CN101392181A - Novel method for preparing biodiesel by in situ extraction of rice oil - Google Patents
Novel method for preparing biodiesel by in situ extraction of rice oil Download PDFInfo
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- CN101392181A CN101392181A CNA2008100513806A CN200810051380A CN101392181A CN 101392181 A CN101392181 A CN 101392181A CN A2008100513806 A CNA2008100513806 A CN A2008100513806A CN 200810051380 A CN200810051380 A CN 200810051380A CN 101392181 A CN101392181 A CN 101392181A
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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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- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P30/00—Technologies relating to oil refining and petrochemical industry
- Y02P30/20—Technologies relating to oil refining and petrochemical industry using bio-feedstock
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Abstract
The invention discloses a new method for preparing a bio-diesel through in situ extraction of rice bran oil, which takes rice bran as a raw material and combines oil extraction and bio-diesel preparation technologies into a whole through the steps of in situ oil extraction- acid catalysis and esterification, synchronous dehydration, acid-base system transition, alkali catalysis and tranesterification, separation and purification of products and the like. The new method, by using the synchronous dehydration and acid-base gradual transition technology, avoids over high concentration of local alkali-water generated which can cause the problem of saponification, wipes off the intermediate trivial raw material treatment process in preparing the bio-diesel by the existing acid-base two-step approach technique and reduces the production cost of the bio-diesel.
Description
Technical field
The present invention relates to a kind of novel method of preparing biodiesel by in situ extraction of rice oil, particularly relate to the technology that dewaters synchronously in this technology and the novel method of soda acid transitional technology and correlation technique thereof.
Background technology
Energy dilemma, environmental degradation have caused the attention of countries in the world, seek renewable new forms of energy, substitute energy and be very urgent task.Petroleum resources are faced with exhausted crisis, and other new forms of energy such as hydrogen energy source, wind energy, sun power, the equidistant large-scale industrial production of nuclear energy and civilian a segment distance arranged still.Therefore, performance will most possibly become substitute energy in a short time near the biofuel of petroleum resources.Biofuel generally is meant methyl esters, ethyl ester or the higher alcohol ester of animal-plant oil through over-churning or transesterify generation, and its structure and combustionproperty and diesel oil are suitable, are typical case'ss " green regenerative energy sources ".Compare with other energy, biofuel more closing to reality is used, and more can solve practical problems in a short time.
Patent CN101050374 discloses a kind of method of preparing biologic diesel oil from cottonseeds directly.This method is raw material with the cottonseed, through peel off, give birth to embryo expanded after, adopting ethanol and methyl alcohol mixed liquor is that solvent leaches gossypol, hair cotton oil in leacher, obtains the wet dregs of rice of removing cotton phenol and solvent hair cotton oil mixed solution; Solvent hair cotton oil mixed solution can directly enter reaction kettle of the esterification, adds solid catalyst, and reaction makes biofuel.Sevil
Investigated the influence that various factors is produced the fatty acid methyl ester yield to former bit esterified Rice pollard oil Deng the people.They are with 50g rice bran and methanol mixed, and the adding vitriol oil is done the catalyst esterification and produced methyl esters.Investigated the influence of original position esterification time, temperature, catalyst levels, rice bran moisture and methanol usage.They find, using the high rice bran of free fatty acid content is the effective means that improves the methyl esters productive rate.When the free fatty acid content of Rice pollard oil when 16.6% is elevated to 84.5%, the methyl esters yield has improved 67%.Temperature is when 20 ℃ are elevated to 65 ℃, and the methyl esters yield has improved 30%.But vitriol oil consumption can not increase the ester yield when 5ml is above.Human soybean in-situ preparing such as Michael J.Haas biofuel, they are soybean flakes and NaOH methanol solution hybrid reaction, find can fully improve reaction in efficient after the soybean flakes drying processed.
No matter still external at home, raw material sources are few, the cost height is the subject matter that restricts the biofuel development at present.The cost of stock oil has occupied more than 70% of biofuel cost.Therefore, in order to reduce the cost of biofuel, choosing of raw material is extremely important.Swill oil and useless frying oil are the raw materials of a lot of research units and producer's first-selection, but owing to collect difficulty, can't large-scale industrial production.
China is paddy big producing country, about 200,000,000 tons of paddy annual production, and be more than 1,000 ten thousand tons as the annual production of paddy processing byproduct rice bran, account for 1/3 of Gross World Product.Contain lipid 16～22% in the rice bran stably of conventional husk rice, then contain manyly in the rice bran of parboiled rice husk rice, be about 25～32%.Contain 15～20% saturated fatty acid and 80～85% unsaturated fatty acids in the Rice pollard oil, wherein contain palmitinic acid 13～18%, oleic acid 40～50%, linolic acid 26～35% is the good raw material of preparation biofuel.With rice bran is the feedstock production biofuel, make full use of originally low value-added paddy processing byproduct, land occupation in addition not only, and in the rice bran of degreasing, contain a large amount of nutritive substances and functional component, as have the rice bran protein of hypoallergenic, antitumour activity and nourishing function; Rice bran polysaccharide with antitumor, strengthening immunity and function of blood sugar reduction; And can promote rice bran phytic acid ca that human body metabolism, bone tissue grow etc.
With the rice bran is raw material, original position is carried oil-esterification/preparing biodiesel by ester exchange, to put forward oil and biodiesel manufacture technology unites two into one, shortened the technical process from the rice bran to the biofuel, the required energy consumption of extraction Rice pollard oil is used for synchronously the production of biofuel, save energy reduces the production cost of biofuel greatly, makes biofuel have the stronger market competitiveness.
Summary of the invention
Its purpose of the present invention is to provide a kind of novel method of preparing biodiesel by in situ extraction of rice oil.This method is applicable to that other oil crops original positions carry oil and produce biofuel.
The technical scheme of being taked comprises for achieving the above object: original position is put forward oil-acid catalyzed esterification, is dewatered synchronously, the transition of soda acid system, base-catalyzed transesterification and product separation and purification etc.Concrete steps are as follows:
In reactor, add alcohol (or mixture of alcohol and solvent) and acid catalyst in proportion, in extractor, add rice bran, in the alkali jar, add water-removal agent and alkaline catalysts.The acid catalyst consumption is 1～2% of a rice bran quality, the alkaline catalysts consumption is 1.2～3.0% of a rice bran quality, the volume ratio of alcohol and solvent is 1～2:1, and the solid-liquid mass ratio of rice bran and alcohol (or alcohol/solvent) is 1:3～4, and the mass ratio of water-removal agent and rice bran is 3～4:10.Open valve 2-1 and 2-2, reflux is extracted Rice pollard oil, and the original position esterified fatty acid.After 1～5 hour, Open valve 5-1 and 5-2, valve-off 2-1 and 2-2 simultaneously, back flow reaction 3～5 hours, alkaline catalysts is all dissolved in the reactor gradually, and system progressively carries out the transition to the alkali environment by acid environment, and in this process, dewater, esterification more completely and transesterification reaction.After reaction finishes, reclaim alcohol/solvent, hot water drip washing product gets product behind collection, the dry oil reservoir.Further purification can be distilled product under reduced pressure, collects the cut of 140～230 ℃ of 0.098MPa.
Compare with existing technology, this technology has following advantage:
1. with the rice bran raw material, original position is carried oil-esterification/preparing biodiesel by ester exchange, to put forward oil and biodiesel manufacture technology unites two into one, shortened the technical process from the rice bran to the biofuel, energy efficient, can reduce the production cost of biofuel greatly, make biofuel have the stronger market competitiveness.
2. remove existing acid-alkali two-step process and prepared the middle loaded down with trivial details raw material treating processes of biofuel.In reaction process, along with the backflow of alcohol and solvent, alkaline catalysts is dissolved in reaction system gradually, and the realization system is by the progressively transition of acid to alkali, thereby avoids that local alkali-generation water concentration is excessive may to cause the saponified problem.Before the system transition alkalize, dewater and further esterification carry out simultaneously.By dewatering synchronously and soda acid these two gordian techniquies of transition progressively, can reduce intermediate treatment cost and waste water.
3. low to raw material rice bran specification of quality, need not rice bran is carried out Passivation Treatment, device can be handled the oilseed acid value scope from 0 to 160mgKOH/g, even higher.
Description of drawings
Fig. 1 is apparatus of the present invention synoptic diagram.
Among the figure:
1,10---prolong;
2---extractor;
3---reactor;
4---reaction liquid phase (the rice bran wet goods that contains alcohol, solvent, catalyzer and extract);
5---the alkali jar;
6---the water-removal agent filter screen;
7---the alkaline catalysts filter screen;
8---alkaline catalysts;
9---water-removal agent;
11---agitator (, need not to open) at single_phase system according to the system difference;
12---rice bran;
2-1,2-2,5-1,5-2---valve.
Embodiment
Below in conjunction with accompanying drawing and example the present invention is described in further detail.
Embodiment 1:
Adding 50kg Rice pollard oil fatty acid content is 34% rice bran in extractor, adds the 200L dehydrated alcohol and 0.5kg 98% vitriol oil in reactor, adds 0.61kg NaOH catalyzer and 17kg CaO water-removal agent in the alkali jar.Open valve 2-1 and 2-2, reacting by heating still, back flow reaction 5h; Valve-off 2-1 and 2-2, Open valve 5-1 and 5-2, back flow reaction 3.5h; Reaction finishes.Reclaim ethanol, hot water drip washing product is collected oil reservoir, the dry product that gets.Product yellow, clarification, transparent, esterification yield are more than 99%, and ester exchange rate can reach more than 85%.Further purification can be distilled product under reduced pressure, collects the cut of 140～230 ℃ of 0.098MPa.
Embodiment 2:
Adding 50kg Rice pollard oil fatty acid content is 51% rice bran in extractor, adds the 200L dehydrated alcohol and 0.6kg 98% vitriol oil in reactor, adds 0.89kg KOH catalyzer and 17kg CaO water-removal agent in the alkali jar.Open valve 2-1 and 2-2, reacting by heating still, back flow reaction 5h; Valve-off 2-1 and 2-2, Open valve 5-1 and 5-2, back flow reaction 3.5h; Reaction finishes, and reclaims ethanol, hot water drip washing product.Collect oil reservoir, the dry product that gets.Product yellow, clarification, transparent, esterification yield are more than 99%, and ester exchange rate can reach more than 85%.
Embodiment 3:
Adding 50kg Rice pollard oil fatty acid content is 69% rice bran in extractor, adds the 200L dehydrated alcohol and 0.7kg 98% vitriol oil in reactor, adds 0.85kg NaOH catalyzer and 17kg CaO water-removal agent in the alkali jar.Open valve 2-1 and 2-2, reacting by heating still, back flow reaction 5h; Valve-off 2-1 and 2-2, Open valve 5-1 and 5-2, back flow reaction 3.5h; Reaction finishes, and reclaims ethanol, hot water drip washing product.Collect oil reservoir, the dry product that gets.Product yellow, clarification, transparent, esterification yield are more than 99%, and ester exchange rate can reach more than 85%.
Embodiment 4:
Adding 50kg Rice pollard oil fatty acid content is 77% rice bran in extractor, adds the 200L dehydrated alcohol and the 0.8kg98% vitriol oil in reactor, adds 1.11kg KOH catalyzer and 17kg CaO water-removal agent in the alkali jar.Open valve 2-1 and 2-2, reacting by heating still back flow reaction 5h; Valve-off 2-1 and 2-2, Open valve 5-1 and 5-2, back flow reaction 3.5h; Reaction finishes, and reclaims ethanol, hot water drip washing product.Collect oil reservoir, the dry product that gets.Product yellow, clarification, transparent, esterification yield are more than 99%, and ester exchange rate can reach more than 85%.
Embodiment 5:
Adding 50kg Rice pollard oil fatty acid content is 34% rice bran in extractor, in reactor, add 120L dehydrated alcohol, 80L sherwood oil (30～60 ℃) and 0.5kg 98% vitriol oil, in the alkali jar, add 0.61kg NaOH catalyzer and 17kg CaO water-removal agent.Open valve 2-1 and 2-2, reacting by heating still, back flow reaction 2h; Valve-off 2-1 and 2-2, Open valve 5-1 and 5-2, back flow reaction 3.5h; Reaction finishes, and reclaims alcohol/solvent, hot water drip washing product.Collect oil reservoir, dry, after desolventizing product.Product is golden yellow, clarification, transparent, and esterification yield is more than 99%, and ester exchange rate can reach more than 85%.
Embodiment 6:
Adding 50kg Rice pollard oil fatty acid content is 51% rice bran in extractor, in reactor, add 120L dehydrated alcohol, 80L sherwood oil (30～60 ℃) and 0.6kg 98% vitriol oil, in the alkali jar, add 0.89kg KOH catalyzer and 17kg CaO water-removal agent.Open valve 2-1 and 2-2, reacting by heating still, back flow reaction 2h; Valve-off 2-1 and 2-2, Open valve 5-1 and 5-2, back flow reaction 3.5h; Reaction finishes, and reclaims alcohol/solvent, hot water drip washing product.Collect oil reservoir, dry, after desolventizing product.Product is golden yellow, clarification, transparent, and esterification yield is more than 99%, and ester exchange rate can reach more than 85%.
Embodiment 7:
Adding 50kg Rice pollard oil fatty acid content is 69% rice bran in extractor, in reactor, add 120L dehydrated alcohol, 80L sherwood oil (30～60 ℃) and 0.7kg 98% vitriol oil, in the alkali jar, add 0.85kg NaOH catalyzer and 17kg CaO water-removal agent.Open valve 2-1 and 2-2, reacting by heating still, back flow reaction 2h; Valve-off 2-1 and 2-2, Open valve 5-1 and 5-2, back flow reaction 3.5h; Reaction finishes, and reclaims alcohol/solvent, hot water drip washing product.Collect oil reservoir, dry, after desolventizing product.Product is golden yellow, clarification, transparent, and esterification yield is more than 99%, and ester exchange rate can reach more than 85%.
Embodiment 8:
Adding 50kg Rice pollard oil fatty acid content is 77% rice bran in extractor, in reactor, add 120L dehydrated alcohol, 80L sherwood oil (30～60 ℃) and 0.8kg 98% vitriol oil, in the alkali jar, add 1.11kg KOH catalyzer and 17kg CaO water-removal agent.Open valve 2-1 and 2-2, reacting by heating still, back flow reaction 2h; Valve-off 2-1 and 2-2, Open valve 5-1 and 5-2, back flow reaction 3.5h; Reaction finishes, and reclaims alcohol/solvent, hot water drip washing product.Collect oil reservoir, dry, after desolventizing product.Product is golden yellow, clarification, transparent, and esterification yield is more than 99%, and ester exchange rate can reach more than 85%.
Embodiment 9:
Adding 50kg Rice pollard oil fatty acid content is 34% rice bran in extractor, in reactor, add 120L anhydrous methanol, 80L sherwood oil (30～60 ℃) and 0.5kg 98% vitriol oil, in the alkali jar, add 0.61kg NaOH catalyzer and 17kg CaO water-removal agent.Open valve 2-1 and 2-2 start stirring, reacting by heating still, back flow reaction 2h; Valve-off 2-1 and 2-2, Open valve 5-1 and 5-2, back flow reaction 3.5h; Reaction finishes, and reclaims alcohol/solvent, hot water drip washing product.Collect oil reservoir, dry, after desolventizing product.Product is golden yellow, clarification, transparent, and esterification yield is more than 99%, and ester exchange rate can reach more than 85%.
Embodiment 10:
Adding 50kg Rice pollard oil fatty acid content is 51% rice bran in extractor, in reactor, add 120L anhydrous methanol, 80L sherwood oil (30～60 ℃) and 0.6kg 98% vitriol oil, in the alkali jar, add 0.89kg KOH catalyzer and 17kg CaO water-removal agent.Open valve 2-1 and 2-2 start stirring, reacting by heating still, back flow reaction 2h; Valve-off 2-1 and 2-2, Open valve 5-1 and 5-2, back flow reaction 3.5h; Reaction finishes, and reclaims alcohol/solvent, hot water drip washing product.Collect oil reservoir, dry, after desolventizing product.Product is golden yellow, clarification, transparent, and esterification yield is more than 99%, and ester exchange rate can reach more than 85%.
Claims (4)
1. the novel method of a preparing biodiesel by in situ extraction of rice oil, its concrete steps are as follows: add alcohol (or mixture of alcohol and solvent) and acid catalyst in proportion in reactor, add rice bran in extractor, adding water-removal agent and alkaline catalysts in the alkali jar.Open valve 2-1 and 2-2, reflux is extracted Rice pollard oil, and the original position esterified fatty acid, after 1～5 hour, valve-off 2-1 and 2-2, while Open valve 5-1 and 5-2, back flow reaction 3～5 hours; After reaction finishes, reclaim alcohol/solvent, hot water drip washing product gets product behind collection, the dry oil reservoir.Further purification can be distilled product under reduced pressure, collects the cut of 140～230 ℃ of 0.098 Mpa.
2. according to the novel method of the described a kind of preparing biodiesel by in situ extraction of rice oil of claim 1, it is characterized in that: used alcohol is dehydrated alcohol or anhydrous methanol, solvent for use is 30～60 ℃ of sherwood oils, used acid catalyst is 98% vitriol oil, used water-removal agent is CaO, and used alkaline catalysts is NaOH or KOH.
3. according to the novel method of the described a kind of preparing biodiesel by in situ extraction of rice oil of claim 1, it is characterized in that: the acid catalyst consumption is 1～2% of a rice bran quality; The alkaline catalysts consumption is on the basis of neutralizing acid catalyzer, and excessive part is 0.2～0.6% of a rice bran quality; The volume ratio of alcohol and solvent is 1～2:1; The solid-liquid mass ratio of rice bran and alcohol (or alcohol/solvent) is 1:3～4; The mass ratio of water-removal agent and rice bran is 3～4:10.
4. according to the novel method of the described a kind of preparing biodiesel by in situ extraction of rice oil of claim 1, it is characterized in that: behind Open valve 5-1 and the 5-2, along with the backflow of alcohol and solvent, alkaline catalysts dissolves in reaction system gradually, the realization system by acid to progressively transition of alkali.
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| CNA2008100513806A CN101392181A (en) | 2008-11-04 | 2008-11-04 | Novel method for preparing biodiesel by in situ extraction of rice oil |
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| CNA2008100513806A CN101392181A (en) | 2008-11-04 | 2008-11-04 | Novel method for preparing biodiesel by in situ extraction of rice oil |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102492561A (en) * | 2011-12-23 | 2012-06-13 | 吉林大学 | Method for preparing bio-diesel by using fresh rice bran |
| CN104450208A (en) * | 2014-11-11 | 2015-03-25 | 西北农林科技大学 | Method for preparing biodiesel by virtue of Soxhlet extraction device |
| CN105886128A (en) * | 2016-04-20 | 2016-08-24 | 吉林大学 | Method for producing pesticide green solvent from rice bran oil |
| CN109852483A (en) * | 2018-12-29 | 2019-06-07 | 中南林业科技大学 | A method of fatty acid methyl ester is prepared with Rice bran crude oil |
-
2008
- 2008-11-04 CN CNA2008100513806A patent/CN101392181A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102492561A (en) * | 2011-12-23 | 2012-06-13 | 吉林大学 | Method for preparing bio-diesel by using fresh rice bran |
| CN104450208A (en) * | 2014-11-11 | 2015-03-25 | 西北农林科技大学 | Method for preparing biodiesel by virtue of Soxhlet extraction device |
| CN105886128A (en) * | 2016-04-20 | 2016-08-24 | 吉林大学 | Method for producing pesticide green solvent from rice bran oil |
| CN109852483A (en) * | 2018-12-29 | 2019-06-07 | 中南林业科技大学 | A method of fatty acid methyl ester is prepared with Rice bran crude oil |
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Application publication date: 20090325 |