CN101319148A - Combined rectification column for preparing biological diesel oil - Google Patents
Combined rectification column for preparing biological diesel oil Download PDFInfo
- Publication number
- CN101319148A CN101319148A CNA2008100226375A CN200810022637A CN101319148A CN 101319148 A CN101319148 A CN 101319148A CN A2008100226375 A CNA2008100226375 A CN A2008100226375A CN 200810022637 A CN200810022637 A CN 200810022637A CN 101319148 A CN101319148 A CN 101319148A
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- tower
- solid catalyst
- filler
- rectification column
- rectifying
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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 present invention discloses a combined type fractionating tower device for preparing biological diesel oil, comprising a tower kettle, a fractionating tower body, and an overhead condenser, wherein the two kettle is provided with the fractionating tower body; the fractionating tower body is provided with the overhead condenser; the fractionating tower body is divided into an upper part and a lower part, wherein the upper part is a tower plate rectifying section and consists of the tower wall of the fractionating tower and a plurality of tower plates; the tower wall is uniformly provided with the plurality of tower plates; the tower plate is provided with a web on which a solid catalyst is adhered; the lower part is a filler catalytic reaction section; the filler is filled in the tower wall of the fractionating tower; the solid catalyst is filled into the filler. Grease and gas state alcohol are conversely fed, which quickly contact the surface of the catalyst, and which participate in an esterification reaction along with the tower plate. The reaction products which are biological diesel oil and glycerol flow into the bottom of the kettle, and the surplus gas state alcohol is subjected to the cooling of the overhead condenser, and then returns to the fractionating tower for duty-cycle operation, thereby realizing the processes of reaction and rectifying in the same device.
Description
Technical field
The present invention relates to a kind of preparation facilities of biofuel, relate in particular to a kind of combined rectification column device that is used to prepare biofuel.
Background technology
Along with becoming increasingly conspicuous of current environment and oil price problem, utilize renewable resources to prepare biofuel and have far-reaching strategic importance.
The preparation method of biofuel mainly is the method production that esterification or transesterification reaction take place under catalyst action with grease and alcohol in reactor at present, and resulting product also needs to relate to a lot of devices and equipment through separating and the purified process.At present emerging method is to adopt supercritical process production biofuel, does not need any catalyzer, and its limitation is required temperature, a pressure height of reaction, to the equipment requirements height, invest bigger, the increase production cost.Greasy utilization is in the experimental study stage mostly to high acid value at present, owing to wherein contain the free fatty acids of various structures, the acid value height is difficult to finish with simple one step of method, and its suitability for industrialized production rests on intermittent type or semicontinuous state all the time.To the research of high acid value preparing biodiesel from lipid, Chinese patent CN1473907A has set forth the method for the high acid value preparing biodiesel from lipid of intermittent type; Chinese patent CN1916114A has discussed the homogeneous phase serialization and has prepared method of bio-diesel oil, and the raw material that relates to is the refining grease of low acid value, and its acid value is below 3.The intermittent process of high acid value stearic reaction, potential safety hazards such as " run, leak, drip " inevitable in the production process, still very serious by the equipment corrosion that an acidic catalyst causes, also make facility investment repeatability too high simultaneously, cause the waste of manpower and materials.According to existing patented technology, also there are not effective ways to realize the complete serialization of high acid value preparing biodiesel from lipid.
From prior art, the overwhelming majority adopts batch still, the pot type mode of production, acid value being higher than 20 raw material finishes reaction and does not isolatingly have in same device, can the also mostly of serialization production be to adopt under super critical condition, to react, severe reaction conditions, temperature, pressure is all very high, so the production cost of these methods is higher, is difficult to realize suitability for industrialized production.
Summary of the invention
In order to solve the severe reaction conditions of the continuously producing biodiesel that prior art exists, be difficult to realize industrialization, batch production can not be finished reaction and isolating shortcoming simultaneously in a device, the invention provides a kind of combined rectification column for preparing biofuel, can in same device, finish reaction and separate, can realize serialization production, reduce the investment of equipment, reduce production costs.
The present invention adopts following technical scheme: a kind of combined rectification column that is used to prepare biofuel, comprise the tower still, the rectifying tower tower body, overhead condenser, described tower still is provided with the rectifying tower tower body, the rectifying tower tower body is provided with overhead condenser, described rectifying tower tower body is divided into, following two portions, top is the column plate rectifying section, tower wall and polylith column plate by rectifying tower are formed, evenly be provided with the polylith column plate on the tower wall, be provided with silk screen on column plate, solid catalyst is attached on the silk screen, and the bottom is the filler catalyst reaction section, in the tower wall of rectifying tower, be filled with filler, fill solid catalyst in the described filler.Column plate is a sieve-board type, the outlet weir height: distance between plates=(0.3～0.5): 1, and the height=40mm-200mm on tray outlet weir.The rectifying tower stage number is the 50-100 piece.Described filler is a Raschig ring, fills solid catalyst in Raschig ring, and the surface of Raschig ring is provided with reticulation.Described solid catalyst is acidic solid catalyst or alkali solid catalyst.Described acidic solid catalyst be in zirconium class solid super-strong acid, tin class solid super-strong acid, sulphonated coal, the lignosulfonic acid any one, described alkali solid catalyst is any one in alkali metal hydroxide, CaO, ZnO, MgO or the compound catalyzer.Described alkali metal hydroxide is any one in potassium hydroxide, sodium hydroxide, the calcium hydroxide.Described compound catalyzer is NaOH/ γ-Al
2O
3, K
2O/ γ-Al
2O
3, KF/ γ-Al
2O
3, among the KF/CaO any one.Solid catalyst is magnetic or non magnetic catalyzer.
Glyceride stock enters from cat head during production, and the solid catalyst that from top to bottom passes through on column plate rectifying section and the column plate reacts fully; Gaseous state alcohol as methyl alcohol, ethanol, branched-chain alcoho etc. are by adding at the bottom of the tower, after the tower still is heated to boiling, from bottom to top under the solid catalyst effect of filler conversion zone with top under grease fully react.Grease and gaseous state alcohol are reverse reinforced, contact rapidly at catalyst surface, carry out esterification in column plate section and packing section in the presence of catalyzer, reaction product biofuel, glycerine flow at the bottom of the still, and unnecessary gaseous state alcohol returns rectifying tower and recycles after the overhead condenser cooling.In same device, finish reaction and rectifying simultaneously, realized successive reaction.Packing section and the reaction of column plate section Continuous Contact make reaction mass fully contact with catalyzer, and duration of contact is long, reacts more complete.If only with tray column or packing tower, the duration of contact of material and catalyzer is short, has partial material and also do not have enough time to participate in reacting just to flow away.
Compared with prior art, the present invention has following advantage:
1) uses this rectifying tower device, make raw oil material and alcohol reverse reinforced, alcohol is entered in the reaction tower in the mode of gas phase, molecular activity is strengthened, enlarged the contact surface of reaction system, make reaction more abundant;
2) technical process of the present invention is simple, finishes the process of esterification and rectifying separation in a rectifying tower simultaneously, and reaction product can be separated at any time, has accelerated speed of response; Investment this part of minimizing equipment, device is few, and investment reduces, and has shortened Production Flow Chart, has reduced the loss of process;
3) the present invention does not have three-waste pollution, and unreacted gaseous state alcohol returns tower internal reaction, recycle again;
4) catalyst cupport of the present invention is on the rectifying tower column plate, but also supported catalyst of the filler in the rectifying tower, the contact that reacts fully, sufficient reacting has reduced the corrosion of catalyzer to equipment;
5) raw material of the present invention is applied widely, is particularly useful for the high acid value grease of raw material acid value between 20-140.
6) catalyzer can recycle, and refluxing the back solid catalyst with polar solvent can cycling and reutilization, has improved the utilization ratio of catalyzer.
Description of drawings
Fig. 1 is the present invention, is used to prepare the combined rectification column device of biofuel
Shown in the figure: 1. tower still; 2. filler; 3. rectifying tower tower body; 4. column plate; 5. overhead condenser; 6. pure receiver
Embodiment
The present invention is further detailed explanation below in conjunction with drawings and Examples, but the scope of protection of present invention is not limited to the scope shown in the embodiment.
Tower still, overhead condenser, pure receiver adopt general general-purpose equipment, and the column plate rectifying section of rectifying tower and filler catalyst reaction section design by the design requirements of common tray column and packing tower respectively.
A kind of combined rectification column that is used to prepare biofuel, comprise tower still 1, rectifying tower tower body 3, overhead condenser 5, described tower still 1 is provided with rectifying tower tower body 3, rectifying tower tower body 3 is provided with overhead condenser 5, described rectifying tower tower body 3 is divided into, following two portions, top is the column plate rectifying section, tower wall and polylith column plate 4 by rectifying tower are formed, evenly be provided with polylith column plate 4 on the tower wall, be provided with silk screen on column plate 4, solid catalyst is attached on the silk screen, and the bottom is the filler catalyst reaction section, in the tower wall of rectifying tower, be filled with filler 2, fill solid catalyst in the described filler 2.Column plate is a sieve-board type, the outlet weir height: distance between plates=(0.3～0.5): 1, and the height=40mm-200mm on tray outlet weir.The rectifying tower stage number is the 50-100 piece.Described filler is a Raschig ring, fills solid catalyst in Raschig ring, and the surface of Raschig ring is provided with reticulation.Described solid catalyst is acidic solid catalyst or alkali solid catalyst.Described acidic solid catalyst be in zirconium class solid super-strong acid, tin class solid super-strong acid, sulphonated coal, the lignosulfonic acid any one, described alkali solid catalyst is any one in alkali metal hydroxide, CaO, ZnO, MgO or the compound catalyzer.Described alkali metal hydroxide is any one in potassium hydroxide, sodium hydroxide, the calcium hydroxide.Described compound catalyzer is NaOH/ γ-Al
2O
3, K
2O/ γ-Al
2O
3, KF/ γ-Al
2O
3, among the KF/CaO any one.Solid catalyst is magnetic or non magnetic catalyzer.
Embodiment 1
Adopt combined rectification column device as shown in Figure 1, the structural parameter of tower are: rectifying tower diameter 1000mm, tray spacing 300mm, aperture 4mm, thickness of slab 2mm, the long 650mm in weir, height of weir 50mm, downtake sectional area/tower section amasss 0.068, hole area/column plate working area 0.09, downtake lower edge and tower plate surface apart from 30mm, filler ceramic raschig rings diameter 25mm, filler wall thickness 2.5mm, in the magnetic sulphonated coal solid catalyst is housed, two ends are sealed with silk screen, and bed stuffing height is 3m.With acid value is that 100 acidifying oil enters from rectifying tower top, and flow velocity is 0.0017m
3/ s, gaseous methanol enter at the bottom of tower continuously, and flow is 0.77m
3/ s, reverse reinforced, tower still temperature is 120 ℃.Silk screen is housed on column plate, fixing support catalyst, the magnetic sulphonated coal granules of catalyst is directly in bulk on column plate, and stage number is 100, and reflux ratio is 1.5.Unreacted methanol is returned the rectifying tower circulation after the overhead condenser condensation.The biofuel, the G ﹠ W that generate flow out through the tower still.
Embodiment 2
Adopt combined rectification column as shown in drawings, acid value is that 20 rubbish oil enters from rectifying tower top, and gaseous state ethanol enters at the bottom of tower continuously, and reverse reinforced, tower still temperature is 130 ℃.Wherein the rectifying tower filler is a Raschig ring, on the column plate and in the filler all load zirconium class solid super acid catalyst is arranged.Tray spacing is 400mm, and the outlet weir height is 120mm, and stage number is 100.Unreacted ethanol returns the rectifying tower circulation after the overhead condenser condensation.The biofuel, the G ﹠ W that generate flow out through the tower still.
Adopting combined rectification column as shown in drawings, is that raw material enters from rectifying tower top with the rapeseed oil, and the gaseous state Virahol enters at the bottom of tower continuously, and reverse reinforced, tower still temperature is 110 ℃.Wherein the rectifying tower filler is a Raschig ring, is placed with on the column plate to be carried on γ-Al
2O
3On the NaOH solid basic catalyst.Tray spacing is 400mm, and the outlet weir height is 200mm, and stage number is 50.Unreacted ethanol returns the rectifying tower circulation after the overhead condenser condensation.The biofuel and the glycerine that generate flow out through the tower still.
Embodiment 4
Adopt combined rectification column device as shown in Figure 1, the structural parameter of tower are: rectifying tower diameter 1000mm, tray spacing 300mm, aperture 4mm, thickness of slab 2mm, the long 650mm in weir, height of weir 50mm, downtake sectional area/tower section amasss 0.068, hole area/column plate working area 0.09, downtake lower edge and tower plate surface apart from 30mm, filler ceramic raschig rings diameter 25mm, filler wall thickness 2.5mm, in tin class solid super-strong acid solid catalyst is housed, two ends are sealed with silk screen, and bed stuffing height is 3m.With acid value is that 100 acidifying oil enters from rectifying tower top, and flow velocity is 0.0017m
3/ s, gaseous methanol enter at the bottom of tower continuously, and flow is 0.77m
3/ s, reverse reinforced, tower still temperature is 120 ℃.Silk screen is housed on column plate, fixing support catalyst, tin class solid super acid catalyst particle is directly in bulk on column plate, and stage number is 100, and reflux ratio is 1.5.Unreacted methanol is returned the rectifying tower circulation after the overhead condenser condensation.The biofuel, the G ﹠ W that generate flow out through the tower still.
Adopt combined rectification column device as shown in Figure 1, the structural parameter of tower are: rectifying tower diameter 1000mm, tray spacing 300mm, aperture 4mm, thickness of slab 2mm, the long 650mm in weir, height of weir 50mm, downtake sectional area/tower section amasss 0.068, hole area/column plate working area 0.09, downtake lower edge and tower plate surface apart from 30mm, filler ceramic raschig rings diameter 25mm, filler wall thickness 2.5mm, in the CaO solid catalyst is housed, two ends are sealed with silk screen, and bed stuffing height is 3m.With acid value is that 100 acidifying oil enters from rectifying tower top, and flow velocity is 0.0017m
3/ s, gaseous methanol enter at the bottom of tower continuously, and flow is 0.77m
3/ s, reverse reinforced, tower still temperature is 120 ℃.Silk screen is housed on column plate, fixing support catalyst, the CaO granules of catalyst is directly in bulk on column plate, and stage number is 100, and reflux ratio is 1.5.Unreacted methanol is returned the rectifying tower circulation after the overhead condenser condensation.The biofuel, the G ﹠ W that generate flow out through the tower still.
Embodiment 6
Adopt combined rectification column device as shown in Figure 1, the structural parameter of tower are: rectifying tower diameter 1000mm, tray spacing 300mm, aperture 4mm, thickness of slab 2mm, the long 650mm in weir, height of weir 50mm, downtake sectional area/tower section amasss 0.068, hole area/column plate working area 0.09, downtake lower edge and tower plate surface apart from 30mm, filler ceramic raschig rings diameter 25mm, filler wall thickness 2.5mm, in the potassium hydroxide solid catalyst is housed, two ends are sealed with silk screen, and bed stuffing height is 3m.With acid value is that 100 acidifying oil enters from rectifying tower top, and flow velocity is 0.0017m
3/ s, gaseous methanol enter at the bottom of tower continuously, and flow is 0.77m
3/ s, reverse reinforced, tower still temperature is 120 ℃.Silk screen is housed on column plate, fixing support catalyst, the potassium hydroxide catalyst particle is directly in bulk on column plate, and stage number is 100, and reflux ratio is 1.5.Unreacted methanol is returned the rectifying tower circulation after the overhead condenser condensation.The biofuel, the G ﹠ W that generate flow out through the tower still.
Claims (9)
1. combined rectification column that is used to prepare biofuel, comprise tower still (1), rectifying tower tower body (3), overhead condenser (5), described tower still (1) is provided with rectifying tower tower body (3), rectifying tower tower body (3) is provided with overhead condenser (5), it is characterized in that described rectifying tower tower body (3) is divided into, following two portions, top is the column plate rectifying section, tower wall and polylith column plate (4) by rectifying tower are formed, evenly be provided with polylith column plate (4) on the tower wall, on column plate (4), be provided with silk screen, solid catalyst is attached on the silk screen, the bottom is the filler catalyst reaction section, in the tower wall of rectifying tower, be filled with filler (2), fill solid catalyst in the described filler (2).
2.. the combined rectification column that is used to prepare biofuel according to claim 1 is characterized in that, column plate (4) is a sieve-board type, the outlet weir height: distance between plates=(0.3～0.5): 1, and the height=40mm-200mm on tray outlet weir.
3. the combined rectification column that is used to prepare biofuel according to claim 1 is characterized in that described filler (2) is a Raschig ring, fills solid catalyst in Raschig ring, and the surface of Raschig ring is provided with reticulation.
4. according to claim 1 or the 3 described combined rectification columns that are used to prepare biofuel, it is characterized in that described solid catalyst is acidic solid catalyst or alkali solid catalyst.
5. the combined rectification column that is used to prepare biofuel according to claim 4, it is characterized in that described acidic solid catalyst be in zirconium class solid super-strong acid, tin class solid super-strong acid, sulphonated coal, the lignosulfonic acid any one, described alkali solid catalyst is any one in alkali metal hydroxide, CaO, ZnO, MgO or the compound catalyzer.
6. the combined rectification column that is used to prepare biofuel according to claim 5 is characterized in that described alkali metal hydroxide is any one in potassium hydroxide, sodium hydroxide, the calcium hydroxide.
7. the combined rectification column that is used to prepare biofuel according to claim 5 is characterized in that described compound catalyzer is NaOH/ γ-Al
2O
3, K
2O/ γ-Al
2O
3, KF/ γ-Al
2O
3, among the KF/CaO any one.
8. the combined rectification column that is used to prepare biofuel according to claim 1 is characterized in that solid catalyst is magnetic or non magnetic catalyzer.
9. the combined rectification column that is used to prepare biofuel according to claim 1 is characterized in that the rectifying tower stage number is the 50-100 piece.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008100226375A CN101319148A (en) | 2008-07-18 | 2008-07-18 | Combined rectification column for preparing biological diesel oil |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008100226375A CN101319148A (en) | 2008-07-18 | 2008-07-18 | Combined rectification column for preparing biological diesel oil |
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|---|---|
| CN101319148A true CN101319148A (en) | 2008-12-10 |
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|---|---|---|---|
| CNA2008100226375A Pending CN101319148A (en) | 2008-07-18 | 2008-07-18 | Combined rectification column for preparing biological diesel oil |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102260595A (en) * | 2010-05-26 | 2011-11-30 | 北京石油化工学院 | Process for producing fatty acid methyl ester with grease waste |
| CN102358866A (en) * | 2011-09-15 | 2012-02-22 | 宁守俭 | Method for distillation synthesis of biodiesel by acid-catalyzed reaction |
| CN102628006A (en) * | 2012-04-13 | 2012-08-08 | 东南大学 | Catalytic distillation production method for biodiesel |
| CN102851122A (en) * | 2011-06-30 | 2013-01-02 | 中国石油化工股份有限公司 | Method for preparation of fatty acid ester |
| CN104479885A (en) * | 2014-11-28 | 2015-04-01 | 浙江赞宇科技股份有限公司 | Method and device for continuously producing triglyceride |
-
2008
- 2008-07-18 CN CNA2008100226375A patent/CN101319148A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102260595A (en) * | 2010-05-26 | 2011-11-30 | 北京石油化工学院 | Process for producing fatty acid methyl ester with grease waste |
| CN102851122A (en) * | 2011-06-30 | 2013-01-02 | 中国石油化工股份有限公司 | Method for preparation of fatty acid ester |
| CN102358866A (en) * | 2011-09-15 | 2012-02-22 | 宁守俭 | Method for distillation synthesis of biodiesel by acid-catalyzed reaction |
| CN102628006A (en) * | 2012-04-13 | 2012-08-08 | 东南大学 | Catalytic distillation production method for biodiesel |
| CN104479885A (en) * | 2014-11-28 | 2015-04-01 | 浙江赞宇科技股份有限公司 | Method and device for continuously producing triglyceride |
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Open date: 20081210 |