CN103627529A - Deacidification method used in biodiesel preparation from Chinese prickly ash seed oil - Google Patents
Deacidification method used in biodiesel preparation from Chinese prickly ash seed oil Download PDFInfo
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- CN103627529A CN103627529A CN201210296648.9A CN201210296648A CN103627529A CN 103627529 A CN103627529 A CN 103627529A CN 201210296648 A CN201210296648 A CN 201210296648A CN 103627529 A CN103627529 A CN 103627529A
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- oil
- fructus zanthoxyli
- prickly ash
- chinese prickly
- seed oil
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
- Y02E50/10—Biofuels, e.g. bio-diesel
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Abstract
The invention relates to a deacidification method used in biodiesel preparation from Chinese prickly ash seed oil. The deacidification method comprises the following steps of 1, carrying out degumming treatment on Chinese prickly ash seed oil, 2, carrying out decoloring on the Chinese prickly ash seed oil, 3, weighing a certain amount of the Chinese prickly ash seed oil, pre-heating the Chinese prickly ash seed oil in a three-necked bottle to a reaction temperature, adding a certain amount of a fully-mixed methanol-concentrated sulfuric acid solution pre-heated to the same temperature into the three-necked bottle, and carrying out stirring for a certain time, and 4, transferring the reaction product to a separating funnel, standing it until the next day, transferring an upper methanol aqueous phase to a rotary evaporator, evaporating methanol, standing a lower esterified oil phase in the separating funnel for a time period, washing the lower esterified oil phase by water, carrying out drying by anhydrous sodium sulfate, and carrying out pumping filtration to obtain esterified oil. Through degumming and decoloring, colloid and chroma of the Chinese prickly ash seed oil are obviously reduced, Chinese prickly ash seed oil quality is improved, and a follow-up deacidification process can be carried out normally. The deacidification method is simple and feasible.
Description
Technical field
The present invention relates to chemical industry energy field, specifically a kind of method of deacidification while utilizing Fructus Zanthoxyli oil to prepare biofuel.
Background technology
Biofuel is the longer chain fatty acid first Ester being generated by transesterification reaction by animal-plant oil and methyl alcohol, is desirable petrifaction diesel substitute.Biofuel is hardly containing aromatic hydrocarbon and sulphur; combustion processes is little to the damage ratio petrifaction diesel of environment; the carbonic acid gas that the carbonic acid gas that simultaneously its combustion processes discharges absorbs far fewer than growing process, therefore use biofuel to protection of the environment, alleviate global greenhouse effect and there is positive effect.
At present, at the animal and plant grease of take of studying, be the high expensive that raw material is manufactured biofuel, Semen Pericarpium Zanthoxyli is the by product obtaining after Chinese prickly ash plantation, wide material sources, cheap and easy to get, the raw material using it as biofuel, has broad prospects.But in Semen Pericarpium Zanthoxyli crude oil, containing a large amount of free fatty acidies (FFA), if adopt base catalysis technique, must carry out deacidification treatment, otherwise FFA can generate saponifiedly with alkali reaction, causes productive rate lower, meanwhile, soap also can hinder biofuel and sweet oil separating.Transesterification reaction requires the acid number of grease to be preferably in 2 mgKOH/g left and right, does not occur the requirement of saponification phenomenon to reach next step transesterify stage.The FFA that contains 30% left and right in Fructus Zanthoxyli oil.
Summary of the invention
According to above-mentioned weak point, the object of this invention is to provide a kind of method of deacidification while utilizing Fructus Zanthoxyli oil to prepare biofuel.
Technical scheme of the present invention is: a kind of method of deacidification while utilizing Fructus Zanthoxyli oil to prepare biofuel, it comprises
1) degumming process of Fructus Zanthoxyli oil: in isothermal reaction still, Fructus Zanthoxyli oil is preheated to 60-70 ℃, adds the phosphoric acid of the heavy 0.2-0.3% of oil, be chilled to 35-40 ℃ after stirring 20-30min.Add hot water, make colloid aquation, after stirring 15-20 min, add the NaOH solution of 1.5-2%, to neutralize excessive phosphoric acid, and make colloid flocculation, continue to stir 15-20 min, finally standing 2 h at 75 ℃.Through centrifugal, washing, dry, Fructus Zanthoxyli oil must come unstuck.
2) decolouring of Fructus Zanthoxyli oil is processed: in the Fructus Zanthoxyli oil that comes unstuck, add alkali lye, stirring at normal temperature, after fluid is separated, precipitate centrifugal, fluid is separated with soap lye.Fluid washs with soft water, repeatedly, obtains final fluid, after concentrating, obtains alkali refining oil (Fructus Zanthoxyli oil after decolouring).
3) take the Fructus Zanthoxyli oil of certainweight, in three-necked bottle, be preheated to temperature of reaction, add a certain amount of methyl alcohol concentrated sulfuric acid solution being preheated to after uniform temp abundant miscible, stir certain hour.
4) reaction product is transferred to separating funnel, spends the night.Upper strata methanol-water phase transition boils off methyl alcohol to Rotary Evaporators.Lower floor's esterification oil phase standing for some time in separating funnel, washing, with anhydrous sodium sulfate drying, suction filtration, obtains esterised oil.
Preferably: the optimum process condition of Fructus Zanthoxyli oil methanol esterification deacidification is: catalyzer vitriol oil concentration is 2-2.5%, molar ratio of methanol to oil is 25-30, and the reaction times is 2-3h, and temperature of reaction is 60-65 ℃.
The invention has the beneficial effects as follows: the present invention, through the processing of coming unstuck and decolour, can make the colloid of Fructus Zanthoxyli oil and colourity significantly reduce, and has improved the quality of Fructus Zanthoxyli oil, be conducive to normally the carrying out of depickling treatment process in later stage, and method simple possible.
Embodiment
Embodiment 1
A method for deacidification while utilizing Fructus Zanthoxyli oil to prepare biofuel, it comprises
1) degumming process of Fructus Zanthoxyli oil: Fructus Zanthoxyli oil is preheated to 60 ℃ in isothermal reaction still, adds oil to weigh 0.2% phosphoric acid, be chilled to 40 ℃ after stirring 20min.Add hot water, make colloid aquation, stir the NaOH solution that adds 1.8% after 20 min, to neutralize excessive phosphoric acid, and make colloid flocculation, continue to stir 15 min, finally standing 2 h at 75 ℃.Through centrifugal, washing, dry, Fructus Zanthoxyli oil must come unstuck.
2) decolouring of Fructus Zanthoxyli oil is processed: in the Fructus Zanthoxyli oil that comes unstuck, add alkali lye, stirring at normal temperature, after fluid is separated, precipitate centrifugal, fluid is separated with soap lye.Fluid washs with soft water, repeatedly, obtains final fluid, after concentrating, obtains alkali refining oil (Fructus Zanthoxyli oil after decolouring).
3) taking the Fructus Zanthoxyli oil of certainweight, be preheated to 65 ℃ in three-necked bottle, is 25 to add the methyl alcohol concentrated sulfuric acid solution being preheated to after uniform temp abundant miscible by molar ratio of methanol to oil, and wherein vitriol oil concentration is 2%, stirs 2h.
4) reaction product is transferred to separating funnel, spends the night.Upper strata methanol-water phase transition boils off methyl alcohol to Rotary Evaporators.Lower floor's esterification oil phase standing for some time in separating funnel, washing, with anhydrous sodium sulfate drying, suction filtration, obtains esterised oil.
Now, Fructus Zanthoxyli oil acid number is 1.69 mg KOH/g.
Embodiment 2
A method for deacidification while utilizing Fructus Zanthoxyli oil to prepare biofuel, it comprises
1) degumming process of Fructus Zanthoxyli oil: Fructus Zanthoxyli oil is preheated to 68 ℃ in isothermal reaction still, adds oil to weigh 0.25% phosphoric acid, be chilled to 35 ℃ after stirring 20min.Add hot water, make colloid aquation, stir the NaOH solution that adds 1.5% after 20 min, to neutralize excessive phosphoric acid, and make colloid flocculation, continue to stir 15 min, finally standing 2 h at 75 ℃.Through centrifugal, washing, dry, Fructus Zanthoxyli oil must come unstuck.
2) decolouring of Fructus Zanthoxyli oil is processed: in the Fructus Zanthoxyli oil that comes unstuck, add alkali lye, stirring at normal temperature, after fluid is separated, precipitate centrifugal, fluid is separated with soap lye.Fluid washs with soft water, repeatedly, obtains final fluid, after concentrating, obtains alkali refining oil (Fructus Zanthoxyli oil after decolouring).
3) taking the Fructus Zanthoxyli oil of certainweight, be preheated to 60 ℃ in three-necked bottle, is 30 to add the methyl alcohol concentrated sulfuric acid solution being preheated to after uniform temp abundant miscible by molar ratio of methanol to oil, and wherein vitriol oil concentration is 2.5%, stirs 2.5h.
4) reaction product is transferred to separating funnel, spends the night.Upper strata methanol-water phase transition boils off methyl alcohol to Rotary Evaporators.Lower floor's esterification oil phase standing for some time in separating funnel, washing, with anhydrous sodium sulfate drying, suction filtration, obtains esterised oil.
Now, Fructus Zanthoxyli oil acid number is 1.35 mg KOH/g.
Claims (2)
1. a method for deacidification while utilizing Fructus Zanthoxyli oil to prepare biofuel, it comprises
1) degumming process of Fructus Zanthoxyli oil: in isothermal reaction still, Fructus Zanthoxyli oil is preheated to 60-70 ℃, adds the phosphoric acid of the heavy 0.2-0.3% of oil, be chilled to 35-40 ℃ after stirring 20-30min;
Add hot water, make colloid aquation, after stirring 15-20 min, add the NaOH solution of 1.5-2%, to neutralize excessive phosphoric acid, and make colloid flocculation, continue to stir 15-20 min, finally standing 2 h at 75 ℃;
Through centrifugal, washing, dry, Fructus Zanthoxyli oil must come unstuck;
2) decolouring of Fructus Zanthoxyli oil is processed: in the Fructus Zanthoxyli oil that comes unstuck, add alkali lye, stirring at normal temperature, after fluid is separated, precipitate centrifugal, fluid is separated with soap lye;
Fluid washs with soft water, repeatedly, obtains final fluid, after concentrating, obtains alkali refining oil (Fructus Zanthoxyli oil after decolouring);
3) take the Fructus Zanthoxyli oil of certainweight, in three-necked bottle, be preheated to temperature of reaction, add a certain amount of methyl alcohol concentrated sulfuric acid solution being preheated to after uniform temp abundant miscible, stir certain hour;
4) reaction product is transferred to separating funnel, spends the night, upper strata methanol-water phase transition boils off methyl alcohol to Rotary Evaporators; Lower floor's esterification oil phase standing for some time in separating funnel, washing, with anhydrous sodium sulfate drying, suction filtration, obtains esterised oil.
2. according to a kind of method of deacidification while utilizing Fructus Zanthoxyli oil to prepare biofuel claimed in claim 1, it is characterized in that: the optimum process condition of Fructus Zanthoxyli oil methanol esterification deacidification is: catalyzer vitriol oil concentration is 2-2.5%, molar ratio of methanol to oil is 25-30, reaction times is 2-3h, and temperature of reaction is 60-65 ℃.
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| CN201210296648.9A CN103627529A (en) | 2012-08-21 | 2012-08-21 | Deacidification method used in biodiesel preparation from Chinese prickly ash seed oil |
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| CN201210296648.9A CN103627529A (en) | 2012-08-21 | 2012-08-21 | Deacidification method used in biodiesel preparation from Chinese prickly ash seed oil |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105268456A (en) * | 2015-11-10 | 2016-01-27 | 陕西科技大学 | Solid acid catalyst, preparing method of solid acid catalyst and acid reducing method based on catalyst |
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- 2012-08-21 CN CN201210296648.9A patent/CN103627529A/en active Pending
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105268456A (en) * | 2015-11-10 | 2016-01-27 | 陕西科技大学 | Solid acid catalyst, preparing method of solid acid catalyst and acid reducing method based on catalyst |
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Application publication date: 20140312 |