CN102268280A - Method for preparing hydrocarbon fuel by using microwave assisted catalytic saponin decarboxylation method - Google Patents
Method for preparing hydrocarbon fuel by using microwave assisted catalytic saponin decarboxylation method Download PDFInfo
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- CN102268280A CN102268280A CN2011101913189A CN201110191318A CN102268280A CN 102268280 A CN102268280 A CN 102268280A CN 2011101913189 A CN2011101913189 A CN 2011101913189A CN 201110191318 A CN201110191318 A CN 201110191318A CN 102268280 A CN102268280 A CN 102268280A
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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
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- 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 method for preparing a hydrocarbon fuel by using a microwave assisted catalytic saponin decarboxylation method. The method comprises the following steps of: (1) adding 95 percent ethanol in an amount which is 0.1-1.5 times that of grease and 30 percent caustic soda liquor in an amount which is 0.5-0.7 time that of the grease into the grease and saponifying at the temperature of 40-100 DEG C; (2) after saponification is finished, recovering ethanol at reduced pressure, and drying fatty acid salt at reduced pressure for later use; (3) adding a proper amount of 40 percent phosphoric acid into mixed residual liquid of glycerol and residual alkali in the step (2) with stirring to adjust the pH value to 7-8, reacting at a constant temperature and centrifuging, wherein the mixture of glycerol and ethanol on the middle layer is used for refining the glycerol and recovering the ethanol, the lower layer is phosphate which is collected as a fertilizer; and (4) conveying the fatty salt acid into a microwave cracking reactor to crack and decarboxylate, and collecting a gas-state product, a liquid-state product and residual solid-state products. The method has the advantages that: (1) the advantage of high-efficiency selective heating of microwave radiation on dipole molecules and polar functional groups thereof is fully utilized, so that selective decarboxylation and hydrocarbon generation of saponin are realized; (2) the grease raw material is saponified, so that the polarity of the raw material is improved and most of glycerol is recovered; and (3) a liquid-state product in a cracking product can reach about 70 percent, comprises various hydrocarbons serving as main components and is rectified to obtain fuels and chemicals such as naphtha, gasoline, kerosene, diesel oil, lubricating oil and the like in the ratio of 1:7:10:2:1. The hydrocarbon fuel has better oxidation stability and lower solidifying point than biodiesel.
Description
Technical field
The present invention relates to the method that a kind of decarboxylation legal system is equipped with hydrocarbon fuel, relate in particular to the method that a kind of micro ware auxiliary catalysis soap class decarboxylation legal system is equipped with hydrocarbon fuel.
Background technology
After entering 21 century, sharply expand to the consumption of oil in the whole world, and energy dilemma is existing frequently, and Greenhouse effect are serious.Fossil energies such as coal of containing on the earth that develops and oil will be respectively 200 years and 40 years with interior exhaustion, Sweet natural gas also can only be with 60 years by reserve-production ratio.Therefore, the energy shortage problem will perplex development of human society for a long time, develops reproducible, environmental protection, substituting green fuel has become one of human important topic of 21 century.
Biomass-based fuel (Biofuels) has advantages such as environmental protection, additional oil supply breach, thereby more and more receives publicity.Modal fatty acid mono is stearic acid, palmitinic acid, oleic acid, linoleic acid plus linolenic acid in the triglyceride level in animal or plant source, because of it contains higher biomass energy, once directly is used as diesel-fuel, but viscosity is big, low-temperature fluidity is poor.Therefore people have researched and developed the method for the fatty acid methyl ester (biofuel) of vegetables oil alcoholysis preparation.Biofuel sulfur-bearing, nitrogen content are lower.But contain 13% combined oxygen in the fatty acid methyl ester, show as that viscosity is big, low-temperature fluidity is poor, oxidation stability is poor, its energy is equivalent to 88% of No. 2 diesel oil approximately, in order to address these problems, biofuel can only low ratio and petrifaction diesel (by the hydro carbons of carbon atom number between 10～22, comprising that paraffinic hydrocarbons, naphthenic hydrocarbon, alkene, aromatic hydrocarbon constitute) below 20% be mixed and use.Utilize vegetable and animals oils to produce composition and could make the biomass-based fuel of a new generation to dock, and need not existing Infrastructure is done too much change with existing communications and transportation fuel with the similar hydro carbons liquid fuel of petrifaction diesel (biobased hydrocarbon fuel) by the cracking decarboxylation.The lipid acid of grease or fat hydrolysis gained is carried out deoxidation or hydrogenation is possible selection, and product is because oxygen level descends, and oxidation stability improves greatly.
A large amount of evidences show that oil is by algae bio matter experience very long geological age, slowly are transformed under harsh geochemical milieu, and wherein to become hydrocarbon be topmost reaction type to the decarboxylation of ester class.Aspect the mechanism of simulation oil formation, the mankind have attempted the method that multiple oil splitting obtains liquid fuel, all get nowhere.As utilize traditional heating mode cracking triglyceride level etc., and reaction lacks selectivity, the product complexity, and yield is low, is not worth.Even grease is converted into the soap class in the traditional heating mode cracking, though the selectivity of reaction has the reaction product of raising still complicated, the hydro carbons yield is also on the low side, and by product is many, does not possess business development equally and is worth.
Microwave heating not only can be heated selectively to the strong component of mixture Semi-polarity, and the more important thing is, microwave radiation also can realize preferential heating for the polar end of a polarity long chain molecule, and this just provides the important techniques means for the present invention utilizes depleted animal grease or Vegetable oil lipoprotein to transform the biomass-based reproducible hydrocarbon fuel of refining.
Summary of the invention
The purpose of this invention is to provide the method that a kind of micro ware auxiliary catalysis soap class decarboxylation legal system is equipped with hydrocarbon fuel, it is a fatty acid soaps salt with fat saponification at first, and soap salt comes the production hydrocarbon fuel through the mode of microwave-assisted decarboxylation.
The present invention realizes that like this its method steps is:
(1) adding quality in grease is 0.1 ~ 1.5 times 95% ethanol and 0.5～0.7 times 30% white liquor, carries out saponification under 40 ℃～100 ℃ condition, 0.5～3 hour reaction times.
(2) after saponification finished, through the oversalting standing demix, the upper strata was that soap, lower floor are raw glycerine, ethanol and residual alkali mixture, decompression recycling ethanol.The soap on upper strata is separated, decompression recycling ethanol, soap decompression oven dry back is standby.
(3) under agitation add an amount of 40% phosphoric acid in glycerine and the residual alkali mixing raffinate in step (2) and regulate pH to 7 ~ 8, centrifugal after the isothermal reaction, the upper strata is the crude fat hydrochlorate, oven dry back and step (2) gained soap mixing for standby use; Middle level glycerine and alcoholic acid mixture are used for refining glycerine and reclaim ethanol; Lower floor is a phosphoric acid salt, collects as chemical fertilizer.
(4) soap is sent in the microwave cracking reactor, cracking decarboxylation under suitable microwave power, collect gaseous state, liquid state and remaining solid product, three's mass ratio is about 1:7:2, wherein liquid product yield can reach 65%～75%, liquid product can obtain petroleum naphtha, gasoline, kerosene, diesel oil and lubricated wet goods hydrocarbon fuel and chemical through rectifying, and the general proportions of five kinds of compositions is 1:7:10:2:1.
Advantage of the present invention is:(1) the present invention makes full use of the advantage of microwave radiation electrode couple molecule and the heating of polar functional group efficient selective thereof, has realized that the selectivity decarboxylation of soap class becomes hydrocarbon; (2) the present invention has promoted the polarity of raw material with the glyceride stock saponification, has reclaimed most glycerine;
(3) liquid product is up to about 70% in the split product, and main component is various hydro carbons, can obtain petroleum naphtha, gasoline, kerosene, diesel oil and lubricated wet goods hydrocarbon fuel and chemical through rectifying, and its ratio is 1:7:10:2:1.Hydrocarbon fuel is better than oxidation stability of biodiesel, and zero pour is lower.
Embodiment
Embodiment one: 100 kilograms discarded lards, 60 kilogram 30% sodium hydroxide, 10 kilograms 95% ethanol are added reactor, open condensation reflux unit, be heated to 90 ℃, stirring reaction 1.2 h take out cooling and saltout, the upper strata fatty acid sodium salt, separatory takes out lower coarse glycerine alcohol mixture, carries out adding an amount of 40% phosphoric acid after ethanol reclaims, regulate pH to 7.0, the crude fat hydrochlorate that the results secondary is separated out; Nubbin carries out purification of glycerin and phosphoric acid salt is collected utilization.The soap that mixes twice collection behind 50 ℃ of following drying under reduced pressure 12 h, adopts the continuous-type microwave device that the fatty acid sodium salt of gained is carried out the decarboxylation cracking, microwave power is transferred to 3500 W, input speed is 200 g/min, and about 2.5 m of uncondensable gas are collected in the ice bath condensation
3As the fuel generating of gas electricity generator, part is supplied the electric energy of whole microwave system; The product liquid quality of collecting is 68 kilograms, and total yield is 68%, and product liquid obtains 3 kilograms of petroleum naphthas, 21 kilograms in gasoline, 31 kilograms of diesel oil, 7 kilograms of kerosene, 3 kilograms of lubricating oil, 3 kilograms of residual high boiling point waxs through rectifying; About 5 kilograms of solid residue, main component is a yellow soda ash, uses through calcination cycle.
Embodiment two: 100 kilograms discarded butter, 60 kilogram 30% sodium hydroxide, 10 kilograms 95% ethanol are added reactor, open condensation reflux unit, be heated to 90 ℃, stirring reaction 1.2 h take out cooling and saltout, the upper strata fatty acid sodium salt, separatory takes out lower coarse glycerine alcohol mixture, carries out adding an amount of 40% phosphoric acid after ethanol reclaims, regulate pH to 7.5, the soap that the results secondary is separated out; Nubbin carries out purification of glycerin and phosphoric acid salt is collected utilization.The soap that mixes twice collection behind 50 ℃ of following drying under reduced pressure 10 h, adopts the continuous-type microwave device that the fatty acid sodium salt of gained is carried out the decarboxylation cracking, microwave power is transferred to 3500 W, input speed is 200 g/min, and about 2.3 m of uncondensable gas are collected in the ice bath condensation
3As the fuel generating of gas electricity generator, part is supplied the electric energy of whole microwave system; The product liquid quality of collecting is 66 kilograms, and total yield is 66%, and product liquid obtains 4 kilograms of petroleum naphthas, 22 kilograms in gasoline, 29 kilograms of diesel oil, 5 kilograms of kerosene, 3 kilograms of lubricating oil, 3 kilograms of residual high boiling point waxs through rectifying; About 5 kilograms of solid residue, main component is a yellow soda ash, uses through calcination cycle.
Embodiment three: 100 kilograms discarded sheep oil, 60 kilogram 30% sodium hydroxide, 19 kilograms 95% ethanol are added reactor, open condensation reflux unit, be heated to 80 ℃, stirring reaction 1.2h takes out cooling and saltouts, the upper strata fatty acid sodium salt, separatory takes out lower coarse glycerine alcohol mixture, carries out adding an amount of 40% phosphoric acid after ethanol reclaims, regulate pH to 8, the soap that the results secondary is separated out; Nubbin carries out purification of glycerin and phosphoric acid salt is collected utilization.The soap that mixes twice collection behind 50 ℃ of following drying under reduced pressure 15 h, adopts the continuous-type microwave device that the fatty acid sodium salt of gained is carried out the decarboxylation cracking, microwave power is transferred to 3500 W, input speed is 200 g/min, and about 2.4 m of uncondensable gas are collected in the ice bath condensation
3As the fuel generating of gas electricity generator, part is supplied the electric energy of whole microwave system; The product liquid quality of collecting is 61.1 kilograms, and total yield is 62%, and product liquid obtains 2.5 kilograms of petroleum naphthas, 18.1 kilograms in gasoline, 28 kilograms of diesel oil, 7 kilograms of kerosene, 2 kilograms of lubricating oil, 3.5 kilograms of residual high boiling point waxs through rectifying; About 5.9 kilograms of solid residue, main component is a yellow soda ash, uses through calcination cycle.
Embodiment four: 100 kilograms wilson dogwood oil, 50 kilogram 30% potassium hydroxide, 17 kilograms 95% ethanol are added reactor, open condensation reflux unit, be heated to 80 ℃, stirring reaction 1 h takes out cooling and saltouts, upper strata lipid acid sylvite, separatory takes out lower coarse glycerine alcohol mixture, carries out adding an amount of 40% phosphoric acid after ethanol reclaims, regulate pH to 7.8, the lipid acid sylvite that the results secondary is separated out; Nubbin carries out purification of glycerin and phosphoric acid salt is collected utilization.The lipid acid sylvite that mixes twice collection behind decompression drying under reduced pressure 19 h under 50 ℃, adopts the continuous-type microwave device that the lipid acid sylvite of gained is carried out the decarboxylation cracking, microwave power is transferred to 3500W, input speed is 200 g/min, and about 2.0 m of uncondensable gas are collected in the ice bath condensation
3As the fuel generating of gas electricity generator, part is supplied the electric energy of whole microwave system; The product liquid quality of collecting is 69 kilograms, and total yield is 69%, and product liquid obtains 4 kilograms of petroleum naphthas, 22 kilograms in gasoline, 30 kilograms of diesel oil, 8 kilograms of kerosene, 3 kilograms of lubricating oil, 2 kilograms of residual high boiling point waxs through rectifying; About 5 kilograms of solid residue, main component is a salt of wormwood, uses through calcination cycle.
Embodiment five: 100 kilograms algae oil, 50 kilogram 30% sodium hydroxide, 15 kilograms 95% ethanol are added reactor, open condensation reflux unit, be heated to 80 ℃, stirring reaction 1 h takes out cooling and saltouts, the upper strata fatty acid sodium salt, separatory takes out lower coarse glycerine alcohol mixture, carries out adding an amount of 40% phosphoric acid after ethanol reclaims, regulate pH to 7.6, the soap that the results secondary is separated out; Nubbin carries out purification of glycerin and phosphoric acid salt is collected utilization.The soap that mixes twice collection behind 50 ℃ of following drying under reduced pressure 8.5 h, adopts the continuous-type microwave device that the fatty acid sodium salt of gained is carried out the decarboxylation cracking, microwave power is transferred to 3500 W, input speed is 200 g/min, and the about 2.1m of uncondensable gas is collected in the ice bath condensation
3As the fuel generating of gas electricity generator, part is supplied the electric energy of whole microwave system; The product liquid quality of collecting is 67 kilograms, and total yield is 67%, and product liquid obtains 3.5 kilograms of petroleum naphthas, 23 kilograms in gasoline, 30 kilograms of diesel oil, 6 kilograms of kerosene, 2 kilograms of lubricating oil, 2.5 kilograms of residual high boiling point waxs through rectifying; About 5 kilograms of solid residue, main component is a yellow soda ash, uses through calcination cycle.
Embodiment six: 100 kilograms waste cooking oils, 60 kilogram 30% sodium hydroxide, 10 kilograms 95% ethanol are added reactor, open condensation reflux unit, be heated to 90 ℃, stirring reaction 1 h takes out cooling and saltouts, the upper strata fatty acid sodium salt, separatory takes out lower coarse glycerine alcohol mixture, carries out adding an amount of 40% phosphoric acid after ethanol reclaims, regulate pH to 7.5, the soap that the results secondary is separated out; Nubbin carries out purification of glycerin and phosphoric acid salt is collected utilization.The soap that mixes twice collection behind 50 ℃ of following drying under reduced pressure 20 h, adopts the continuous-type microwave device that the fatty acid sodium salt of gained is carried out the decarboxylation cracking, microwave power is transferred to 3500 W, input speed is 200 g/min, and about 2.2 m of uncondensable gas are collected in the ice bath condensation
3As the fuel generating of gas electricity generator, part is supplied the electric energy of whole microwave system; The product liquid quality of collecting is 61 kilograms, and total yield is 61%, and product liquid obtains 2 kilograms of petroleum naphthas, 20.5 kilograms in gasoline, 28 kilograms of diesel oil, 5 kilograms of kerosene, 4 kilograms of lubricating oil, 1.5 kilograms of residual high boiling point waxs through rectifying; About 5 kilograms of solid residue, main component is a yellow soda ash, uses through calcination cycle.
Claims (4)
1. a micro ware auxiliary catalysis soap class decarboxylation legal system is equipped with the method for hydrocarbon fuel, it is characterized in that method steps is:
(1) adding quality in grease is 0.1 ~ 1.5 times 95% ethanol and 0.5～0.7 times 30% white liquor, carries out saponification under 40 ℃～100 ℃ condition, 0.5～3 hour reaction times;
(2) after saponification finished, through the oversalting standing demix, the upper strata was that soap, lower floor are raw glycerine, ethanol and residual alkali mixture, and decompression recycling ethanol is separated the soap on upper strata, decompression recycling ethanol, and soap decompression oven dry back is standby;
(3) under agitation add an amount of 40% phosphoric acid in glycerine and the residual alkali mixing raffinate in step (2) and regulate pH to 7 ~ 8, centrifugal after the isothermal reaction, the upper strata is the crude fat hydrochlorate, oven dry back and step (2) gained soap mixing for standby use; Middle level glycerine and alcoholic acid mixture are used for refining glycerine and reclaim ethanol; Lower floor is a phosphoric acid salt, collects as chemical fertilizer;
(4) soap is sent in the microwave cracking reactor, cracking decarboxylation under suitable microwave power, collect gaseous state, liquid state and remaining solid product, three's mass ratio is about 1:7:2, wherein liquid product yield can reach 65%～75%, liquid product can obtain petroleum naphtha, gasoline, kerosene, diesel oil and lubricated wet goods hydrocarbon fuel and chemical through rectifying, and the general proportions of five kinds of compositions is 1:7:10:2:1.
2. a kind of micro ware auxiliary catalysis soap class decarboxylation legal system according to claim 1 is equipped with the method for hydrocarbon fuel, it is characterized in that described grease comprises: animal oil such as lard, butter, sheep oil; Vegetables oil such as wilson dogwood oil; Microbial oil such as little algae oil, yeast oil; Abendoned oil such as waste cooking oil, acidifying oil.
3. a kind of micro ware auxiliary catalysis soap class decarboxylation legal system according to claim 1 is equipped with the method for hydrocarbon fuel, and 95% ethanol and grease weight ratio used in the described saponification process are 0.1 ~ 1.5:1.
4. a kind of micro ware auxiliary catalysis soap class decarboxylation legal system according to claim 1 is equipped with the method for hydrocarbon fuel, and used alkali is that alkali metal hydroxide is molten in the described saponification process, and used alkali lye and greasy weight ratio are 0.5～0.7:1.
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| CN2011101913189A CN102268280A (en) | 2011-07-08 | 2011-07-08 | Method for preparing hydrocarbon fuel by using microwave assisted catalytic saponin decarboxylation method |
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| CN2011101913189A CN102268280A (en) | 2011-07-08 | 2011-07-08 | Method for preparing hydrocarbon fuel by using microwave assisted catalytic saponin decarboxylation method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105585424A (en) * | 2014-10-24 | 2016-05-18 | 中国石油化工股份有限公司 | Removal method of organic chlorine in by-product glycerol of transesterification reaction of grease |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1915948A (en) * | 2006-08-25 | 2007-02-21 | 暨南大学 | Method for refining glycerol being as byproduct of biology diesel oil |
| CN101457149A (en) * | 2007-12-14 | 2009-06-17 | 周鼎力 | Method for producing gasoline and diesel oil by lipid |
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- 2011-07-08 CN CN2011101913189A patent/CN102268280A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1915948A (en) * | 2006-08-25 | 2007-02-21 | 暨南大学 | Method for refining glycerol being as byproduct of biology diesel oil |
| CN101457149A (en) * | 2007-12-14 | 2009-06-17 | 周鼎力 | Method for producing gasoline and diesel oil by lipid |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105585424A (en) * | 2014-10-24 | 2016-05-18 | 中国石油化工股份有限公司 | Removal method of organic chlorine in by-product glycerol of transesterification reaction of grease |
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Application publication date: 20111207 |