A (en) * | 2013-12-30 | 2016-08-17 | 3M创新有限公司 | Composite membranes and methods of use |
| CN108031303A (en) * | 2017-11-24 | 2018-05-15 | 大连理工大学 | A kind of preparation method of infiltration evaporation metal organic framework UiO-66 series gasoline desulfurizing films |
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