CN107118791A - A kind of method that alkane type biodiesel is prepared by raw material of soap stock - Google Patents
A kind of method that alkane type biodiesel is prepared by raw material of soap stock Download PDFInfo
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- CN107118791A CN107118791A CN201710426037.4A CN201710426037A CN107118791A CN 107118791 A CN107118791 A CN 107118791A CN 201710426037 A CN201710426037 A CN 201710426037A CN 107118791 A CN107118791 A CN 107118791A
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- soap stock
- raw material
- catalyst
- alkane type
- oil
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Classifications
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G3/00—Production of liquid hydrocarbon mixtures from oxygen-containing organic materials, e.g. fatty oils, fatty acids
- C10G3/42—Catalytic treatment
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G3/00—Production of liquid hydrocarbon mixtures from oxygen-containing organic materials, e.g. fatty oils, fatty acids
- C10G3/50—Production of liquid hydrocarbon mixtures from oxygen-containing organic materials, e.g. fatty oils, fatty acids in the presence of hydrogen, hydrogen donors or hydrogen generating compounds
-
- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10G—CRACKING HYDROCARBON OILS; PRODUCTION OF LIQUID HYDROCARBON MIXTURES, e.g. BY DESTRUCTIVE HYDROGENATION, OLIGOMERISATION, POLYMERISATION; RECOVERY OF HYDROCARBON OILS FROM OIL-SHALE, OIL-SAND, OR GASES; REFINING MIXTURES MAINLY CONSISTING OF HYDROCARBONS; REFORMING OF NAPHTHA; MINERAL WAXES
- C10G2300/00—Aspects relating to hydrocarbon processing covered by groups C10G1/00 - C10G99/00
- C10G2300/10—Feedstock materials
- C10G2300/1003—Waste materials
-
- 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
-
- 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
A kind of method that alkane type biodiesel is prepared by raw material of soap stock, soap stock is added in mixture kettle, is stirred continuously the lower acid that adds and is adjusted to lower aqueous solution, acidification oil is obtained after layered dehydration, filtration treatment；The acidification oil, solvent and catalyst of acquisition are separately added into autoclave, hydrogen is passed through, heating and mechanical agitation is opened, after reaction terminates, C is obtained after filtering out catalyst, revolving desolvation14‑C20Liquid alkane mixture, as alkane type biodiesel.The present invention realizes the higher value application of soap stock waste resource, using vegetable oil refining discarded object soap stock as raw material, the raw material for preparing alkane type biodiesel is obtained after acidified pretreatment, open the utilization new way of soap stock, effectively solve waste and the environmental problem of soap stock efficient resource, and effectively alleviate insufficient raw material, the problems such as cost is high.
Description
Technical field
The invention belongs to the preparation of alkane type biodiesel and the higher value application technical field of vegetable oil refining discarded object,
It is more particularly to a kind of using soap stock as method of the catalytic material Hydrogenation for alkane type biodiesel.
Background technology
Grease is the very important green regenerative energy sources carrier of a class, efficiently converts grease with catalyst technology
It is the most direction of industrial applications potentiality in current biomass trans-utilization for the especially green HC fuel of liquid fuel,
Therefore receive much concern.Most common mode is that ester-interchange method prepares first generation biodiesel, and the technology is existing at present widely to grind
Study carefully report, establish complete complete industrialized unit all over the world in Europe, South America etc., and in varing proportions with petrochemical industry fuel oil
Blending, improves exhaust emissions, is widely used.But biodiesel is mainly constituted in being fatty acid methyl ester, with oil
Hydrocarbon compound have certain difference in nature in physics and chemistry, its oxygen content is higher so that its calorific value is relatively low, oxidation stability
Difference, viscosity is larger, and condensation point is higher, it is impossible to used in very cold area, seriously hinders it as the wide of substitute energy source for petroleum
General application.Nearly ten years, vegetable fat catalytic hydrogenation prepares the biodiesel of liquid alkane second and attracted attention, and turns into
The study hotspot all received much concern in current world wide.National Biomass Energy Development " 13 " planning also mentions quickening emphatically
Advanced biological liquid fuel technological progress and production demonstration are promoted, the year two thousand twenty is striven, biological liquid fuel year utilization reaches
To more than 6,000,000 tons.
Grease catalytic hydrogenation is the technology that the oxy radical removing in grease is generated to long chain alkane using hydrogenation catalyst.
Due to generation long chain alkane molecule in structure composition and properties all than biodiesel closer to petrifaction diesel, therefore
It can be made an addition in practical application with bigger ratio in petrifaction diesel, with more preferable application prospect.Invention
CN104722329A discloses a kind of method that bio-oil catalytic hydrogenation prepares alkane, and wherein bio-oil mainly uses peanut
Oil, rapeseed oil, olive oil etc.；Invention CN105237319A discloses a kind of unrighted acid and prepares long chain alkane for raw material
Method, wherein main use tetradecenoic acid, gaidic acid, oleic acid, linoleic acid etc. for original；Invention CN103555362A is disclosed
A kind of method that utilization tung oil prepares alkane biodiesel.So, at present it has been reported that mainly use soybean oil, palm
The vegetable fat such as oil, castor oil, vegetable oil cost is higher, and there is the problem of striving grain with people.The activity of current hydrogenation catalyst
Component is mainly Pt, Pd noble metal, and partial catalyst needs to be vulcanized, and easily causes sulphur loss, causes diesel oil sulfur content
Cross high, have a strong impact on quality.
With the continuous improvement developed rapidly with fats and Oils Refining Technology of oil prodution industry, oil foot in oil and fat refining process and
The yield of the accessory substances such as soap stock is increasing.China can discharge nearly ten million ton of various oil foots and soap stock every year, if these resources
Deal with improperly, the waste and environmental pollution of resource can be caused, or even threaten human body health；, will be into but if rationally utilizing
To prepare the valuable source of high-quality biological liquid fuel, effectively alleviate energy demand and the resource ring of restriction socio-economic development
Border problem.《National Long-and Medium-term Development planning outline (2006~the year two thousand twenty)》Also clearly by " regenerative resource low-coat scale
Change and develop " it is used as the theme first developed.Therefore, using largely idle discarded soap stock resource, reproducible the is developed
Two generation alkane type biodiesel technologies of preparing, may advantageously facilitate the development and innovation of biomass liquid fuel industry, contribute to excellent
Change energy resource structure, improve the ecological environment, develop a circular economy, with important economic benefits, ecological effect and social effect.
The content of the invention
The technical problem of solution：The new way of high-quality biological diesel oil is prepared by waste resource catalyzed conversion in order to open up one
Footpath, solves current biodiesel industry and there is cost of material height, the defects such as grain are striven with people；Sulphurized catalyst non-environmental protection, and cause
The excessively high deficiency of product sulfur content, the present invention provides a kind of method that alkane type biodiesel is prepared by raw material of soap stock.
Technical scheme：A kind of method that alkane type biodiesel is prepared by raw material of soap stock, comprises the following steps：(1) soap
Pin is pre-processed：Soap stock is added in mixture kettle, be stirred continuously it is lower add acid regulation to lower aqueous solution into pH value be 5-6,
Acidification oil is obtained after 20min, layered dehydration, filtration treatment are incubated at 60-80 DEG C；(2) catalytic hydrogenation reaction：By the acid of acquisition
Carburetion, solvent and catalyst are separately added into autoclave, and solvent load is the 20wt.%-60wt.% of acidification oil consumption,
Catalyst amount is the 0.5wt.%-2wt.% of acidification oil consumption；Hydrogen is passed through, reaction initial pressure is 1-3MPa, opens and adds
Heat and mechanical agitation, controlling reaction temperature are 280-350 DEG C, react 2-6h, after reaction terminates, and filter out catalyst, revolving removing
C is obtained after solvent14-C20Liquid alkane mixture, as alkane type biodiesel.
It is preferred that, the soap stock is the accessory substance of vegetable oil refining process, water containing 30wt.%-45wt.%,
25wt.%-40wt.% fatty acid sodium salts, 10wt.%-30wt.% glyceride.
It is preferred that, the pretreated acidification oil acid number of soap stock is 90-140mgKOH/g.
Above-mentioned hydrogenation reaction path is mainly at least one of hydrogenation deoxidation, hydrogenation decarboxylation and hydrogenation decarbonylation.
It is preferred that, the solvent is at least one of n-hexane, normal heptane, hexamethylene, normal octane.
It is preferred that, the catalyst is the load type metal catalyst handled by hydrogen reducing, and the total of active component bears
Loading capacity is 4wt.%-20wt.%, and metal active constituent is at least one of Ni, Mo, Co.
Carrier is γ-Al in the catalyst2O3、SiO2, at least one of SAPO-11.
Beneficial effect：(1) present invention realizes the higher value application of soap stock waste resource, with vegetable oil refining discarded object soap
Pin is raw material, and the raw material for preparing alkane type biodiesel is obtained after acidified pretreatment, the utilization new way of soap stock is opened, has
Effect solves waste and the environmental problem of soap stock efficient resource, and effectively alleviates insufficient raw material, the problems such as cost is high；
(2) present invention realizes unvulcanised catalyst soap stock acidification oil Hydrogenation for alkane type biodiesel, overcomes
Conventional vulcanized catalyst causes the excessively high defect of product sulfur content.
(3) the invention provides the overall path of an alkane type biodiesel that high-quality is prepared using waste resource,
Cost is low, process is simple, is suitable for industrialized production, with preferable environmental benefit and social benefit.
Brief description of the drawings
Fig. 1 is technological process of production schematic diagram of the invention.
Embodiment
The following examples are that the present invention is expanded on further, but the invention is not restricted to this.
Embodiment 1
Soybean oil soap stock is added in mixing kettle, be stirred continuously it is lower add acid regulation to lower aqueous solution into pH value be 5-
6,20min is incubated at 60-80 DEG C, it is 126mgKOH/g acidification oils that acid number is obtained after dehydration, filtration treatment；By the acid of acquisition
Carburetion, solvent hexamethylene and (5%-8%) Ni-Mo/ γ-Al2O3Catalyst is separately added into autoclave, hexamethylene consumption
For the 30wt.% of acidification oil consumption, catalyst amount is the 0.8wt.% of acidification oil consumption, is passed through hydrogen, reacts initial pressure
For 2.5MPa, heating and mechanical agitation are opened, controlling reaction temperature is 340 DEG C, reacts 5h, after reaction terminates, filters out catalysis
C is obtained after agent, revolving desolvation14-C20Liquid alkane mixture, as alkanes biodiesel.
Embodiment 2
Cottonseed oil soap stock is added in mixing kettle, be stirred continuously it is lower add acid regulation to lower aqueous solution into pH value be 5-
6,20min is incubated at 60-80 DEG C, it is 108mgKOH/g acidification oils that acid number is obtained after dehydration, filtration treatment；By the acid of acquisition
Carburetion, solvent normal octane and (4%-8%) Co-Mo/ γ-Al2O3Catalyst is separately added into autoclave, normal octane consumption
For the 60wt.% of acidification oil consumption, catalyst amount is the 0.5wt.% of acidification oil consumption, is passed through hydrogen, reacts initial pressure
For 1.0MPa, open heating and stir, controlling reaction temperature is 350 DEG C, react 6h, after reaction terminates, filter to isolate catalysis
C is obtained after agent, revolving desolvation14-C20Liquid alkane mixture, as alkanes biodiesel.
Embodiment 3
Rapeseed oil soapstock is added in mixing kettle, be stirred continuously it is lower add acid regulation to lower aqueous solution into pH value be 5-
6,20min is incubated at 60-80 DEG C, it is 95mgKOH/g acidification oils that acid number is obtained after dehydration, filtration treatment；By the acid of acquisition
Carburetion, solvent hexane and (8%-4%) Ni-Mo/SiO2Catalyst is separately added into autoclave, and n-hexane consumption is acid
The 20wt.% of carburetion consumption, catalyst amount is the 1.5wt.% of acidification oil consumption, is passed through hydrogen, and reaction initial pressure is
1.5MPa, opens heating and stirs, and controlling reaction temperature is 330 DEG C, reacts 4h, after reaction terminates, filters to isolate catalyst,
C is obtained after revolving desolvation14-C20Liquid alkane mixture, as alkanes biodiesel.
Embodiment 4
Sunflower oil soap stock is added in mixing kettle, be stirred continuously lower addition acid regulation is to lower aqueous solution into pH value
5-6,20min is incubated at 60-80 DEG C, and it is 115mgKOH/g acidification oils that acid number is obtained after dehydration, filtration treatment；By acquisition
Acidification oil, solvent n-heptane and (5%-10%) Co-Mo/SiO2Catalyst is separately added into autoclave, normal heptane consumption
For the 30wt.% of acidification oil consumption, catalyst amount is the 0.5wt.% of acidification oil consumption, is passed through hydrogen, reacts initial pressure
For 1.6MPa, open heating and stir, controlling reaction temperature is 360 DEG C, react 3h, after reaction terminates, filter to isolate catalysis
C is obtained after agent, revolving desolvation14-C20Liquid alkane mixture, as alkanes biodiesel.
Embodiment 5
Corn oil soap stock is added in mixing kettle, be stirred continuously it is lower add acid regulation to lower aqueous solution into pH value be 5-
6,20min is incubated at 60-80 DEG C, it is 132mgKOH/g acidification oils that acid number is obtained after dehydration, filtration treatment；By the acid of acquisition
Carburetion, solvent hexane and (10%-10%) Ni-Mo/SAPO-11 catalyst are separately added into autoclave, and n-hexane is used
Measure as the 60wt.% of acidification oil consumption, catalyst amount is the 1.0wt.% of acidification oil consumption, be passed through hydrogen, the initial pressure of reaction
Power is 2.4MPa, opens heating and stirs, and controlling reaction temperature is 280 DEG C, reacts 6h, after reaction terminates, filters to isolate and urge
C is obtained after agent, revolving desolvation14-C20Liquid alkane mixture, as alkanes biodiesel.
Embodiment 6
Soybean oil soap stock is added in mixing kettle, be stirred continuously it is lower add acid regulation to lower aqueous solution into pH value be 5-
6,20min is incubated at 60-80 DEG C, it is 140mgKOH/g acidification oils that acid number is obtained after dehydration, filtration treatment；By the acid of acquisition
Carburetion, solvent normal octane and (10%-5%) Co-Mo/SAPO-11 catalyst are separately added into autoclave, normal octane consumption
For the 40wt.% of acidification oil consumption, catalyst amount is the 1.8wt.% of acidification oil consumption, is passed through hydrogen, reacts initial pressure
For 2.8MPa, open heating and stir, controlling reaction temperature is 320 DEG C, react 2h, after reaction terminates, filter to isolate catalysis
C is obtained after agent, revolving desolvation14-C20Liquid alkane mixture, as alkanes biodiesel.
Reaction result in the embodiment of table 1
| Embodiment | Catalyst | Hydrogenation conversion % | Bio-diesel yield % |
| 1 | (10%-5%) Ni-Mo/ γ-Al2O3 | 100 | 79.4 |
| 2 | (4%-8%) Co-Mo/ γ-Al2O3 | 97 | 77.3 |
| 3 | (8%-4%) Ni-Mo/SiO2 | 92 | 74.2 |
| 4 | (5%-10%) Co-Mo/SiO2 | 99 | 78.1 |
| 5 | (10%-10%) Ni-Mo/SAPO-11 | 100 | 72.5 |
| 6 | (5%-10%) Co-Mo/SAPO-11 | 96 | 70.5 |
Claims (7)
1. a kind of method that alkane type biodiesel is prepared by raw material of soap stock, it is characterised in that comprise the following steps：
（1）Soap stock is pre-processed：Soap stock is added in mixture kettle, is stirred continuously and lower adds acid regulation to lower aqueous solution into pH value
For 5-6, acidification oil is obtained after 20 min, layered dehydration, filtration treatment are incubated at 60-80 DEG C；
（2）Catalytic hydrogenation reaction：The acidification oil, solvent and catalyst of acquisition are separately added into autoclave, solvent load
For the 20wt.%-60 wt.% of acidification oil consumption, catalyst amount is 0.5 wt.%-2 wt.% of acidification oil consumption；It is passed through hydrogen
Gas, reaction initial pressure is 1-3 MPa, opens heating and mechanical agitation, and controlling reaction temperature is 280-350 DEG C, reacts 2-6
H, after reaction terminates, C is obtained after filtering out catalyst, revolving desolvation14-C20Liquid alkane mixture, as alkane type are biological
Diesel oil.
2. according to claim 1 it is a kind of by raw material of soap stock prepare alkane type biodiesel method, it is characterised in that institute
The accessory substance that soap stock is vegetable oil refining process is stated, containing 30 wt.%-45 wt.% water, 25 wt.%-40 wt.% aliphatic acid
Sodium salt, 10 wt.%-30 wt.% glyceride.
3. according to claim 1 it is a kind of by raw material of soap stock prepare alkane type biodiesel method, it is characterised in that institute
The pretreated acidification oil acid number of soap stock is stated for 90-140 mgKOH/g.
4. according to claim 1 it is a kind of by raw material of soap stock prepare alkane type biodiesel method, it is characterised in that institute
It is mainly at least one of hydrogenation deoxidation, hydrogenation decarboxylation and hydrogenation decarbonylation to state hydrogenation reaction path.
5. according to claim 1 it is a kind of by raw material of soap stock prepare alkane type biodiesel method, it is characterised in that institute
It is at least one of n-hexane, normal heptane, hexamethylene, normal octane to state solvent.
6. according to claim 1 it is a kind of by raw material of soap stock prepare alkane type biodiesel method, it is characterised in that institute
It is the load type metal catalyst handled by hydrogen reducing to state catalyst, and the total load weight of active component is 4 wt.%-20
Wt.%, metal active constituent is at least one of Ni, Mo, Co.
7. according to claim 1 it is a kind of by raw material of soap stock prepare alkane type biodiesel method, it is characterised in that institute
It is γ-Al to state carrier in catalyst2O3、SiO2, at least one of SAPO-11.
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| CN201710426037.4A CN107118791A (en) | 2017-06-08 | 2017-06-08 | A kind of method that alkane type biodiesel is prepared by raw material of soap stock |
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| CN201710426037.4A CN107118791A (en) | 2017-06-08 | 2017-06-08 | A kind of method that alkane type biodiesel is prepared by raw material of soap stock |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112410118A (en) * | 2020-10-30 | 2021-02-26 | 中国林业科学研究院林产化学工业研究所 | Thermochemical pretreatment method for waste grease or soapstock |
| CN113355125A (en) * | 2021-06-11 | 2021-09-07 | 厦门大学 | Method for preparing long-chain alkane from waste biological oil through selective hydrogenation |
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| US4855037A (en) * | 1984-09-12 | 1989-08-08 | Nippon Kokan Kabushiki Kaisha | Hydrogenation catalyst for coal tar, a method of hydrogenation of coal tar with use of such catalyst, and a method of producing super needle coke from the hydrogenation product of coal tar |
| CN101067091A (en) * | 2007-06-08 | 2007-11-07 | 清华大学 | Solid catalysis process of preparing biodiesel oil continuously with high acid value material |
| CN105524667A (en) * | 2016-01-08 | 2016-04-27 | 北京航空航天大学 | Aviation alternative fuel and preparation method thereof |
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2017
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Patent Citations (3)
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|---|---|---|---|---|
| US4855037A (en) * | 1984-09-12 | 1989-08-08 | Nippon Kokan Kabushiki Kaisha | Hydrogenation catalyst for coal tar, a method of hydrogenation of coal tar with use of such catalyst, and a method of producing super needle coke from the hydrogenation product of coal tar |
| CN101067091A (en) * | 2007-06-08 | 2007-11-07 | 清华大学 | Solid catalysis process of preparing biodiesel oil continuously with high acid value material |
| CN105524667A (en) * | 2016-01-08 | 2016-04-27 | 北京航空航天大学 | Aviation alternative fuel and preparation method thereof |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112410118A (en) * | 2020-10-30 | 2021-02-26 | 中国林业科学研究院林产化学工业研究所 | Thermochemical pretreatment method for waste grease or soapstock |
| CN113355125A (en) * | 2021-06-11 | 2021-09-07 | 厦门大学 | Method for preparing long-chain alkane from waste biological oil through selective hydrogenation |
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