CN105194895B - A kind of method that biodiesel is prepared using thermal coupling next door reactive distillation column - Google Patents
A kind of method that biodiesel is prepared using thermal coupling next door reactive distillation column Download PDFInfo
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- CN105194895B CN105194895B CN201510553668.3A CN201510553668A CN105194895B CN 105194895 B CN105194895 B CN 105194895B CN 201510553668 A CN201510553668 A CN 201510553668A CN 105194895 B CN105194895 B CN 105194895B
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E50/00—Technologies for the production of fuel of non-fossil origin
- Y02E50/10—Biofuels, e.g. bio-diesel
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P30/00—Technologies relating to oil refining and petrochemical industry
- Y02P30/20—Technologies relating to oil refining and petrochemical industry using bio-feedstock
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Abstract
The invention discloses a kind of production method that biodiesel is prepared for thermal coupling next door reactive distillation column.Thermal coupling next door reactive distillation column includes condenser, reboiler and the king-tower with partition wall；The king-tower includes Reaction Separation region, extraction region and bottom of towe region；The preparation method of the high-purity biodiesel includes feedstock oil and alcohol contacts with catalyst into Reaction Separation region after preheating and carries out reaction pre-separation, water byproduct at the top of Reaction Separation region by producing, target product high-purity biodiesel component is produced as bottom of towe region and energy needed for providing raw material preheating, and unreacted component raw material alcohol at the top of extraction region via producing.The method of the present invention will be reacted and the separation of three kinds of materials is integrated into a tower, the effect of two rectifying columns is realized by a rectifying column, compared with common process, thermal coupling next door reactive distillation column has the effect saved equipment investment and reduce energy consumption production high-purity biodiesel.
Description
Technical field
The present invention relates to technical field of biochemical industry, more particularly to a kind of prepared using thermal coupling next door reactive distillation column to give birth to
The method of thing diesel oil.
Background technology
Biodiesel (Biodiesel Fuel) is for long-chain list alkane made of feedstock oil with vegetable oil or animal tallow etc.
Base ester, the reproducibility diesel fuel that petrifaction diesel can be replaced to be used in compression ignition engine, compared with traditional fossil energy, its
Sulphur and arene content are low, flash-point is high, Cetane number is high, have good lubricity, partly can be added in petrifaction diesel.
In recent years, with increasingly depleted and the mankind drastically the riseing to fuel energy demand of fossil energy, biological bavin
Oily industry is in widespread attention.Energy net gain can be improved, if there is environmental benefit and economic competitiveness, and can not subtract
A large amount of productions are the premises that can biodiesel realize commercial Application on the premise of few staple food supply.In production biodiesel process
In, catalyst plays the effect of key, and conventional has base catalyst, acidic catalyst, enzyme catalyst and organic catalyst etc..
Biological enzyme production biodiesel have reaction condition gentle, energy consumption is low, it is low for equipment requirements the advantages that.Patent
CN1436834A provides a kind of method of short-chain aliphatic ester synthesising biological oil plant, is urged at a suitable temperature using biology enzyme
Change the renewable resources such as animal and plant fat production biodiesel.But biological enzyme production cost is high, reaction efficiency is low, and catalyzing enzyme
Easy in inactivation, which prevent the application of biological enzyme technology in the industrial production, the research to it is now in the exploratory stage.
Compared with biological enzyme biodiesel synthesis, chemical method production biodiesel have production cost it is relatively low, reaction hold
Easy to control, the advantages that grease conversion ratio is high, for improving production efficiency, to reduce production cost significant.Patent CN
103756791A utilizes waste grease, biodiesel is produced in the presence of composite catalyst, grease conversion ratio is higher, catalyst
Reusable edible.Patent CN 103756792A remove most of free fatty in degreasing by pretreatment and effectively reduction contains
Water, by the soap in the effectively removing biodiesel of atlapulgite processing in ester exchange, glycerine, part foreign pigment etc., and
Stabilizer is added in post processing, adds the stability of biodiesel.
Although chemical method can improve the conversion ratio of bio-oil, production cost, its higher energy consumption load are reduced
As this method in the industry extensively using one of problems faced.Domestic and international experts and scholars are reducing plant energy consumption, reduce operation
Outstanding contribution is made that in terms of expense.Patent CN 103320233A propose a kind of biological using continuous tubular reactor production
The method of diesel oil, this method esterification reaction process is not heated, not stirred, energy-efficient, and whole flow process is under low-temperature atmosphere-pressure environment
Carry out, energy expenditure is low, utilization rate is high, energy-conserving and environment-protective；Patent US 2008312460A1 develop a kind of Vltrasonic device, utilize
Multi-frequency ultrasonic energy, vegetable oil or animal oil are converted into biodiesel, save energy consumption.
The content of the invention
Produce this higher problem of energy consumption in biodiesel process to reduce chemical method, the present invention propose it is a kind of by using
Thermal coupling next door reactive distillation column produces biodiesel to reduce the high-purity biodiesel preparation side that equipment investment reduces energy consumption
Method.
It is an object of the invention to provide a kind of process and device for producing high-purity biodiesel.The present invention passes through profit
Traditional two-tower process is reduced to single column flow with thermal coupling next door reactive distillation column, reduces equipment investment, and utilize tower
Interior thermal coupling reduces the energy consumption of production of biodiesel, and bottom of towe high-temperature product is used for into raw material preheating followed by, significantly carried
High energy utilization efficiency.
The present invention adopts the following technical scheme that：
The thermal coupling next door reactive distillation column that the present invention is used to prepare biodiesel includes king-tower, tower top with partition wall
Water condenser, tower top alcohol condenser and tower bottom reboiler；It is divided into Reaction Separation region inside king-tower, produces region and bottom of towe area
Domain, bottom of towe region are located at rectifying column bottom, and Reaction Separation region and extraction region are located at the middle and upper part of rectifying column, and both pass through perpendicular
Straight dividing plate is separated, and vertical clapboard upper end is connected with rectifying column tower top, and lower end is hanging in bottom of towe overlying regions.
Feedstock oil feed pipe and raw alcohol feed pipe are connected with outside the rectifying column in Reaction Separation region, is distinguished on two pipelines
Provided with fuel oil preheating device and raw alcohol preheater；The tower top that tower top water condenser passes through pipeline coupled reaction separated region；Tower
Push up the tower top that alcohol condenser connects extraction region by pipeline；The bottom of towe of rectifying column is provided with discharge nozzle, and discharge nozzle is divided into two, and one
Root connection tower bottom reboiler reconnects the rectifying tower body in extraction region, and another is sequentially connected fuel oil preheating device and raw alcohol is pre-
Hot device.
The Reaction Separation area filling catalysts, reactive distillation effect is played, produce region and bottom of towe region is filled out
High Efficient Standard Packing or column plate are filled, plays rectifying centrifugation.
The method of biodiesel is prepared using the thermal coupling next door reactive distillation column of the present invention is：
Feedstock oil and alcohol contact after preheating into Reaction Separation region with catalyst carries out reaction pre-separation, accessory substance
Water is by flowing out at the top of Reaction Separation region, and target product high-purity biodiesel component is flowed out by bottom of towe region and to provide raw material pre-
Energy needed for heat, unreacted component methanol is via extraction at the top of extraction region.
Described feedstock oil is free fatty.
Described raw alcohol is monohydric alcohol, preferably methanol.
Described catalyst is solid phase acid catalyst.
Thermal coupling next door reactive distillation column operating pressure is 100~1000kPa, reaction zone tower top operation temperature is 117~
152 DEG C, Reaction Separation region (I) operation temperature is 102~145 DEG C, and bottom of towe region (III) operation temperature is 120~350 DEG C.
Comprise the following steps that：
Thermal coupling next door reactive distillation column is entered by Reaction Separation region bottom after raw alcohol is preheated, feedstock oil is preheated
Thermal coupling next door reactive distillation column is entered by Reaction Separation area top afterwards, two raw materials occur in the presence of solid acid catalyst
Esterification, generate target product biodiesel and water byproduct.The Reaction Separation region of reactive distillation column in thermal coupling next door
Byproduct of reaction water is separated, and the water of high-purity is obtained in tower top, by overhead condenser condensation rear portion extraction, another portion
It is allocated as returning in tower for overhead reflux.In thermal coupling next door, the bottom of towe region high boiling component biodiesel of reactive distillation column obtains
Separation, and the biodiesel of high-purity is obtained in bottom of towe, the thermal source through tower bottom reboiler heat exchange rear portion as feeding preheating
The biodiesel that temperature reduces after being exchanged heat by feed preheater is produced as product, and another part flows back as bottom of towe to be risen
Steam is returned in tower.In thermal coupling next door, the extraction region unreacted components methanol of reactive distillation column is separated, and in tower top
The methanol of high-purity is obtained, by the condensation rear portion extraction of tower top alcohol condenser, another part is returned in tower as overhead reflux.
Relative to prior art, effect of the invention is that：
The production of high-purity biodiesel is realized in the reactive distillation column of thermal coupling next door, by traditional reactive distillation with after
The multitower of continuous process for separating and purifying is incorporated into a thermal coupling next door reactive distillation column, is saved equipment investment, is reduced energy
Consumption.Thermal coupling next door reactive distillation tower process realizes closed cycle, the raw material backflow recycling do not reacted completely, improves total
Conversion ratio.
The feed side filling catalysts of next door rectifying column of the present invention, make reaction be carried out in pre-separation section, i.e. structure
Into thermal coupling next door reactive distillation column.By the technique, more than 99%, gained biodiesel purity exists feedstock oil conversion ratio
More than 99.5%, reach same percent hydrolysis and product separation requirement, more than 30% is can save energy than popular response distillation process.
Brief description of the drawings
Fig. 1 is the process flow diagram that thermal coupling next door reactive distillation column produces high-purity biodiesel；
Description of reference numerals：
E1 tower top water condensers；E2 tower bottom reboilers；E3 tower top alcohol condensers；E4 fuel oil preheating devices；E5 raw alcohols are pre-
Hot device；RDWC thermal couplings next door reactive distillation column king-tower；1 feedstock oil；Feedstock oil after 2 preheatings；3 raw alcohols；Original after 4 preheatings
Expect alcohol；5 Reaction Separation area overhead vapor streams；6 extraction area's tower top methanol steams；7 condensed water；8 condensed methanol；9 is anti-
Answer Disengagement zone overhead reflux；10 extraction area's overhead refluxes；11 return tower section biodiesel；12 return tower biodiesel vapor；13 adopt
Go out part biological diesel oil；14 with raw alcohol heat exchange after biodiesel oil product；15 with feedstock oil heat exchange after biodiesel oil product；
I Reaction Separation region；II extraction region；III bottom of towe region.
Embodiment
The embodiment of the present invention is described in detail below in conjunction with accompanying drawing.It should be appreciated that this place is retouched
The embodiment stated is merely to illustrate and explain the present invention, and is not intended to limit the invention.
As shown in Figure 1：The thermal coupling next door reactive distillation column for being used to prepare biodiesel of the present invention, which includes having, to be separated
King-tower RDWC, the tower top water condenser E1 of wall, tower top alcohol condenser E3 and tower bottom reboiler E2；It is divided into Reaction Separation inside king-tower
Region I, produces region II and bottom of towe region III, and bottom of towe region III is located at rectifying column bottom, Reaction Separation region I and extraction region
II is located at the middle and upper part of rectifying column, and both are separated by vertical dividing plate, and vertical clapboard upper end is connected with rectifying column tower top,
Lower end is hanging above bottom of towe region III.
Feedstock oil feed pipe and raw alcohol feed pipe are connected with outside the rectifying column in Reaction Separation region I, is divided on two pipelines
She You not fuel oil preheating device E4 and raw alcohol preheater E5；Tower top water condenser E1 passes through pipeline coupled reaction separated region I
Tower top；Tower top alcohol condenser E3 connects the tower top of extraction region II by pipeline；The bottom of towe of rectifying column is provided with discharge nozzle, discharging
Pipe is divided into two, and a connection tower bottom reboiler E2 reconnects the rectifying tower body of extraction region II, and another is sequentially connected raw material
Oil preheater E4 and raw alcohol preheater E5.
Catalysts are filled in the Reaction Separation region I, are played reactive distillation effect, are produced region II and bottom of towe region
III filling High Efficient Standard Packing or column plate, play rectifying centrifugation.
The present invention use thermal coupling next door reactive distillation process flow for raw alcohol it is preheated after by Reaction Separation region
Bottom enters thermal coupling next door reactive distillation column RDWC, enters thermal coupling by the top of Reaction Separation region I after feedstock oil is preheated
Esterification, generation target product biology occur in the presence of solid acid catalyst for next door reactive distillation column RDWC, two raw materials
Diesel oil and water byproduct.In thermal coupling next door, the reactive distillation column RDWC byproduct of reaction water of Reaction Separation region I is separated,
The water of high-purity is obtained in tower top, by overhead condenser E1 condensation rear portion extraction, another part returns as overhead reflux
In tower.Separated in the bottom of towe region high boiling component biodiesel of thermal coupling next door reactive distillation column (RDWC), and in tower
Bottom obtains the biodiesel of high-purity, temperature after a part is exchanged heat as the thermal source of feeding preheating by feed preheater E4 and E5
The biodiesel that spending reduces produces as product, and another part rises steam after tower bottom reboiler E2 heat exchange as bottom of towe backflow
Return in tower.In thermal coupling next door, reactive distillation column RDWC extraction region II unreacted components methanol is separated, and in tower
Top obtains the methanol of high-purity, and by overhead condenser E3 condensation rear portion extraction, another part returns to tower as overhead reflux
It is interior.
In order to which the production effect of the present invention is better described, chooses three examples and be illustrated, these examples are only for act
The purpose of example explanation, and it is not intended to limitation the scope of the present invention.
Example 1：
The present invention use thermal coupling next door reactive distillation process flow for raw alcohol it is preheated after by Reaction Separation region
Bottom enters thermal coupling next door reactive distillation column RDWC, enters thermal coupling by the top of Reaction Separation region I after feedstock oil is preheated
Esterification, generation target product biology occur in the presence of solid acid catalyst for next door reactive distillation column RDWC, two raw materials
Diesel oil and water byproduct.In thermal coupling next door, the reactive distillation column RDWC byproduct of reaction water of Reaction Separation region I is separated,
The water of high-purity is obtained in tower top, by overhead condenser E1 condensation rear portion extraction, another part returns as overhead reflux
In tower.Separated in the bottom of towe region high boiling component biodiesel of thermal coupling next door reactive distillation column (RDWC), and in tower
Bottom obtains the biodiesel of high-purity, temperature after a part is exchanged heat as the thermal source of feeding preheating by feed preheater E4 and E5
The biodiesel that spending reduces produces as product, and another part rises steam after tower bottom reboiler E2 heat exchange as bottom of towe backflow
Return in tower.In thermal coupling next door, reactive distillation column RDWC extraction region II unreacted components methanol is separated, and in tower
Top obtains the methanol of high-purity, and by overhead condenser E3 condensation rear portion extraction, another part returns to tower as overhead reflux
It is interior.
Flow as shown in Figure 1.Each region actual plate number is as shown in table 1, and feed rate and composition are as shown in table 2.Feedstock oil
Feed entrance point (counting from top to bottom) with alcohol is respectively the 3rd piece and the 22nd piece theoretical plate of thermal coupling next door reactive distillation column RDWC,
Feeding temperature is 100 DEG C.Thermal coupling next door reactive distillation column RDWC operating pressures are 350kPa, and Reaction Separation region tower top is adopted
Output is 100kmol/h, and head temperature is 138 DEG C, and bottom temp is 107 DEG C；It is 100kmol/ to produce region overhead extraction amount
H, head temperature are 99 DEG C, and bottom temp is 104 DEG C；Bottom of towe zone flow is 100kmol/h, and head temperature is 107 DEG C, bottom
Temperature is 339 DEG C.Each logistics flux and composition are as shown in table 2, and gained biodiesel purity is 99.99%.
Each region actual plate number of table 1
| Tower section | Reactive distillation region | Produce region | Bottom of towe region |
| Actual plate number | 24 | 24 | 6 |
2 example of table 1 each logistics quality flow and each component mass fraction
Example 2：
The present invention use thermal coupling next door reactive distillation process flow for raw alcohol it is preheated after by Reaction Separation region
Bottom enters thermal coupling next door reactive distillation column RDWC, enters thermal coupling by the top of Reaction Separation region I after feedstock oil is preheated
Esterification, generation target product biology occur in the presence of solid acid catalyst for next door reactive distillation column RDWC, two raw materials
Diesel oil and water byproduct.In thermal coupling next door, the reactive distillation column RDWC byproduct of reaction water of Reaction Separation region I is separated,
The water of high-purity is obtained in tower top, by overhead condenser E1 condensation rear portion extraction, another part returns as overhead reflux
In tower.Separated in the bottom of towe region high boiling component biodiesel of thermal coupling next door reactive distillation column (RDWC), and in tower
Bottom obtains the biodiesel of high-purity, temperature after a part is exchanged heat as the thermal source of feeding preheating by feed preheater E4 and E5
The biodiesel that spending reduces produces as product, and another part rises steam after tower bottom reboiler E2 heat exchange as bottom of towe backflow
Return in tower.In thermal coupling next door, reactive distillation column RDWC extraction region II unreacted components methanol is separated, and in tower
Top obtains the methanol of high-purity, and by overhead condenser E3 condensation rear portion extraction, another part returns to tower as overhead reflux
It is interior.
Flow as shown in Figure 1.Each region actual plate number is as shown in table 3, and feed rate and composition are as shown in table 4.Feedstock oil
Feed entrance point (counting from top to bottom) with alcohol is respectively the 3rd piece and the 22nd piece theoretical plate of thermal coupling next door reactive distillation column RDWC,
Feeding temperature is 100 DEG C.Thermal coupling next door reactive distillation column RDWC operating pressures are 350kPa, and Reaction Separation region tower top is adopted
Output is 80kmol/h, and head temperature is 139 DEG C, and bottom temp is 107 DEG C；It is 80kmol/h to produce region overhead extraction amount,
Head temperature is 100 DEG C, and bottom temp is 105 DEG C；Bottom of towe zone flow is 80kmol/h, and head temperature is 107 DEG C, bottom temperature
Spend for 339 DEG C.Each logistics flux and composition are as shown in table 2, and gained biodiesel purity is 99.99%.
Each region actual plate number of table 3
| Tower section | Reactive distillation region | Produce region | Bottom of towe region |
| Actual plate number | 24 | 24 | 6 |
4 example of table 1 each logistics quality flow and each component mass fraction
Example 3：
The present invention use thermal coupling next door reactive distillation process flow for raw alcohol it is preheated after by Reaction Separation region
Bottom enters thermal coupling next door reactive distillation column RDWC, enters thermal coupling by the top of Reaction Separation region I after feedstock oil is preheated
Esterification, generation target product biology occur in the presence of solid acid catalyst for next door reactive distillation column RDWC, two raw materials
Diesel oil and water byproduct.In thermal coupling next door, the reactive distillation column RDWC byproduct of reaction water of Reaction Separation region I is separated,
The water of high-purity is obtained in tower top, by overhead condenser E1 condensation rear portion extraction, another part returns as overhead reflux
In tower.Separated in the bottom of towe region high boiling component biodiesel of thermal coupling next door reactive distillation column (RDWC), and in tower
Bottom obtains the biodiesel of high-purity, temperature after a part is exchanged heat as the thermal source of feeding preheating by feed preheater E4 and E5
The biodiesel that spending reduces produces as product, and another part rises steam after tower bottom reboiler E2 heat exchange as bottom of towe backflow
Return in tower.In thermal coupling next door, reactive distillation column RDWC extraction region II unreacted components methanol is separated, and in tower
Top obtains the methanol of high-purity, and by overhead condenser E3 condensation rear portion extraction, another part returns to tower as overhead reflux
It is interior.
Flow as shown in Figure 1.Each region actual plate number is as shown in table 5, and feed rate and composition are as shown in table 6.Feedstock oil
Feed entrance point (counting from top to bottom) with alcohol is respectively the 3rd piece and the 22nd piece theoretical plate of thermal coupling next door reactive distillation column RDWC,
Feeding temperature is 100 DEG C.Thermal coupling next door reactive distillation column RDWC operating pressures are 350kPa, and Reaction Separation region tower top is adopted
Output is 90kmol/h, and head temperature is 139 DEG C, and bottom temp is 107 DEG C；It is 90kmol/h to produce region overhead extraction amount,
Head temperature is 99 DEG C, and bottom temp is 105 DEG C；Bottom of towe zone flow is 90kmol/h, and head temperature is 106 DEG C, bottom temperature
Spend for 339 DEG C.Each logistics flux and composition are as shown in table 2, and gained biodiesel purity is 99.99%.
Each region actual plate number of table 5
| Tower section | Reactive distillation region | Produce region | Bottom of towe region |
| Actual plate number | 24 | 24 | 6 |
6 example of table 1 each logistics quality flow and each component mass fraction
Although an embodiment of the present invention has been shown and described, for the ordinary skill in the art, can be with
A variety of changes, modification can be carried out to these embodiments, replace without departing from the principles and spirit of the present invention by understanding
And modification, the scope of the present invention is defined by the appended.
Claims (6)
- A kind of 1. method that biodiesel is prepared using thermal coupling next door reactive distillation column, it is characterised in that：Described rectifying column Including the king-tower (RDWC) with partition wall, tower top water condenser (E1), tower top alcohol condenser (E3) and tower bottom reboiler (E2)； It is divided into Reaction Separation region (I) inside king-tower, produces region (II) and bottom of towe region (III), bottom of towe region (III) is located at rectifying column Bottom, Reaction Separation region (I) and extraction region (II) are located at the middle and upper part of rectifying column, and both are separated by vertical dividing plate Come, vertical clapboard upper end is connected with rectifying column tower top, and lower end is hanging above bottom of towe region (III)；Feedstock oil feed pipe and raw alcohol feed pipe are connected with outside the rectifying column of the Reaction Separation region (I), on two pipelines It is respectively equipped with fuel oil preheating device (E4) and raw alcohol preheater (E5)；Tower top water condenser (E1) passes through pipeline coupled reaction point From the tower top of region (I)；Tower top alcohol condenser (E3) connects the tower top of extraction region (II) by pipeline；The bottom of towe of rectifying column is set There is discharge nozzle, discharge nozzle is divided into two, and a connection tower bottom reboiler (E2) reconnects the rectifying tower body of extraction region (II), separately One is sequentially connected fuel oil preheating device (E4) and raw alcohol preheater (E5)；The Reaction Separation region (I) fills catalysts, plays reactive distillation effect, produces region (II) and bottom of towe region (III) High Efficient Standard Packing or column plate are filled, plays rectifying centrifugation；The method that described thermal coupling next door reactive distillation column prepares biodiesel, it is comprised the following steps that：Feedstock oil and alcohol contact after preheating into Reaction Separation region (I) with catalyst carries out reaction pre-separation, accessory substance By being flowed out at the top of Reaction Separation region (I), target product high-purity biodiesel component is flowed out and carried by bottom of towe region (III) water For energy needed for raw material preheating, unreacted component methanol is via extraction at the top of extraction region (II).
- 2. preparation method as claimed in claim 1, it is characterised in that：Described feedstock oil is free fatty.
- 3. preparation method as claimed in claim 1, it is characterised in that：Described raw alcohol is monohydric alcohol.
- 4. preparation method as claimed in claim 3, it is characterised in that：Described raw alcohol is methanol.
- 5. preparation method as claimed in claim 1, it is characterised in that：Described catalyst is solid phase acid catalyst.
- 6. preparation method as claimed in claim 1, it is characterised in that：Thermal coupling next door reactive distillation column operating pressure is 100 ~1000kPa, reaction zone tower top operation temperature are 117~152 DEG C, and Reaction Separation region (I) operation temperature is 102~145 DEG C, Bottom of towe region (III) operation temperature is 120~350 DEG C.
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| CN102188831B (en) * | 2010-03-03 | 2013-12-25 | 中国石油化工股份有限公司 | Reactive distillation method |
| CN102358866A (en) * | 2011-09-15 | 2012-02-22 | 宁守俭 | Method for distillation synthesis of biodiesel by acid-catalyzed reaction |
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