CN108211823A - It is a kind of for polyvinyl butyral/polyacrylonitrile compound film of gasoline desulfurization and preparation method thereof - Google Patents
It is a kind of for polyvinyl butyral/polyacrylonitrile compound film of gasoline desulfurization and preparation method thereof Download PDFInfo
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- CN108211823A CN108211823A CN201810066352.5A CN201810066352A CN108211823A CN 108211823 A CN108211823 A CN 108211823A CN 201810066352 A CN201810066352 A CN 201810066352A CN 108211823 A CN108211823 A CN 108211823A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/38—Polyalkenylalcohols; Polyalkenylesters; Polyalkenylethers; Polyalkenylaldehydes; Polyalkenylketones; Polyalkenylacetals; Polyalkenylketals
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D69/00—Semi-permeable membranes for separation processes or apparatus characterised by their form, structure or properties; Manufacturing processes specially adapted therefor
- B01D69/12—Composite membranes; Ultra-thin membranes
- B01D69/125—In situ manufacturing by polymerisation, polycondensation, cross-linking or chemical reaction
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D71/00—Semi-permeable membranes for separation processes or apparatus characterised by the material; Manufacturing processes specially adapted therefor
- B01D71/06—Organic material
- B01D71/40—Polymers of unsaturated acids or derivatives thereof, e.g. salts, amides, imides, nitriles, anhydrides, esters
- B01D71/42—Polymers of nitriles, e.g. polyacrylonitrile
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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
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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
- 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)
- Chemical Kinetics & Catalysis (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Engineering & Computer Science (AREA)
- General Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Separation Using Semi-Permeable Membranes (AREA)
- Manufacture Of Macromolecular Shaped Articles (AREA)
Abstract
The invention discloses a kind of polyvinyl butyral/polyacrylonitrile compound films for pervaporation method gasoline desulfurization, are made of active layer and supporting layer, and active layer is polyvinyl butyral, and supporting layer is polyacrylonitrile；Preparation method is as follows：Polyacrylonitrile, plasticizer, polyethylene glycol 200, n,N dimethylformamide are added in round-bottomed flask, until completely dissolved, press filtration, degassing, knifing, drying is carried out, obtains polyacrylonitrile counterdie；Polyvinyl butyral, polyethylene glycol 200, tetrahydrofuran and ethyl alcohol are added in round-bottomed flask, after it is completely dissolved, add in crosslinking agent, it is configured to homogeneous casting solution, then it is filtered, standing and defoaming, then the scraper of the casting solution after deaeration is coated on polyacrylonitrile counterdie, be then placed into convection oven, except in striping solvent to get to polyvinyl butyral/polyacrylonitrile compound film.The composite membrane can be used for FCC gasoline desulfurization, and desulfurization effect protrudes.
Description
Technical field
The present invention relates to a kind of polyvinyl butyral/polyacrylonitrile compound film for pervaporation method gasoline desulfurization,
And the preparation method of the complex film for gasoline desulfurization.
Background technology
The whole world is increasingly stringent to the enhancing of environmental protection consciousness and environmental regulation so as to automobile-used in world wide
Gasoline discharge standard requires also increasingly tighter.Four discharge standard of motor petrol national standard state of enforcement of China in 2015 is formally real
It applies, plans simultaneously, implemented five discharge standard of petrol and diesel oil state by 2018.But still have one compared with external advanced standard
Fixed gap.FCC gasoline is the main source of gasoline, and it is the key that reduce content of sulfur in gasoline to reduce the sulfur content in FCC gasoline.
Although traditional hydrodesulfurization, catalytic desulfurization can effectively remove thiophene sulfides, there are high energy consumption, loss octane number,
The shortcomings of operating cost is high.Therefore, the other inexpensive deep desulfurization of gasoline technologies of research and development are that China's oil refining industry is focused on
It solves the problems, such as.
With the application of membrane technology and the development of development, especially polymer membrane so that membrane technology is grasped in chemical industry
Application in work is more and more extensive.A kind of infiltration evaporation isolation technics wide as prospects for commercial application because its energy consumption less,
It is economical, easily amplification, can deep desulfuration (feed sulphur content can be reduced to 10ppm), do not lose octane number, clean and effective and by
Pay attention to.Pre- place is not required to for flexibility of the raw material with height, (no elution, adsorbent and catalyst) easy to operate, raw material
The reason of reason does not chemically react, is infiltration evaporation potential as desulfurization process of gasoline alternative technique.
Invention content
Based on above-mentioned technical problem, the present invention provides a kind of polyvinyl alcohol for pervaporation method FCC gasoline desulfurization and contracts
Butyraldehyde/polyacrylonitrile compound film and preparation method thereof.
The adopted technical solution is that：
A kind of polyvinyl butyral/polyacrylonitrile compound film for pervaporation method gasoline desulfurization is by activity
Layer and supporting layer are formed, and active layer is polyvinyl butyral, and supporting layer is polyacrylonitrile；Active layer is coated on supporting layer and obtains
To polyvinyl butyral/polyacrylonitrile compound film.
Preferably, the thickness of the active layer is 10~15 μm, and the thickness of supporting layer is 110 μm.
The preparation method of above-mentioned polyvinyl butyral/polyacrylonitrile compound film for pervaporation method gasoline desulfurization,
Include the following steps：
A adds in polyacrylonitrile, plasticizer, polyethylene glycol 200, n,N dimethylformamide in round-bottomed flask, treats completely molten
Xie Hou carries out press filtration, degassing, knifing, drying, polyacrylonitrile film is obtained, as counterdie；
B adds in polyvinyl butyral, polyethylene glycol 200, tetrahydrofuran and ethyl alcohol in round-bottomed flask, treats that it is completely molten
Xie Hou obtains lysate, crosslinking agent is then added in into lysate, is configured to homogeneous casting solution；
C filters the copper mesh of 300 mesh of homogeneous casting solution obtained in step b；
D stands the casting solution after step c filterings, to remove bubble；
Casting solution after step d deaerations scraper is coated on polyacrylonitrile counterdie by e, is then placed into convection oven
In, except in striping solvent to get to polyvinyl butyral/polyacrylonitrile compound film.
Preferably, in step a：During dissolving, round-bottomed flask is positioned over 12h in 50 DEG C of waters bath with thermostatic control.
Preferably, in step a：Using knifing machine on non-woven fabrics knifing, it is 100 μm to adjust the thickness of scraper, will be scraped
Film immerse 72h in deionized water, be put into oven drying, it is 110 μm of polyacrylonitrile film to obtain thickness.
Preferably, in step b：The volume ratio of the tetrahydrofuran and ethyl alcohol is 2: 1.
Preferably, in step b：The crosslinking agent is boric acid.
Preferably, in step b：The additive amount of the crosslinking agent is the 0.5%-1% of lysate quality.
Preferably, in step d：The standing and defoaming time is 12h.
Preferably, in step e：Using 50~100 μm of scraper film, the thickness of acquired polyvinyl butyral film layer
It is 10~15 μm；It is 60 DEG C~65 DEG C to control the temperature in air dry oven.
The method have the benefit that：
Polyvinyl butyral/polyacrylonitrile compound film of the present invention can be used for FCC gasoline desulfurization, and effect protrudes, sulphur enrichment
The factor reaches 5, flux 1.5kg/m2.h)；The composite membrane is using polyacrylonitrile film as counterdie, and polyacrylonitrile film is ultrafiltration membrane, is
The preferable supporter of osmosis vaporizing compound membrane material selects polyvinyl butyral to meet dissolving as active membrane material layer
Parameter theory is spent, there are the advantages such as excellent solvent resistance, flexibility.
Show that the forms of motion of sulfur component (predominantly thiophene) in PVB films in gasoline is by molecular simulation result
It jumps and migrates in polymer hole, be conducive to it through film, table 1 is respectively to represent interaction energy of the component in film in gasoline
Δ E, Δ E show that more greatly interaction can be stronger, and molecule, which diffuses out contact surface, will overcome higher energy barrier, can see
It arrives, the interaction of PVB and thiophene can be less than remaining four kinds of typical petrol molecule, and thiophene diffuses out the energy of contact surface needs
It measures minimum, is easiest to spread, so as to be detached with components other in gasoline.
Table 1
Table 2
Table 2 is the diffusion rate of thiophene and hydrocarbon component in PVB films in binary mixture, wherein the diffusion choosing of thiophene
Sex factor is selected as α, Dt/Dh is defined as, is respectively 1.0203,1.1667 and 1.4838 for cycloalkane, alkene and aromatic hydrocarbons system,
Show in PVB polymer, other hydrocarbon components of thiophene molecular proportion have stronger motility, it is easier to it is spread in film, so as to
It is detached with components other in gasoline, sulfur-containing compound is removed.
Preparation method of the present invention has the following advantages：
(1) composite membrane desulfuration efficiency obtained by is high, can be in deep removal oil product more than 80% thiophene-based sulfur-bearing chemical combination
Object.
(2) reaction condition is mild, and equipment investment and operating cost are low.
(3) loss of octane number is small, and technological process is simple.
The desulfurization principle of polyvinyl butyral/polyacrylonitrile compound film of the present invention approximately as：
It is spy based on specific compound or a kind of compound to membrane material that infiltrating and vaporizing membrane, which can be realized to the separation of component,
Different affinity, in gasoline separation of the sulfur component in Pervaporation membrane meet solubility-diffusion model, i.e. molecule in three steps
Through Pervaporation membrane：Separated object matter is selectively adsorbed and is dissolved on the surface of the film；It is oozed by being diffused in film
Thoroughly；The opposite side of film become gas phase desorption and and UF membrane.
Specific embodiment
Embodiment 1
A is by 45.883g polyacrylonitrile, 0.695g dimethyl terephthalate (DMT)s, 7.058g polyvinyl alcohol 200,300mLN, N
Dimethylformamide is added in round-bottomed flask, 50 DEG C of water bath with thermostatic control 12h, until completely dissolved, carries out press filtration, degassing.Using scraping
Film machine knifing on non-woven fabrics, the thickness for adjusting scraper are 100 μm, and the film scraped is immersed 72h in deionized water, is subsequently placed into
Oven drying obtains 110 μm of polyacrylonitrile film, i.e. counterdie.
B adds in 4.00g polyvinyl butyrals, 0.45g polyethylene glycol 200s, solvents tetrahydrofurane 20mL, ethyl alcohol 10mL
In the round-bottomed flask of 100mL, 65 DEG C of oil bath heating after it is completely dissolved, obtains lysate.
C adds in 1g crosslinking agent boric acid into solution prepared by step b, stirs 8h, and casting solution is made.
D filters the copper mesh of 300 mesh of casting solution obtained in step c, and the casting solution of filtering then is stood 12h with de-
Bubble removing.
The scraper that degassing casting solution thickness obtained by step d is 50~100 μm is coated on polyacrylonitrile counterdie by e,
Be subsequently placed in convection oven, solvent made to volatilize at 60 DEG C, with remove in striping solvent to get to polyvinyl butyral/
Polyacrylonitrile compound film.
Embodiment 2
A is by 45.883g polyacrylonitrile, 0.695g plasticizer, 7.058g polyvinyl alcohol 200,300mLN, N dimethyl formyl
Amine is added in round-bottomed flask, 50 DEG C of water bath with thermostatic control 12h, until completely dissolved, carries out press filtration, degassing.Using knifing machine in nonwoven
Knifing on cloth, the thickness for adjusting scraper are 100 μm, and the film scraped is immersed 72h in deionized water, is subsequently placed into oven drying,
Obtain 110 μm of polyacrylonitrile film, i.e. counterdie.
B adds in 5.00g polyvinyl butyrals, 0.45g polyethylene glycol 200s, solvents tetrahydrofurane 20mL, ethyl alcohol 10mL
In the round-bottomed flask of 100mL, 65 DEG C of oil bath heating after it is completely dissolved, obtains lysate.
C adds in 0.5% crosslinking agent boric acid into solution prepared by step b, stirs 8h, and casting solution is made.
D filters the copper mesh of 300 mesh of casting solution obtained in step c, and the casting solution of filtering then is stood 12h with de-
Bubble removing.
The scraper that degassing casting solution thickness obtained by step d is 50~100 μm is coated on polyacrylonitrile counterdie by e,
Be subsequently placed in convection oven, solvent made to volatilize at 65 DEG C, with remove in striping solvent to get to polyvinyl butyral/
Polyacrylonitrile compound film.
Embodiment 3
A is by 45.883g polyacrylonitrile, 0.695g plasticizer, 7.058g polyvinyl alcohol 200,300mLN, N dimethyl formyl
Amine is added in round-bottomed flask, 50 DEG C of water bath with thermostatic control 12h, until completely dissolved, carries out press filtration, degassing.Using knifing machine in nonwoven
Knifing on cloth, the thickness for adjusting scraper are 100 μm, and the film scraped is immersed 72h in deionized water, is subsequently placed into oven drying,
Obtain 110 μm of polyacrylonitrile film, i.e. counterdie.
B adds in 4.00g polyvinyl butyrals, 0.45g polyethylene glycol 200s, solvents tetrahydrofurane 20mL, ethyl alcohol 10mL
In the round-bottomed flask of 100mL, 65 DEG C of oil bath heating after it is completely dissolved, obtains lysate.
C adds in 0.75% crosslinking agent boric acid into solution prepared by step b, stirs 8h, and casting solution is made.
D filters the copper mesh of 300 mesh of casting solution obtained in step c, and the casting solution of filtering then is stood 12h with de-
Bubble removing.
The scraper that degassing casting solution thickness obtained by step d is 50~100 μm is coated on polyacrylonitrile counterdie by e,
Be subsequently placed in convection oven, solvent made to volatilize at 65 DEG C, with remove in striping solvent to get to polyvinyl butyral/
Polyacrylonitrile compound film.
Polyvinyl butyral made from embodiment 1/polyacrylonitrile compound film progress pervaporation method FCC gasoline is chosen to take off
Sulphur is tested, and using existing infiltration evaporation evaluating apparatus, polyvinyl alcohol contracting fourth made from the embodiment of the present invention 1 is used in device assembly
Aldehyde/polyacrylonitrile compound film, concrete outcome are as follows：
FCC gasoline of the initial sulfur content in 250mg/L is added in into infiltration evaporation evaluating apparatus, flow 90mLmin- 1,,
Permeation flux 2.3kg/ (m2.h), circulation time 72h, sulfur content in gasoline 10mg/L.
FCC heavy petrol of the initial sulfur content in 900mg/L is added in into infiltration evaporation evaluating apparatus, flow 90mLmin- 1,, permeation flux 1.5kg/ (m2.h), circulation time 72h, sulfur content in gasoline 50mg/L.
FCC sulfur-rich gasoline of the initial sulfur content in 1330mg/L is added in into infiltration evaporation evaluating apparatus, flow 90mL
min- 1,, permeation flux 1.2kg/ (m2.h), circulation time 100h, sulfur content in gasoline 50mg/L.
Claims (10)
1. a kind of polyvinyl butyral/polyacrylonitrile compound film for pervaporation method gasoline desulfurization, it is characterised in that：It should
Composite membrane is made of active layer and supporting layer, and active layer is polyvinyl butyral, and supporting layer is polyacrylonitrile；Active layer applies
It overlays on supporting layer and obtains polyvinyl butyral/polyacrylonitrile compound film.
2. a kind of polyvinyl butyral/polyacrylonitrile for pervaporation method gasoline desulfurization according to claim 1
Composite membrane, it is characterised in that：The thickness of the active layer is 10~15 μm, and the thickness of supporting layer is 110 μm.
It is 3. compound for polyvinyl butyral/polyacrylonitrile of pervaporation method gasoline desulfurization as claimed in claim 1 or 2
The preparation method of film, it is characterised in that include the following steps：
A adds in polyacrylonitrile, plasticizer, polyethylene glycol 200, n,N dimethylformamide in round-bottomed flask, waits to be completely dissolved
Afterwards, press filtration, degassing, knifing, drying are carried out, polyacrylonitrile film is obtained, as counterdie；
B adds in polyvinyl butyral, polyethylene glycol 200, tetrahydrofuran and ethyl alcohol in round-bottomed flask, treats that it is completely dissolved
Afterwards, lysate is obtained, crosslinking agent is then added in into lysate, is configured to homogeneous casting solution；
C filters the copper mesh of 300 mesh of homogeneous casting solution obtained in step b；
D stands the casting solution after step c filterings, to remove bubble；
Casting solution after step d deaerations scraper is coated on polyacrylonitrile counterdie by e, is then placed into convection oven,
Except in striping solvent to get to polyvinyl butyral/polyacrylonitrile compound film.
4. polyvinyl butyral/polyacrylonitrile according to claim 3 for pervaporation method gasoline desulfurization is compound
The preparation method of film, which is characterized in that in step a：During dissolving, round-bottomed flask is positioned over 12h in 50 DEG C of waters bath with thermostatic control.
5. polyvinyl butyral/polyacrylonitrile according to claim 3 for pervaporation method gasoline desulfurization is compound
The preparation method of film, which is characterized in that in step a：Using knifing machine, knifing, the thickness for adjusting scraper are 100 μ on non-woven fabrics
The film scraped is immersed 72h in deionized water, is put into oven drying by m, obtains the polyacrylonitrile film that thickness is 110 μm.
6. polyvinyl butyral/polyacrylonitrile according to claim 3 for pervaporation method gasoline desulfurization is compound
The preparation method of film, which is characterized in that in step b：The volume ratio of the tetrahydrofuran and ethyl alcohol is 2: 1.
7. polyvinyl butyral/polyacrylonitrile according to claim 3 for pervaporation method gasoline desulfurization is compound
The preparation method of film, which is characterized in that in step b：The crosslinking agent is boric acid.
8. polyvinyl butyral/polyacrylonitrile according to claim 3 for pervaporation method gasoline desulfurization is compound
The preparation method of film, which is characterized in that in step b：The additive amount of the crosslinking agent is the 0.5%-1% of lysate quality.
9. polyvinyl butyral/polyacrylonitrile according to claim 3 for pervaporation method gasoline desulfurization is compound
The preparation method of film, which is characterized in that in step d：The standing and defoaming time is 12h.
10. polyvinyl butyral/polyacrylonitrile according to claim 3 for pervaporation method gasoline desulfurization is compound
The preparation method of film, which is characterized in that in step e：Using 50~100 μm of scraper film, acquired polyvinyl butyral
The thickness of film layer is 10~15 μm；It is 60 DEG C~65 DEG C to control the temperature in air dry oven.
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Cited By (3)
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| CN109251765A (en) * | 2018-10-31 | 2019-01-22 | 中国石油大学(华东) | Polyurethane/poly-vinylidene-fluoride composite film and preparation method thereof of organic sulfur compound is extracted in a kind of naphtha |
| CN111013411A (en) * | 2019-12-17 | 2020-04-17 | 美蓝飘尔(上海)过滤设备有限公司 | Nanofiltration membrane for purifying water and preparation method and application thereof |
| CN111992059A (en) * | 2020-09-01 | 2020-11-27 | 安徽美邦树脂科技有限公司 | PVB-based ultrafiltration membrane and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109251765A (en) * | 2018-10-31 | 2019-01-22 | 中国石油大学(华东) | Polyurethane/poly-vinylidene-fluoride composite film and preparation method thereof of organic sulfur compound is extracted in a kind of naphtha |
| CN109251765B (en) * | 2018-10-31 | 2020-05-05 | 中国石油大学(华东) | Polyurethane/polyvinylidene fluoride composite membrane for extracting organic sulfide from naphtha and preparation method thereof |
| US11458438B2 (en) | 2018-10-31 | 2022-10-04 | China University Of Petroleum(East China) | Polyurethane/polyvinylidene fluoride composite membrane for extracting organic sulfide from naphtha and preparation method therefor |
| CN111013411A (en) * | 2019-12-17 | 2020-04-17 | 美蓝飘尔(上海)过滤设备有限公司 | Nanofiltration membrane for purifying water and preparation method and application thereof |
| CN111013411B (en) * | 2019-12-17 | 2021-10-01 | 美蓝飘尔(上海)过滤设备有限公司 | Nanofiltration membrane for purifying water and preparation method and application thereof |
| CN111992059A (en) * | 2020-09-01 | 2020-11-27 | 安徽美邦树脂科技有限公司 | PVB-based ultrafiltration membrane and preparation method thereof |
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| CN108211823B (en) | 2019-12-06 |
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