CN101664648A - Complex film for gasoline desulfurization by pervaporation and preparation method thereof - Google Patents
Complex film for gasoline desulfurization by pervaporation and preparation method thereof Download PDFInfo
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- CN101664648A CN101664648A CN 200910023323 CN200910023323A CN101664648A CN 101664648 A CN101664648 A CN 101664648A CN 200910023323 CN200910023323 CN 200910023323 CN 200910023323 A CN200910023323 A CN 200910023323A CN 101664648 A CN101664648 A CN 101664648A
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Abstract
The invention relates to a complex film for gasoline desulfurization by pervaporation and a preparation method thereof. The preparation method comprises the following steps: dissolving aniline into ahydrochloride solution, adding into an oxidant dissolved with deionized water, and obtaining a polyaniline solid material through reaction; dissolving polyvinyl alcohol into the deionized water to prepare a polyvinyl alcohol solution, and adding polyaniline powder to prepare a blending film liquid; scraping the prepared film liquid onto a pre-prepared bottom film; and carrying out heat treatment to obtain the complex film needing to be prepared. The prepared complex film contains 0.1-3 percent of polyaniline PANI by mass and 97-99.9 percent of polyvinyl alcohol PVA by mass, can remove the organic sulfur in gasoline with high selectivity in gasoline desulfurization, overcomes the defect of low self-flux of other existing film materials, and can greatly increase the permeation flux while keeping excellent separation performance.
Description
Technical field
The present invention relates to a kind of infiltrating and vaporizing membrane separation technology field, particularly a kind of complex film for gasoline desulfurization by pervaporation and preparation method thereof of belonging to.
Background technology
Be the protection environment, each country has limited the content of sulfur in gasoline by legal form.Sulphur in the gasoline is the direct sources of various SOx in the air, has also destroyed the low temperature active of automobile catalytic cleaner simultaneously.When considering that fuel composition changes the influencing of discharging, reduce sulfur content and have maximum potentiality for the total release that reduces hydrocarbon, CO and NOx.Sulfide existence form in the catalytic gasoline is based on these 4 kinds of organic sulfur compounds of thiophene-based, mercaptan, thioether and disulphide, wherein the content of thiophene sulphur accounts for more than 60% of total sulfur content, and the content of thioether sulphur and thiophenic sulfur accounts for more than 85% of total sulfur, and FCC is similar substantially with content distribution with the sulphur type in the RFCC gasoline.
Though more existing sulfur methods are all undesirable, although hydrotreatment can make the sulfur content of gasoline reduce to the level of any needs, installing or increasing necessary hydrotreatment ability needs appreciable investment and high running cost.In addition, alkene and cyclanes compound to the hydrogenation sensitivity, can cause octane number significantly to reduce during hydrotreatment.For this reason, it is very necessary to continue to seek new desulfur technology.
The core of infiltration evaporation is the selection of membrane material, the gasoline main component is C4～C12 hydro carbons, be one of hydrocarbon mixture article, it is a kind of colourless or faint yellow, volatile and flammable liquid, has off-odor, its special odor is owing to contain the extremely sulfurous organic compound of trace in the gasoline, mainly is mercaptan, thioether.The character such as the table 1 of key component in the gasoline:
Table 1 physical parameter
| Component | Molecular weight (gmol -1) | Molal volume (cm 3mol -1) | Solubility parameter (J 1/2cm -.3/2) | Boiling point (℃) |
| Normal heptane | ??100.21 | ??147.5 | ??15.3 | ??98.5 |
| N-butyl mercaptan | ??90.18 | ??109.8 | ??18.4 | ??98.4 |
| Ethyl sulfide | ??90.18 | ??111.2 | ??18.1 | ??95.0 |
The immense pressure that current as can be seen from the above table petroleum chemical enterprise is faced aspect gasoline desulfur.At first, because the boiling point of these several components is extremely close, if by traditional distillation or rectifying, reach qualified gasoline sulfure content, just need constantly to increase the quantity and the rectifying progression of column plate, therefore so not only can consume a large amount of energy, and can propose great challenge to equipment, traditional distillation, rectifying means have no advantage and can say in the desulfurization of analog gasoline.Secondly, according to the solubility parameter principle, when a kind of solubility of substances during near the solubility parameter of infiltrating and vaporizing membrane, this material will be in surperficial preferential adsorption, the dissolving of film, and then realize the enrichment of component to be separated, but from table 1, find that the gap of solubility parameter of component to be separated and normal heptane is very little.Therefore from the angle of solubility parameter, be difficult to find a suitable membrane material to realize removing of sulfur-containing compound in the normal heptane.Once more, investigate from the angle of sieve effect, sieve effect is the basic point of departure of a lot of lock out operation, mainly is to utilize the gap of component to be separated on volume (comprising the volume of macroscopic particles and atom, molecule volume), bulky component is trapped, and the component that volume is little is removed thoroughly.But in these several components of analog gasoline, the gap of individual molecule volume is also little, and the trickle gap on the microcosmic makes that the selection of membrane material is more difficult.
Summary of the invention
In order to overcome above-mentioned the deficiencies in the prior art, the object of the present invention is to provide a kind of complex film for gasoline desulfurization by pervaporation and preparation method thereof, prepared film has overcome the existing low shortcoming of other membrane materials self flux, can be when keeping outstanding separating property, permeation flux increases considerably.
In order to achieve the above object, technical scheme of the present invention is achieved in that
A kind of preparation method of complex film for gasoline desulfurization by pervaporation may further comprise the steps:
(1) aniline is dissolved in the 1-1.5mol/L hydrochloric acid HCl solution, the aniline mass percent concentration is 6-12%, is cooled to 0-10 ℃ with ice bath; The ammonium persulfate oxidant is dissolved in the deionized water, and the ammonium persulfate mass percent concentration is 15-25%, is chilled to 0-10 ℃ in advance; The above-mentioned ammonium sulfate oxidizing agent solution that is dissolved in the deionized water is dropped in the aniline solution with the speed of dropping funel by the 2-10 ml/min by 1: 1 mass ratio, in course of reaction, use ice-water bath control reaction temperature to be 0-5 ℃, react and stopped in 5-9 hour reacting; Adopt 80-100 purpose filter cloth to carry out vacuum filtration; Under 60-100 ℃ of condition vacuum drying 10-24 hour, obtain the polyaniline solids material;
(2) PVAC polyvinylalcohol is dissolved in 70-90 ℃ the deionized water, the PVAC polyvinylalcohol mass percent is 8-10%, keep 70-90 ℃ temperature stabilization 3-5 hour, obtain PVAC polyvinylalcohol solution, be cooled to normal temperature, it is standby to bottle;
(3) become the 60-100 purpose Powdered the polyaniline solids material porphyrize that obtains in the step 1, polyaniline powder is dispersed in the PVAC polyvinylalcohol solution of step 2, polyaniline PANI accounts for the 0.1-3% of gross mass, adopt conventional ultra-sonic dispersion method, jitter time is 1-5 hour, cause the volatilization in advance of solvent in order to prevent that solution temperature from raising during this period, use ice cube to control its temperature and be 0-10 ℃;
(4) after the blend film liquid of gained in the step 3 filtration deaeration, hydrostomia is on preprepared milipore filter uniformly, and thickness is 20-100 μ m; Dry under infrared lamp 30-50 ℃, make solvent evaporates 2-6 hour, dry 6-20 hour film forming under 80-120 ℃ is the composite membrane that will prepare in baking oven.
The composite film material composition that the present invention makes is:
Polyaniline PANI quality percentage composition is 0.1-3%, and the PVAC polyvinylalcohol mass percent is 97-99.9%.
The separating property of the prepared film of the present invention is by flux and two parameter evaluations of rich thioneine.The fluxmeter formula is as follows:
Rich thioneine sub-definite formula is as follows:
In the formula, C
PAnd C
FBe respectively the feed liquid side and see through the sulfur content of side.
The invention has the beneficial effects as follows: the present invention is with low cost, to the sulfide in the gasoline have stronger selection permeability, can withstand high temperatures, can tolerate the complex component in the liquefied gas.Have a extensive future, particularly important aspect the environmental protection of increasingly stringent.This new technology will have been opened up a new road for China pollutes from watershed management city SOx poisonous gas, to promoting and promoting the scientific and technical innovation and the technological progress of Environmental Protection in China and petroleum chemical enterprise to have material impact.
The specific embodiment
Below in conjunction with specific embodiment technical scheme of the present invention is further described.
Embodiment one
The preparation method of present embodiment is achieved in that and may further comprise the steps:
(1) aniline is dissolved in the 1mol/L hydrochloric acid HCl solution, the aniline mass percent concentration is 8%, is cooled to 0 ℃ with ice bath; The ammonium persulfate oxidant is dissolved in the deionized water, and the ammonium persulfate mass percent concentration is 20%, is chilled to 0 ℃ in advance; The above-mentioned ammonium sulfate oxidizing agent solution that is dissolved in the deionized water is dropped in the aniline solution with the speed of dropping funel by 4 ml/min by 1: 1 mass ratio, and using ice-water bath control reaction temperature in course of reaction is 0 ℃, reacts to stop reaction in 6 hours; Adopt 80 purpose filter clothes to carry out vacuum filtration; Vacuum drying is 12 hours under 70 ℃ of conditions, obtains the polyaniline solids material;
(2) PVAC polyvinylalcohol is dissolved in 70 ℃ the deionized water, the PVAC polyvinylalcohol mass percent is 8%, keeps 70 ℃ of temperature stabilizations 4 hours, obtains PVAC polyvinylalcohol solution, is cooled to normal temperature, and it is standby to bottle;
(3) become 60 purposes Powdered the polyaniline solids material porphyrize that obtains in the step 1, polyaniline powder is dispersed in the PVAC polyvinylalcohol solution of step 2, polyaniline PANI accounts for 0.8% of gross mass, adopt conventional ultra-sonic dispersion method, jitter time is 2 hours, cause the volatilization in advance of solvent in order to prevent that solution temperature from raising during this period, using ice cube to control its temperature is 0 ℃;
(4) after the blend film liquid of gained in the step 3 filtration deaeration, hydrostomia is on preprepared milipore filter uniformly, and thickness is 40 μ m; Dry down 30 ℃ of infrared lamps, made solvent evaporates 6 hours, 80 ℃ of down dry 8 hours film forming are the composite membrane that will prepare in baking oven.
The composite film material composition that present embodiment makes is:
Polyaniline PANI quality percentage composition is 0.8%, and the PVAC polyvinylalcohol mass percent is 99.2%.
Embodiment two
The preparation technology of present embodiment is achieved in that and may further comprise the steps:
(1) aniline is dissolved in the 1.5mol/L hydrochloric acid HCl solution, the aniline mass percent concentration is 10%, is cooled to 2 ℃ with ice bath; The ammonium persulfate oxidant is dissolved in the deionized water, and the ammonium persulfate mass percent concentration is 25%, is chilled to 5 ℃ in advance; The above-mentioned ammonium sulfate oxidizing agent solution that is dissolved in the deionized water is dropped in the aniline solution with the speed of dropping funel by 6 ml/min by 1: 1 mass ratio, and using ice-water bath control reaction temperature in course of reaction is 2 ℃, reacts to stop reaction in 7 hours; Adopt 90 purpose filter clothes to carry out vacuum filtration; Vacuum drying is 16 hours under 80 ℃ of conditions, obtains the polyaniline solids material;
(2) PVAC polyvinylalcohol is dissolved in 80 ℃ the deionized water, the PVAC polyvinylalcohol mass percent is 9%, keeps 80 ℃ of temperature stabilizations 5 hours, obtains PVAC polyvinylalcohol solution, is cooled to normal temperature, and it is standby to bottle;
(3) become 90 purposes Powdered the polyaniline solids material porphyrize that obtains in the step 1, polyaniline powder is dispersed in the PVAC polyvinylalcohol solution of step 2, polyaniline PANI accounts for 1% of gross mass, adopt conventional ultra-sonic dispersion method, jitter time is 1 hour, cause the volatilization in advance of solvent in order to prevent that solution temperature from raising during this period, using ice cube to control its temperature is 5 ℃;
(4) after the blend film liquid of gained in the step 3 filtration deaeration, hydrostomia is on preprepared milipore filter uniformly, and thickness is 30 μ m; Dry down 35 ℃ of infrared lamps, made solvent evaporates 4 hours, 90 ℃ of down dry 16 hours film forming are the composite membrane that will prepare in baking oven.
The composite film material composition that present embodiment makes is:
Polyaniline PANI quality percentage composition is 1%, and the PVAC polyvinylalcohol mass percent is 99%.
Embodiment three
The preparation method of present embodiment is achieved in that and may further comprise the steps:
(1) aniline is dissolved in the 1.2mol/L hydrochloric acid HCl solution, the aniline mass percent concentration is 10%, is cooled to 5 ℃ with ice bath; The ammonium persulfate oxidant is dissolved in the deionized water, and the ammonium persulfate mass percent concentration is 22%, is chilled to 3 ℃ in advance; The above-mentioned ammonium sulfate oxidizing agent solution that is dissolved in the deionized water is dropped in the aniline solution with the speed of dropping funel by 8 ml/min by 1: 1 mass ratio, and using ice-water bath control reaction temperature in course of reaction is 5 ℃, reacts to stop reaction in 9 hours; Adopt 100 purpose filter clothes to carry out vacuum filtration; Vacuum drying is 24 hours under 90 ℃ of conditions, obtains the polyaniline solids material;
(2) PVAC polyvinylalcohol is dissolved in 85 ℃ the deionized water, the PVAC polyvinylalcohol mass percent is 10%, keeps 90 ℃ of temperature stabilizations 3 hours, obtains PVAC polyvinylalcohol solution, is cooled to normal temperature, and it is standby to bottle;
(3) become 80 purposes Powdered the polyaniline solids material porphyrize that obtains in the step 1, polyaniline powder is dispersed in the PVAC polyvinylalcohol solution of step 2, polyaniline PANI accounts for 2% of gross mass, adopt conventional ultra-sonic dispersion method, jitter time is 3 hours, cause the volatilization in advance of solvent in order to prevent that solution temperature from raising during this period, using ice cube to control its temperature is 2 ℃;
(4) after the blend film liquid of gained in the step 3 filtration deaeration, hydrostomia is on preprepared milipore filter uniformly, and thickness is 60 μ m; Dry down 45 ℃ of infrared lamps, made solvent evaporates 3 hours, 90 ℃ of down dry 11 hours film forming are the composite membrane that will prepare in baking oven.
The composite film material composition that present embodiment makes is:
Polyaniline PANI quality percentage composition is 2%, and the PVAC polyvinylalcohol mass percent is 98%.
More than 3 prepared composite membrane performances of embodiment see the following form
Annotate: infiltration evaporation performance test time 2h; Effective film area 2.17 * 10
-3m
2
Claims (8)
1, a kind of preparation method of complex film for gasoline desulfurization by pervaporation is characterized in that, may further comprise the steps: (1) is dissolved in aniline in the 1-1.5mol/L hydrochloric acid HCl solution, and the aniline mass percent concentration is 6-12%, is cooled to 0-10 ℃ with ice bath; The ammonium persulfate oxidant is dissolved in the deionized water, and the ammonium persulfate mass percent concentration is 15-25%, is chilled to 0-10 ℃ in advance; The above-mentioned ammonium sulfate oxidizing agent solution that is dissolved in the deionized water is dropped in the aniline solution with the speed of dropping funel by the 2-10 ml/min by 1: 1 mass ratio, in course of reaction, use ice-water bath control reaction temperature to be 0-5 ℃, react and stopped in 5-9 hour reacting; Adopt 80-100 purpose filter cloth to carry out vacuum filtration; Under 60-100 ℃ of condition vacuum drying 10-24 hour, obtain the polyaniline solids material; (2) PVAC polyvinylalcohol is dissolved in 70-90 ℃ the deionized water, the PVAC polyvinylalcohol mass percent is 8-10%, keep 70-90 ℃ temperature stabilization 3-5 hour, obtain PVAC polyvinylalcohol solution, be cooled to normal temperature, it is standby to bottle; (3) become the 60-100 purpose Powdered the polyaniline solids material porphyrize that obtains in the step 1, polyaniline powder is dispersed in the PVAC polyvinylalcohol solution of step 2, polyaniline PANI accounts for the 0.1-3% of gross mass, adopt conventional ultra-sonic dispersion method, jitter time is 1-5 hour, uses ice cube to control its temperature and is 0-10 ℃; (4) after the blend film liquid of gained in the step 3 filtration deaeration, hydrostomia is on preprepared milipore filter uniformly, and thickness is 20-100 μ m; Dry under infrared lamp 30-50 ℃, make solvent evaporates 2-6 hour, dry 6-20 hour film forming under 80-120 ℃ is the composite membrane that will prepare in baking oven.
2, the preparation method of a kind of complex film for gasoline desulfurization by pervaporation according to claim 1 is characterized in that, (1) is dissolved in aniline in the 1mol/L hydrochloric acid HCl solution, and the aniline mass percent concentration is 8%, is cooled to 0 ℃ with ice bath; The ammonium persulfate oxidant is dissolved in the deionized water, and the ammonium persulfate mass percent concentration is 20%, is chilled to 0 ℃ in advance; The above-mentioned ammonium sulfate oxidizing agent solution that is dissolved in the deionized water is dropped in the aniline solution with the speed of dropping funel by 4 ml/min by 1: 1 mass ratio, and using ice-water bath control reaction temperature in course of reaction is 0 ℃, reacts to stop reaction in 6 hours; Adopt 80 purpose filter clothes to carry out vacuum filtration; Vacuum drying is 12 hours under 70 ℃ of conditions, obtains the polyaniline solids material; (2) PVAC polyvinylalcohol is dissolved in 70 ℃ the deionized water, the PVAC polyvinylalcohol mass percent is 8%, keeps 70 ℃ of temperature stabilizations 4 hours, obtains PVAC polyvinylalcohol solution, is cooled to normal temperature, and it is standby to bottle; (3) become 60 purposes Powdered the polyaniline solids material porphyrize that obtains in the step 1, polyaniline powder is dispersed in the PVAC polyvinylalcohol solution of step 2, polyaniline PANI accounts for 0.8% of gross mass, adopt conventional ultra-sonic dispersion method, jitter time is 2 hours, and using ice cube to control its temperature is 0 ℃; (4) after the blend film liquid of gained in the step 3 filtration deaeration, hydrostomia is on preprepared milipore filter uniformly, and thickness is 40 μ m; Dry down 30 ℃ of infrared lamps, made solvent evaporates 6 hours, 80 ℃ of down dry 8 hours film forming are the composite membrane that will prepare in baking oven.
3, the preparation method of a kind of complex film for gasoline desulfurization by pervaporation according to claim 1 is characterized in that, (1) is dissolved in aniline in the 1.5mol/L hydrochloric acid HCl solution, and the aniline mass percent concentration is 10%, is cooled to 2 ℃ with ice bath; The ammonium persulfate oxidant is dissolved in the deionized water, and the ammonium persulfate mass percent concentration is 25%, is chilled to 5 ℃ in advance; The above-mentioned ammonium sulfate oxidizing agent solution that is dissolved in the deionized water is dropped in the aniline solution with the speed of dropping funel by 6 ml/min by 1: 1 mass ratio, and using ice-water bath control reaction temperature in course of reaction is 2 ℃, reacts to stop reaction in 7 hours; Adopt 90 purpose filter clothes to carry out vacuum filtration; Vacuum drying is 16 hours under 80 ℃ of conditions, obtains the polyaniline solids material; (2) PVAC polyvinylalcohol is dissolved in 80 ℃ the deionized water, the PVAC polyvinylalcohol mass percent is 9%, keeps 80 ℃ of temperature stabilizations 5 hours, obtains PVAC polyvinylalcohol solution, is cooled to normal temperature, and it is standby to bottle; (3) become 90 purposes Powdered the polyaniline solids material porphyrize that obtains in the step 1, polyaniline powder is dispersed in the PVAC polyvinylalcohol solution of step 2, polyaniline PANI accounts for 1% of gross mass, adopt conventional ultra-sonic dispersion method, jitter time is 1 hour, and using ice cube to control its temperature is 5 ℃; (4) after the blend film liquid of gained in the step 3 filtration deaeration, hydrostomia is on preprepared milipore filter uniformly, and thickness is 30 μ m; Dry down 35 ℃ of infrared lamps, made solvent evaporates 4 hours, 90 ℃ of down dry 16 hours film forming are the composite membrane that will prepare in baking oven.
4, the preparation method of a kind of complex film for gasoline desulfurization by pervaporation according to claim 1 is characterized in that, (1) is dissolved in aniline in the 1.2mol/L hydrochloric acid HCl solution, and the aniline mass percent concentration is 10%, is cooled to 5 ℃ with ice bath; The ammonium persulfate oxidant is dissolved in the deionized water, and the ammonium persulfate mass percent concentration is 22%, is chilled to 3 ℃ in advance; The above-mentioned ammonium sulfate oxidizing agent solution that is dissolved in the deionized water is dropped in the aniline solution with the speed of dropping funel by 8 ml/min by 1: 1 mass ratio, and using ice-water bath control reaction temperature in course of reaction is 5 ℃, reacts to stop reaction in 9 hours; Adopt 100 purpose filter clothes to carry out vacuum filtration; Vacuum drying is 24 hours under 90 ℃ of conditions, obtains the polyaniline solids material; (2) PVAC polyvinylalcohol is dissolved in 85 ℃ the deionized water, the PVAC polyvinylalcohol mass percent is 10%, keeps 90 ℃ of temperature stabilizations 3 hours, obtains PVAC polyvinylalcohol solution, is cooled to normal temperature, and it is standby to bottle; (3) become 80 purposes Powdered the polyaniline solids material porphyrize that obtains in the step 1, polyaniline powder is dispersed in the PVAC polyvinylalcohol solution of step 2, polyaniline PANI accounts for 2% of gross mass, adopt conventional ultra-sonic dispersion method, jitter time is 3 hours, and using ice cube to control its temperature is 2 ℃; (4) after the blend film liquid of gained in the step 3 filtration deaeration, hydrostomia is on preprepared milipore filter uniformly, and thickness is 60 μ m; Dry down 45 ℃ of infrared lamps, made solvent evaporates 3 hours, 90 ℃ of down dry 11 hours film forming are the composite membrane that will prepare in baking oven.
5, a kind of complex film for gasoline desulfurization by pervaporation is characterized in that, polyaniline PANI quality percentage composition is 0.1-3%, and the PVAC polyvinylalcohol mass percent is 97-99.9%.
6, a kind of complex film for gasoline desulfurization by pervaporation according to claim 5 is characterized in that, polyaniline PANI quality percentage composition is 0.8%, and the PVAC polyvinylalcohol mass percent is 99.2%.
7, a kind of complex film for gasoline desulfurization by pervaporation according to claim 5 is characterized in that, polyaniline PANI quality percentage composition is 1%, and the PVAC polyvinylalcohol mass percent is 99%.
8, a kind of complex film for gasoline desulfurization by pervaporation according to claim 5 is characterized in that, polyaniline PANI quality percentage composition is 2%, and the PVAC polyvinylalcohol mass percent is 98%.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102302904A (en) * | 2011-05-17 | 2012-01-04 | 清华大学 | Method for preparing polystyrene maleimide membrane for gasoline desulfurization by pervaporation |
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| CN108211823B (en) * | 2018-01-24 | 2019-12-06 | 中国石油大学(华东) | Polyvinyl butyral/polyacrylonitrile composite film for gasoline desulfurization and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102302904A (en) * | 2011-05-17 | 2012-01-04 | 清华大学 | Method for preparing polystyrene maleimide membrane for gasoline desulfurization by pervaporation |
| CN102302904B (en) * | 2011-05-17 | 2013-07-03 | 清华大学 | Method for preparing polystyrene maleimide membrane for gasoline desulfurization by pervaporation |
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