CN101338213A - Biodesel and method for preparing same - Google Patents
Biodesel and method for preparing same Download PDFInfo
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- CN101338213A CN101338213A CNA2007101439891A CN200710143989A CN101338213A CN 101338213 A CN101338213 A CN 101338213A CN A2007101439891 A CNA2007101439891 A CN A2007101439891A CN 200710143989 A CN200710143989 A CN 200710143989A CN 101338213 A CN101338213 A CN 101338213A
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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
Abstract
The invention relates to bio-based diesel oil and a preparation method thereof. The biological diesel oil comprises the components with the weight percentage of 3-10 percent of mixed ester of methyl, ethyl and butyl, 2-5 percent of butanol and isobutanol, 0.1-0.3 percent of carbonate rare earth lanthanum cerium polyol oleate copolymer, and the rest is C<12-14> alkane and C<12-14> isoparaffin. The preparation method is divided into two steps: biological oil which is prepared through rapid middle temperature thermal cracking and plant grease with 35-40 percent of the C more than or equal to 18 fatty acid content are used as raw materials, and high pressure hydrofing cracking and all formulation screening process are used for the preparation. The prepared bio-based diesel oil has the advantages of high thermal value, high cleanness, low freezing point and good stability, can be used as both the necessary component of highly clean diesel oil and a novel environmental protection solvent and can completely substitute present various diesel oil fuels.
Description
One, technical field:
The present invention relates to a kind of bio-based diesel oil and preparation method thereof, the field of biodiesel oil that belongs to bioenergy in the biomass engineering, particularly relate to a kind ofly utilize that bio oil and all kinds of animal-plant oil are refining with high-pressure hydrogenation, product and technology of preparing thereof that cracking and full formula screening technology prepare high-performance bio-based diesel oil.
Two, background technology:
Biofuel is meant the fatty acid methyl ester class I liquid I fuel of producing for raw material with oil crops, oil-yielding shrubs fruit, oil plant waterplant etc.Complete processing is mainly ester-interchange method at present, its product chemical composition is a fatty acid methyl ester, the main defective that this class process products exists is that calorific value is lower, the discharging nitride does not reduce, be used for diesel motor, exist engine power to descend (5%～12%), package stability is poor, NO in the exhaust emissions
XIncrease.So generally can only be on a small quantity (5%～20%, now external threshold limit value is 5%), mix the back mutually with petroleum diesel and use as motor vehicle fuel.
High-performance bio-based diesel oil is meant that with bio oil and animal-plant oil be raw material, and with the high-cleanness diesel oil fuel of high-pressure hydrogenation, refining, cracking and the preparation of full formula screening technology, its chemical composition is C
12～14Alkane and isoparaffin, fatty acid mixed ester (methyl esters, ethyl ester and butyl ester), butanols and isobutyl alcohols material, its incendivity, emission performance, low temperature properties, stability in storage are significantly higher than the fatty acid methyl ester biofuel, are applicable to that diesel motors such as heavy truck, military armored vehicle use.
High-performance bio-based diesel product meets all requirements of EN590 and WWEC-4, is to be used for the total high-quality bio-based component of forming of ULSD (Britain's ultra-low-sulphur diesel).
The production of biofuel at present, domestic have only the fatty acid methyl esters product, and do not have C
12～14The alkanes product, hydrogenolysis is also adopted in the production of petroleum diesel, but its raw material, catalyzer and control condition all are not inconsistent with this technology.
Three, summary of the invention:
The purpose of this invention is to provide a kind of is raw material with bio oil and all kinds of animal-plant oil, by refining, cracking process, preparation calorific value height, abrasive, lowly coagulate, good stability, can be used as the indispensable component of high-cleanness diesel oil, also can be used as the novel environment friendly solvent, can substitute the bio-based diesel oil and the technology of preparation method thereof of existing various diesel oil fuels fully.
The objective of the invention is to realize by following mode:
The composition of bio-based diesel oil of the present invention is by mass percentage: fatty acid methyl, second, fourth mixed ester 3～10%, and butanols and isopropylcarbinol 2～5%, carbonate Rare Earth Lanthanum cerium polyvalent alcohol oleic acid ester multipolymer 0.1～0.3%, all the other are C
12～14Alkane and C
12～ 14Isoparaffin.
The preparation of bio-based diesel oil of the present invention is to be raw material with bio oil or all kinds of animal-plant oil, and concrete processing step is as follows:
(1) raw materials pretreatment: bio oil and C that thermo-cracking is made
〉=18Fatty acid content filters through supercharging at 35～40at% plant quasi-grease, and supercharging pressure is in 0.8～1.0MPa, processed, and (colloid, resin, unsaponifiables and inorganics enter behind the surge tank to injection pump to remove solid impurity;
(2) new hydrogen supercharging: hydrogen is fed separating tank, and pressure 1.0～1.2MPa removes the middle moisture that degass, and makes water-content≤0.5 μ g/g enter three sections reciprocation compressors then;
(3) hydrogenation reaction: adopt the high-pressure hydrocracking method, reactor is fixed-bed reactor, flow process is single hop series connection recycle to extinction hydrocracking, the catalyst for refining that adopts is " base metal nickel is component+molecular sieve+Rare Earth Lanthanum, cerium ", and the cracking catalyst of employing is " base metal copper chromium manganese is component+acidic molecular sieve+Rare Earth Lanthanum, cerium "; In hydrofining reactor, control reaction temperature is 300～320 ℃, pressure 10～13MPa, 3～5 minutes reaction times;
In hydrocracking reactor, control reaction temperature is 320～400 ℃, and total pressure 12～15MPa controls iodine number below 85,13～15 minutes reaction times;
Refining reaction device operating parameters is:
| Condition | Unit | Parameter |
| The hydrogen dividing potential drop | MPa | 10～13 |
| Temperature of reaction | ℃ | 300～320 |
| Air speed | h -1 | 0.8～1.8 |
| Hydrogen to oil volume ratio | 800～1000 |
The cracking case operating parameters is:
| Condition | Unit | Parameter |
| The hydrogen dividing potential drop | MPa | 12～15 |
| Temperature of reaction | ℃ | 320～400 |
| Air speed | h -1 | 0.8～1.8 |
| Hydrogen to oil volume ratio | 1200～1700 |
(4) high pressure separates: mix hydrogen+thermal high separation process scheme after adopting stove, leave standstill extracting with the excess hydrogen in the reaction product, water and other component (C
12～14Alkane and isoparaffin and unreacted oil content) separate;
The reaction product of being come out by reactor enters high-pressure separator through the heat exchange cooling, after being cooled to 160～180 ℃, with the H in the reaction product
2, H
2O and oil ingredient (C
12～14Alkane and isoparaffin and unreacted oil content) separate, isolated gas contains the hydrogen of 90～95v%, and most of as the recycle hydrogen use after the recycle compressor supercharging, small part is removed preprocessing part;
(5) vacuum fractionation: adopt the vacuum fractionation tower, will be dissolved in the C in the oil
≤ 4Light hydrocarbon evaporate, light hydrocarbon directly reclaims incorporates gas ductwork into;
(6) full formula screening: the component that separation column obtains is C
12～14Alkane and C
12～14Isoparaffin is at C
12～14Alkane and C
12～ 14In the isoparaffin, add rare earth high polymer material functional agent (carbonate Rare Earth Lanthanum cerium polyvalent alcohol oleic acid ester multipolymer) 0.1 ~ 0.3at% successively, fatty acid methyl, second, fourth mixed ester 3 ~ 10at%, butanols and isopropylcarbinol 2 ~ 5at%, after mixing, filter, obtain high-performance bio-based diesel oil of the present invention.
The invention has the beneficial effects as follows: with bio oil and all kinds of animal-plant oil is raw material, the catalyst for refining that adopts is " base metal nickel is component+molecular sieve+rare earth (lanthanum cerium) ", the cracking catalyst that adopts is " base metal copper chromium manganese is component+acidic molecular sieve+rare earth (lanthanum cerium) ", finish refining, cracking process, reactor can adopt traditional fixed-bed reactor, has adjusted density and viscosity, oilness, low temperature properties index by full formula screening.Reaction characteristics is first deoxidation, deolefination (comprising saturation of olefins), then cracking, a secondary cracking, take off hysomer, generate C
12～14Positive structure or isoparaffin, bio-based diesel oil is prepared in last desulfurization, decolouring, deodorization, the bio-based diesel oil calorific value height, abrasive of preparation, lowly coagulate, good stability, can be used as the indispensable component of high-cleanness diesel oil, also can be used as the novel environment friendly solvent, can substitute existing various diesel oil fuels fully, performance all reaches international EN590 standard, and the index contrast is as follows:
| Project | Unit | Bio-based diesel oil | EN590 diesel oil | Test method |
| Cetane value 〉= | 90 | 58 | GB/T386 | |
| Cetane index 〉= | 70 | 46 | ||
| Density | g·cm -3 | 0.825～0.835 | 0.820～0.835 | GB/T1884 |
| The condensed-nuclei aromatics massfraction≤ | ％ | Do not have | 1 | |
| T 95 ≤ | ℃ | 330 | 340 | |
| Sulphur content≤ | g/g | 10 | 50(10) | GB/T380 |
| Oilness (HFRR60 ℃)≤ | 450 | 460 | ||
| Emission standard 〉= | V | IV | ||
| Flash-point (remaining silent) 〉= | ℃ | 90 | 55 | GB/T261 |
| Condensation point≤ | ℃ | -35 | -30 | GB/T510 |
| Calorific value 〉= | MJ/kg | 49.3 | 43 | GB/T384 |
| Kinematic viscosity (40 ℃) | mm 2·s -1 | 3～4 | 2～4.5 | GB/T265 |
| Oxidation stability (110 ℃) 〉= | h | 30 | 25 | EN14112 |
| Copper corrosion (50 ℃, 3h -1) ≥ | Level | 1 | 1 | GB/T5096 |
Four, description of drawings:
Fig. 1 is that bio oil and animal-plant oil single hop series connection recycle to extinction thermal high separate system novel high-performance bio-based diesel oil process flow sheet.
Five, embodiment:
As starting material, prepare bio-based diesel oil (process flow sheet as shown in Figure 1) with the mountain peach kernel oil.Concrete processing step is as follows:
(1) raw materials pretreatment: mountain peach kernel oil oil is after the oil pump supercharging, with 14m
3/ h flow enters strainer, removes solid impurity after filtration, then through the hot processed of water knockout, removes excessive moisture in the degrease, enters behind the surge tank to injection pump.Make water-content≤50 μ g/g.Entering-anti-refining section before, oil plant and the feed liquid heat exchange of coming out, and be heated to through process furnace and specify the feed liquor temperature from separator.
(2) new hydrogen supercharging: with hydrogen (99.99%) with 2500m
3/ h gas speed feeds separating tank, removes the middle drop that degass, and enters three sections reciprocation compressors then.After supercharging, new hydrogen pressure can arrive 1.0MPa.Entering-anti-refining section before, new hydrogen with mix warp and the feed liquid heat exchange that goes out reactor, and through being heated to the appointment inlet air temperature from the isolated recycle hydrogen of high-pressure separator.
(3) hydrogenation reaction: the oil plant after pretreated, through volume pump with 30m
3/ h flow enters the refining section of single hop series connection recycle to extinction reactor from an anti-top, inlet pressure remains on 0.25MPa, and temperature is about 190 ℃.Reactor is fixed-bed reactor, the catalyst for refining that adopts is " non-heavy metal nickel is component+molecular sieve+rare earth (lanthanum cerium) ", oil plant with enter catalytic bed after hydrogen mixes and react, temperature of reaction is 310 ℃, pressure 12MPa, the oil plant air speed remains on 1.0h
-1, the saturated and hydrogenolysis by hydrogenation, portion C
18Hydrogenation of olefins is saturated, removes the oxygen-bearing organic matter component, generates water.4 minutes reaction times.
Treat that refining reaction is complete, reaction product is from counter come out, after heat exchange, cooling, enter two anti-cracking zone reactors rapidly, with enter catalytic bed after hydrogen mixes and react, the cracking catalyst of employing is " non-heavy metal copper chromium manganese is component+acidic molecular sieve+rare earth (lanthanum cerium) ", temperature of reaction is 360 ℃, total pressure 13MPa, the oil plant air speed remains on 1.2h
-1, in cracking case, the C of macromolecular chain
18Alkane etc. are cracked into C through hydroisomerization and ring-opening reaction
12～14Alkane and isoparaffin are failed cracking or rearrange alkane or other components of purpose product simultaneously, and through the directed desired alkane that generates of reforming, unsaturated fully and fracture component generates required finished product via hydrogenation catalyst.Reaction must be controlled iodine value below 85,13 minutes reaction times.
(4) high pressure separates: the reaction product of being come out by reactor comprises lighter hydrocarbons, unreacting hydrogen, oil plant, water, after interchanger cooling cooling, enter high-pressure separator, reactant carries out gas-liquid separation in this at 270 ℃, leaves standstill extracting with the H in the reaction product by high pressure
2, H
2O separates with oil ingredient.Hot high score bottom feed liquid is directly sent to fractionation, and components such as the isolated lighter hydrocarbons in hot high score top, hydrogen enter cold high score through cooling, under 50 ℃ of working temperatures, lighter hydrocarbons, hydrogen and lighting end is separated.Contain the hydrogen of 90～95v% at isolated gas, most ofly after the recycle compressor supercharging use as recycle hydrogen, small part is removed preprocessing part.
(5) vacuum fractionation: hot high score bottom feed liquid enters the vacuum fractionation tower with 320 ℃ of temperature ins, and the control tower top pressure is 48mmHg, 130 ℃ of tower top temperatures, 250 ℃ of column bottom temperatures.The employing vacuum fractionation will be dissolved in the light hydrocarbon (C in the oil
≤ 4) evaporate, lighter hydrocarbons directly reclaim incorporates gas ductwork into.Product is extracted section out and is flowed out the purpose product down for 170 ℃ in temperature, is under the 80mmHg at interior steaming section pressure, and the part gas phase obtains liquefied synthetic gas at this through flash of steam.
(6) full formula screening: the component that separation column obtains is C
12～14Alkane and isoparaffin are at C
12～14In alkane and the isoparaffin, add rare earth high polymer material functional agent (carbonate Rare Earth Lanthanum cerium polyvalent alcohol oleic acid ester multipolymer) 0.2at% successively, fatty acid methyl, second, fourth mixed ester 5at%, butanols and isopropylcarbinol 3at%, temperature is controlled at 55 ℃, mixing 10min filters through filter after treating evenly, obtains novel high-performance bio-based diesel oil.
The quality index of prepared high-performance bio-synthetic diesel product is as follows:
| Project | Unit | Quality index | Test method |
| 20 ℃ of density | g·cm -3 | 0.830 | GB/T1884 |
| 40 ℃ of kinematic viscosity | mm 2·s -1 | 3.5 | GB/T265 |
| Cold filter clogging temperature | ℃ | -50 | SH/T0248 |
| Condensation point | ℃ | -39 | GB/T510 |
| Flash-point (remaining silent) | ℃ | 110℃ | 6B/T261 |
| Cetane value | 93 | GB/T386 | |
| Cetane index | 76 | ||
| Acid number | mgKOH/g | 0.56 | GB/T264 |
| Free glycerol content | ％ | 0.010 | ASTMD6584 |
| Total glycerol content | ％ | 0.140 | ASTMD6584 |
| Sulphur content | ％ | 0.001 | GB/T380 |
| Calorific value | MJ/kg | 51.3 | GB/T384 |
Claims (2)
1, a kind of bio-based diesel oil, it is characterized in that: the composition of bio-based diesel oil is by mass percentage: fatty acid methyl, second, fourth mixed ester 3～10%, butanols and isopropylcarbinol 2～5%, carbonate Rare Earth Lanthanum cerium polyvalent alcohol oleic acid ester multipolymer 0.1～0.3%, all the other are C
12～14Alkane and C
12～14Isoparaffin.
2, the preparation method of bio-based diesel oil according to claim 1 is characterized in that: the preparation of bio-based diesel oil of the present invention is to be raw material with bio oil or all kinds of animal-plant oil, and concrete processing step is as follows:
(1) raw materials pretreatment: bio oil and C that thermo-cracking is made
〉=18Fatty acid content filters through supercharging at 35～40at% plant quasi-grease, and supercharging pressure is in 0.8～1.0MPa, processed, and (colloid, resin, unsaponifiables and inorganics enter behind the surge tank to injection pump to remove solid impurity;
(2) new hydrogen supercharging: hydrogen is fed separating tank, and pressure 1.0～1.2MPa removes the middle moisture that degass, and makes water-content≤0.5 μ g/g enter three sections reciprocation compressors then;
(3) hydrogenation reaction: adopt the high-pressure hydrocracking method, reactor is fixed-bed reactor, flow process is single hop series connection recycle to extinction hydrocracking, the catalyst for refining that adopts is " base metal nickel is component+molecular sieve+Rare Earth Lanthanum, cerium ", and the cracking catalyst of employing is " base metal copper chromium manganese is component+acidic molecular sieve+Rare Earth Lanthanum, cerium "; In hydrofining reactor, control reaction temperature is 300～320 ℃, pressure 10～13MP
a, 3～5 minutes reaction times;
In hydrocracking reactor, control reaction temperature is 320～400 ℃, total pressure 12～15MP
a, control iodine number below 85,13～15 minutes reaction times;
Refining reaction device operating parameters is:
The cracking case operating parameters is:
(4) high pressure separates: mix hydrogen+thermal high separation process scheme after adopting stove, leave standstill extracting the excess hydrogen in the reaction product, water are separated with other component;
The reaction product of being come out by reactor enters high-pressure separator through the heat exchange cooling, after being cooled to 160～180 ℃, with the H in the reaction product
2, H
2O separates with oil ingredient, and isolated gas contains the hydrogen of 90～95v%, and most of as the recycle hydrogen use after the recycle compressor supercharging, small part is removed preprocessing part;
(5) vacuum fractionation: adopt the vacuum fractionation tower, will be dissolved in the C in the oil
≤ 4Light hydrocarbon evaporate, light hydrocarbon directly reclaims incorporates gas ductwork into;
(6) full formula screening: the component that separation column obtains is C
12～14Alkane and C
12～14Isoparaffin is at C
12～14Alkane and C
12～ 14In the isoparaffin, add rare earth high polymer material functional agent carbonate Rare Earth Lanthanum cerium polyvalent alcohol oleic acid ester multipolymer 0.1 ~ 0.3at% successively, fatty acid methyl, second, fourth mixed ester 3 ~ 10at%, butanols and isopropylcarbinol 2 ~ 5at%, after mixing, filter, obtain high-performance bio-based diesel oil of the present invention.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007101439891A CN101338213A (en) | 2007-08-17 | 2007-08-17 | Biodesel and method for preparing same |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2007101439891A CN101338213A (en) | 2007-08-17 | 2007-08-17 | Biodesel and method for preparing same |
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| Publication Number | Publication Date |
|---|---|
| CN101338213A true CN101338213A (en) | 2009-01-07 |
Family
ID=40212385
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNA2007101439891A Pending CN101338213A (en) | 2007-08-17 | 2007-08-17 | Biodesel and method for preparing same |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101831328A (en) * | 2010-05-21 | 2010-09-15 | 张小红 | Green fuel oil and preparation method thereof |
| CN102504866A (en) * | 2011-11-08 | 2012-06-20 | 海南临高化工实业有限公司 | Method for preparing biodiesel by mixing waste edible oil with mineral diesel oil and hydrogenization |
| CN101690474B (en) * | 2009-10-16 | 2013-04-24 | 深圳诺普信农化股份有限公司 | Method for preparing botanical solvent |
| US10563130B2 (en) | 2014-07-17 | 2020-02-18 | Sabic Global Technologies B.V. | Upgrading hydrogen deficient streams using hydrogen donor streams in a hydropyrolysis process |
| CN111944555A (en) * | 2020-08-12 | 2020-11-17 | 中国科学院青岛生物能源与过程研究所 | Homogeneous hydrogenation process for producing biodiesel from biomass oil |
| CN113337310A (en) * | 2021-06-29 | 2021-09-03 | 海南盈科生物科技有限公司 | Method for preparing biodiesel by deep processing of biomass residual oil |
-
2007
- 2007-08-17 CN CNA2007101439891A patent/CN101338213A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101690474B (en) * | 2009-10-16 | 2013-04-24 | 深圳诺普信农化股份有限公司 | Method for preparing botanical solvent |
| CN101831328A (en) * | 2010-05-21 | 2010-09-15 | 张小红 | Green fuel oil and preparation method thereof |
| CN102504866A (en) * | 2011-11-08 | 2012-06-20 | 海南临高化工实业有限公司 | Method for preparing biodiesel by mixing waste edible oil with mineral diesel oil and hydrogenization |
| CN102504866B (en) * | 2011-11-08 | 2013-11-27 | 海南环宇新能源有限公司 | Method for preparing biodiesel by mixing waste edible oil with mineral diesel oil through hydrogenization |
| US10563130B2 (en) | 2014-07-17 | 2020-02-18 | Sabic Global Technologies B.V. | Upgrading hydrogen deficient streams using hydrogen donor streams in a hydropyrolysis process |
| CN111944555A (en) * | 2020-08-12 | 2020-11-17 | 中国科学院青岛生物能源与过程研究所 | Homogeneous hydrogenation process for producing biodiesel from biomass oil |
| CN113337310A (en) * | 2021-06-29 | 2021-09-03 | 海南盈科生物科技有限公司 | Method for preparing biodiesel by deep processing of biomass residual oil |
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Open date: 20090107 |