CN105733817A - Low-cost separation method and device for fatty acid mixture - Google Patents
Low-cost separation method and device for fatty acid mixture Download PDFInfo
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- CN105733817A CN105733817A CN201610087105.4A CN201610087105A CN105733817A CN 105733817 A CN105733817 A CN 105733817A CN 201610087105 A CN201610087105 A CN 201610087105A CN 105733817 A CN105733817 A CN 105733817A
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- C—CHEMISTRY; METALLURGY
- C11—ANIMAL OR VEGETABLE OILS, FATS, FATTY SUBSTANCES OR WAXES; FATTY ACIDS THEREFROM; DETERGENTS; CANDLES
- C11C—FATTY ACIDS FROM FATS, OILS OR WAXES; CANDLES; FATS, OILS OR FATTY ACIDS BY CHEMICAL MODIFICATION OF FATS, OILS, OR FATTY ACIDS OBTAINED THEREFROM
- C11C1/00—Preparation of fatty acids from fats, fatty oils, or waxes; Refining the fatty acids
- C11C1/08—Refining
- C11C1/10—Refining by distillation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/10—Vacuum distillation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/143—Fractional distillation or use of a fractionation or rectification column by two or more of a fractionation, separation or rectification step
- B01D3/148—Fractional distillation or use of a fractionation or rectification column by two or more of a fractionation, separation or rectification step in combination with at least one evaporator
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
- B01D3/26—Fractionating columns in which vapour and liquid flow past each other, or in which the fluid is sprayed into the vapour, or in which a two-phase mixture is passed in one direction
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/43—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/43—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
- C07C51/44—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation by distillation
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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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
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/10—Greenhouse gas [GHG] capture, material saving, heat recovery or other energy efficient measures, e.g. motor control, characterised by manufacturing processes, e.g. for rolling metal or metal working
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Abstract
The invention discloses a low-cost separation method and device for fatty acid mixture.A decompression rectifying tower is used for continuously separating and refining C12-C22 fatty acid components.A direct contact condensation mode is adopted in the tower top to efficiently cool rising material steam, the cooled rising material steam is processed by a heat recovery boiler into secondary steam to be used, a vapor-phase product on the tower bottom is processed by a demister and then condensed, and acceptable products are extracted.Residues on the tower bottom enter a wiped film evaporator and an erucic acid refining tower to be separated, and high-purity erucic acid is acquired.In the whole process, by means of thermal coupling gradient utilization, the heat consumption in the production process is minimized, and low cost, low emission and high yield are achieved.
Description
Technical field
The present invention relates to chemical field, be specifically related to low-cost separation method and the segregation apparatus thereof of a kind of fatty acid mixed.
Background technology
Fatty acid is to be linked, by hydro carbons group, the class carboxylic acid compound that carboxyl is constituted, and is the basic material of the important raw material of industry and oil and fat chemical.Fatty acid radical can be divided into short-chain fatty acid according to carbon chain lengths, and the carbon number in its carbochain is less than 6；Medium-chain fatty acid, in its carbochain, carbon number is the fatty acid of 6-12, mainly sad and capric acid；Long-chain fatty acid, in its carbochain, carbon number is more than 12.Can also be divided three classes according to the difference that whether saturated the C-H bond on its hydrocarbon backbone is: satisfied fatty acid, the C-H bond on its hydrocarbon backbone does not contain unsaturated double-bond；Monounsaturated fatty acid, the C-H bond on its hydrocarbon backbone has a unsaturated double-bond, also known as oleic acid；Polyunsaturated fatty acid, containing two or more unsaturated double-bonds in the C-H bond on its hydrocarbon backbone, such as linoleic acid, linolenic acid etc..
For the mixed type fatty acid system containing satisfied fatty acid, monounsaturated fatty acid and polyunsaturated fatty acid, existing separation and purification process ubiquity small scale, energy consumption are high, product yield is low with purity, temperature-sensitive decomposition is many and high value added product separates many defects such as difficulty.Therefore develop advanced technologies and the key equipment of new fatty acid mixed separation and purification process, improve product yield, reduce production cost, not only assist in enterprise and increase economic efficiency, more meet the requirement of energy-saving and emission-reduction.
Summary of the invention
It is contemplated that at least solve one of technical problem of existence in prior art.
To achieve these goals, technical scheme is as follows:
A kind of low-cost separation method of fatty acid mixed, its technological process is as it is shown in figure 1, it comprises the following steps:
Step 1, fatty acid mixed feedstock transportation to be separated is easily separated to vacuum rectification tower (T1)；The theoretical cam curve of described vacuum rectification tower (T1) is 50-80 block, described mixing-in fat acid starting material is the hydrolyzate of C12-C18 Petiolus Trachycarpi wet goods Vegetable oil lipoprotein and the fatty acid mixed being mixed to form by different proportion with Animal fat hydrolyzate thereof, and its carbon atom substantially forms and with content is: C12-C14:5-15%；C16:20-30%；C18:55-65%；C22:1-3%；Heavy constituent ≯ 1%, the feeding temperature of described vacuum rectification tower (T1) is 40-160 DEG C, operation pressure is 0.08-0.3MPa, vacuum rectification tower overhead vapours condensation rear portion is as backflow, reflux ratio is between 3-20, extraction part is the fatty acid of the first products C 12-C14, and the temperature of condensed water is heated to 85-120 DEG C, and the first order for raw material heats；
Step 2, side line output C16 fatty acid between the rectifying section 10-30 block column plate of described vacuum rectification tower (T1), with the waste heat of the C16 fatty acid of output, raw material is carried out second level heating, being then input to storage tank, the purity of C16 fatty acid can reach 99.2%；
Step 3, vacuum rectification tower (T1) bottom temperature is 230-250 DEG C, kettle material pumps into falling-film reboiler (E4), described falling-film reboiler (E4) uses the conduction oil of 260-300 DEG C or the steam heating higher than 260 DEG C, the operation pressure of vacuum rectification tower is 1-3kPa, liquid-vapor mixture enters storage tank (S2) and separates, a gaseous phase materials part in storage tank (S2) returns to vacuum rectification tower (T1), after being partly into demister (D1) process, enter the 4th heat exchanger (E5), output C18 fatty acid after heat exchange condensation, the water that cold flow body is 60-80 DEG C that 4th heat exchanger (E5) uses produces the steam of 2-3atm after heat exchange, heat energy produces for downstream；
Liquid phase part in step 4, above-mentioned storage tank (S2) is pumped to luwa evaporator (E6), vapour-liquid material in luwa evaporator (E6) is delivered to erucic acid rectifying column (T2), pressure in erucic acid rectifying column (T2) is 0.5-2.5kPa, column bottom temperature is 270-300 DEG C, overhead extraction C18 fatty acid mixt, extraction C22 erucic acid at the bottom of tower, purity reaches 99.5%；
Wherein step 2, step 3 and step 4 are without time order and function order.
The low-cost separation method of the fatty acid mixed of the present invention adopts the combination of continuous rectification under vacuum, wiped film vaporization and rectified purified process, namely side line vacuum rectification tower separate raw materials more than is first adopted, such as from top to bottom, four strands of materials such as extraction C12～C14, C16, C18, C18～C22 successively.In rectification under vacuum column overhead, an overhead condensation gained liquid part is sent into tower top as coolant after cooling in the 3rd heat exchanger and is continued condensation upflowing vapor, namely traditional vapour-liquid heat exchange pattern is substituted by the mode of the liquid direct condensation by contact of liquid heat exchange, heat-transfer effect is good, can effectively prevent the condensation of material, and solve susceptible to plugging problem during conventional tubular heat exchanger process high-boiling components material.At the bottom of tower, adopting pump forced conveyance, preventing high-temperature material from crossing thermal decomposition or carbonization with falling-film reboiler form, improve the thermal efficiency, improve the yield of product.Gained steam, a part is after demister processes, and condensed acquisition liquid-phase product extraction, all the other steam then enter at the bottom of tower to maintain continuous rectification operation.In sum, the low-cost separation method of the fatty acid mixed of the present invention can fractionation of fatty acid starting material well, obtain product quality better, wide in variety, yield is higher.
The present invention also provides for the low-cost separation method equipment therefor vacuum rectification tower of a kind of fatty acid mixed.
nullA kind of vacuum rectification tower of the low-cost separation method for above-mentioned two fatty acid mixeds，It is a filler and the mixing rectifying column of valve plate composition，Its rectifying section arranges 10000-18000mm without the regular wire packing of wall stream,It is divided into 2-3 section，Liquid distribution adopts LQ-II without point of accumulation liquid distribution trough,Overhead reflux part adopts sprinkling equipment，Stripping section arranges the 20-40 super valve plate of block STV，It can also be other metal structured packing，It is highly 10000-20000mm,Rectification under vacuum column overhead has a dividing plate，Dividing plate has multiple riser 4 communicated with rectifying section under dividing plate，Each riser 4 there is a cover cap，Cover cap can allow the rising gas of riser (4) enter above dividing plate，It is avoided that the liquid that tower top sprays enters riser (4) simultaneously，So，Described dividing plate constitutes liquid trap (3)，Liquid trap (3) has the 5th pipeline (5) and valve that the liquid in liquid trap (3) is imported surge tank (S1)，And separately have pipeline to be guided into by the liquid in liquid trap (3) liquid distributor under dividing plate makes backflow；The tower reactor of vacuum rectification tower is funnel type, and wherein tubule section diameter is 200-800mm, and tubule Partial Height is 500-3000mm, and reducing part height in funnel top is 300-1000mm.
Accompanying drawing explanation
Fig. 1 is the process chart of the low-cost separation method of fatty acid mixed of the present invention.
Wherein: T1 is rectifying column；T2 is erucic acid treating column (rectifying column)；S1 is surge tank；S2 is storage tank；E1, E2, E3, E5 be first, second, third, fourth heat exchanger respectively；E4 is falling-film reboiler；D1 is demister；E6 is luwa evaporator；6,15,24 respectively the first pump, the second pump, the 3rd pump；1～2,5,7～14,16～23,25～27 respectively the first pipeline, second pipe, the 5th pipeline, the 7th-14 pipeline, the the ten six the-the two ten three pipeline, the the 25th the-the two ten seven pipeline；3 is liquid trap；4 is gas lift pipe.
Detailed description of the invention
Being described below in detail embodiments of the invention, the example of described embodiment is shown in the drawings, and wherein same or similar label represents same or similar element or has the element of same or like function from start to finish.The embodiment described below with reference to accompanying drawing is illustrative of, and is only used for explaining the present invention, and is not considered as limiting the invention.
Embodiment 1: certain 5kt/aC12～C22 fatty acid continuous treating project
The technique of this continuous treating fatty acid is as shown in Figure 1.The constituent mass mark of raw material of fatty acid is as follows: C12～C14:5%～15%；C16:20%～30%；C18:55%～65%；C22:1%～3%, heavy constituent is less than 1%.Treating capacity is 625kg/h.The tower diameter of described vacuum rectification tower T1 is 1400mm, height overall 32000mm, and its section of evaporating arranges 16000mmSINOPAK-B2 without the regular wire packing of wall stream, is divided into 3 sections.Liquid distribution adopts LQ-II without point of accumulation liquid distribution trough, and overhead reflux part adopts sprinkling equipment.Stripping section arranges 18 blocks of super valve platies of STV.The tower reactor of rectifying column is funnel type, and wherein tubule section diameter is 250mm, and tubule Partial Height is 2800mm, and reducing part height in funnel top is 800mm.Luwa evaporator area 15m2, erucic acid treating column tower diameter is 100mm, arranges SINOPAK-B2 without the regular wire packing 5000mm of wall stream.
625kg/h raw material of fatty acid is sent into rectifying column T1 through second pipe 2 by the first pipeline 1 after First Heat Exchanger E1, the second heat exchanger E2 heating are to 175 DEG C and carries out rectification under vacuum.The tower top pressure of rectifying column T1 is about 1.8kPa, and reflux ratio is about 1.2.Being also connected with the 11st pipeline 11 directly over tower top, the 11st pipeline is vacuum tube.Condensing after the subcooled liquid direct contact heat transfer that steam is sprayed after gas lift pipe 4 enters tower top, post liquefaction falls into liquid trap 3.Material in liquid trap 3 flows into surge tank S1 by the 5th pipeline 5, carries through the first pump 6, and a part is delivered to tower top as coolant spray, direct condensation by contact overhead vapours by after being water-cooled to 120 DEG C through the tenth pipeline 10 in the 3rd heat exchanger E3.And the cooling water of 40 DEG C is heated to 85～95 DEG C and is delivered in First Heat Exchanger E1 for preheating material by the 9th pipeline 9 in the 3rd heat exchanger E3, C12～C14 product is via the 8th pipeline 8 extraction.Being positioned at the side line of the rectifying section C16 product through the 15th pipeline 12 extraction after raw material is carried out second level heating by the second heat exchanger E2, be finally expelled to storage tank by the 13rd pipeline 13, purity is about 99.2% after testing；The temperature of rectifying column T1 tower reactor is 240 DEG C～250 DEG C, the material of tower reactor is pumped into falling-film reboiler E4 through the 14th pipeline 14 by the second pump 15, falling-film reboiler E4 uses the heat-conducting oil heating of about 270 DEG C, pressure is 2.3kPa, liquid-vapor mixture enters storage tank S2 and separates, a gaseous phase materials part in storage tank S2 returns to rectifying column T1 through the 17th pipeline 17, demister D1 process is entered in part through the 18th pipeline 18, condenser E5 is entered then through the 19th pipeline 19, the water that cold flow body is 60～80 DEG C that condenser E5 uses, the steam of 2～3atm is obtained after heat exchange, discharged by the 22nd pipeline 22, heat energy produces for downstream, C18 product is through the 20th pipeline 20 extraction.Condensed water inlet pipeline i.e. the 21st pipeline 21 is provided with flow control valve, controls the produced quantity of C18 by controlling the flow of condensed water, and then controls the opposing steam flow amount in the 17th pipeline 17.Restructuring lease making the 23rd pipeline 23 and the 3rd pump 24 in storage tank S2 enter luwa evaporator E6, luwa evaporator E6 uses the conduction oil of 300 DEG C to be hot fluid, and the tower reactor of luwa evaporator E6 discharges the impurity such as remaining high boiling component, non-saponifiable matter, non-volatile component by the 27th pipeline 27；Gas-liquid material in luwa evaporator E6 is delivered in rectifying column (i.e. erucic acid treating column T2), pressure in erucic acid treating column T2 is 2.1kPa, column bottom temperature is about 290 DEG C, tower top passes through the 26th pipeline 26 extraction C18 (linoleic acid, oleic acid, stearic acid) mixture, through the 25th pipeline 25 extraction C22 erucic acid at the bottom of tower, purity is about 99.5%.
Obtaining through metering and accounting, adopt this method with device separating mixed fatty acid compared with original Technology, yield can improve 6.5%, and energy consumption of unit product can save 36.2%, and the investment of ton material equipment saves more than 30%.
Embodiment 2: certain 10kt/aC12～C22 fatty acid continuous treating project
The technique of this continuous treating fatty acid is as shown in Figure 1.The constituent mass mark of raw material of fatty acid is as follows: C12～C14:4%～10%；C16:25%～30%；C18:55%～60%；C22:1%～2%, heavy constituent is less than 1%, and treating capacity is 1250kg/h.Described vacuum rectification tower T1 diameter 2000mm, height overall 36000mm, its rectifying section arranges regular wire packing 18000mm, is divided into 3 sections.Overhead reflux part adopts sprinkling equipment, and liquid distribution adopts without point of accumulation liquid distribution trough.Stripping section arranges regular wire packing 16000mm, and the tower reactor of rectifying column is funnel type, and wherein tubule section diameter is 500mm, and tubule Partial Height is 3000mm, and reducing part height in funnel top is 600mm.Luwa evaporator area 30m2, erucic acid treating column tower diameter is 150mm, arranges regular wire packing 5000mm.
1250kg/h raw material of fatty acid is sent into rectifying column T1 through second pipe 2 by the first pipeline 1 after First Heat Exchanger E1, the second heat exchanger E2 heating are to 173 DEG C and carries out rectification under vacuum.The tower top pressure of rectifying column T1 is about 1.7kPa, and reflux ratio is about 1.15.Being also connected with the 11st pipeline 11 directly over tower top, the 11st pipeline is vacuum tube.Condensing after the subcooled liquid direct contact heat transfer that steam is sprayed after gas lift pipe 4 enters tower top, post liquefaction falls into liquid trap 3.Material in liquid trap 3 flows into surge tank S1 by the 5th pipeline 5, carries through the first pump 6, and a part is delivered to tower top as coolant spray, direct condensation by contact overhead vapours by after being water-cooled to 120 DEG C through the tenth pipeline 10 in the 3rd heat exchanger E3.And the cooling water of 42 DEG C is heated to 92 DEG C and is delivered in First Heat Exchanger E1 for preheating material by the 9th pipeline 9 in the 3rd heat exchanger E3, C12～C14 product is via the 8th pipeline 8 extraction.Being positioned at the side line of the rectifying section C16 product through the 15th pipeline 12 extraction after raw material is carried out second level heating by the second heat exchanger E2, be finally expelled to storage tank by the 13rd pipeline 13, purity is about 99.4% after testing；The temperature of rectifying column T1 tower reactor is 248 DEG C, the material of tower reactor is pumped into falling-film reboiler E4 through the 14th pipeline 14 by the second pump 15, falling-film reboiler E4 uses the heat-conducting oil heating of about 272 DEG C, pressure is 2.1kPa, liquid-vapor mixture enters storage tank S2 and separates, a gaseous phase materials part in storage tank S2 returns to rectifying column T1 through the 17th pipeline 17, demister D1 process is entered in part through the 18th pipeline 18, condenser E5 is entered then through the 19th pipeline 19, the water that cold flow body is 68 DEG C that condenser E5 uses, the steam of 2.6atm is obtained after heat exchange, discharged by the 22nd pipeline 22, heat energy produces for downstream, C18 product is through the 20th pipeline 20 extraction.Condensed water inlet pipeline i.e. the 21st pipeline 21 is provided with flow control valve, controls the produced quantity of C18 by controlling the flow of condensed water, and then controls the opposing steam flow amount in the 17th pipeline 17.Restructuring lease making the 23rd pipeline 23 and the 3rd pump 24 in storage tank S2 enter luwa evaporator E6, luwa evaporator E6 uses the steam of 280 DEG C to be hot fluid, and the tower reactor of luwa evaporator E6 discharges the impurity such as remaining high boiling component, non-saponifiable matter, non-volatile component by the 27th pipeline 27；Gas-liquid material in luwa evaporator E6 is delivered in rectifying column (i.e. erucic acid treating column T2), pressure in erucic acid treating column T2 is 2.0kPa, column bottom temperature is about 289 DEG C, tower top passes through the 26th pipeline 26 extraction C18 (linoleic acid, oleic acid, stearic acid) mixture, through the 25th pipeline 25 extraction C22 erucic acid at the bottom of tower, purity is about 99.1%.
Obtaining through metering and accounting, adopt this method with device separating mixed fatty acid compared with existing Technology, yield can improve 6.6%, and energy consumption of unit product can save 40.6%, and the investment of ton material equipment saves more than 42%.Embodiment 3: certain 100kt/aC12～C22 fatty acid continuous treating project
The technique of this continuous treating fatty acid is as shown in Figure 1.The constituent mass mark of raw material of fatty acid is as follows: C12～C14:5%～10%；C16:23%～35%；C18:50%～68%；C22:2%～3%, heavy constituent is less than 1%, and treating capacity is 12500kg/h,
Rectifying column T1 diameter 6000mm, height overall 40000mm, its rectifying section arranges 20000mm, and regular wire packing is divided into 3 sections.Liquid distribution adopts without point of accumulation liquid distribution trough.Stripping section arranges 24 blocks of super valve platies of STV, and the tower reactor of rectifying column is funnel type, and wherein tubule section diameter is 500mm, and tubule Partial Height is 5500mm, and reducing part height in funnel top is 1500mm.Adopting 3 luwa evaporators in parallel, every table top amasss 100m2, erucic acid treating column tower diameter is 800mm, arranges without the regular wire packing 7000mm of wall stream.
12500kg/h raw material of fatty acid is sent into rectifying column T1 through second pipe 2 by the first pipeline 1 after First Heat Exchanger E1, the second heat exchanger E2 heating are to 173 DEG C and carries out rectification under vacuum.The tower top pressure of rectifying column T1 is about 1.9kPa, and reflux ratio is about 1.3.Being also connected with the 11st pipeline 11 directly over tower top, the 11st pipeline is vacuum tube.Condensing after the subcooled liquid direct contact heat transfer that steam is sprayed after gas lift pipe 4 enters tower top, post liquefaction falls into liquid trap 3.Material in liquid trap 3 flows into surge tank S1 by the 5th pipeline 5, carries through the first pump 6, and a part is delivered to tower top as coolant spray, direct condensation by contact overhead vapours by after being water-cooled to 120 DEG C through the tenth pipeline 10 in the 3rd heat exchanger E3.And the cooling water of 46 DEG C is heated to 100 DEG C and is delivered in First Heat Exchanger E1 for preheating material by the 9th pipeline 9 in the 3rd heat exchanger E3, C12～C14 product is via the 8th pipeline 8 extraction.Being positioned at the side line of the rectifying section C16 product through the 15th pipeline 12 extraction after raw material is carried out second level heating by the second heat exchanger E2, be finally expelled to storage tank by the 13rd pipeline 13, purity is about 99.1% after testing；The temperature of rectifying column T1 tower reactor is 251 DEG C, the material of tower reactor is pumped into falling-film reboiler E4 through the 14th pipeline 14 by the second pump 15, falling-film reboiler E4 uses the steam heating of about 285 DEG C, rectifying column operation pressure is 2.4kPa, liquid-vapor mixture enters storage tank S2 and separates, a gaseous phase materials part in storage tank S2 returns to rectifying column T1 through the 17th pipeline 17, demister D1 process is entered in part through the 18th pipeline 18, condenser E5 is entered then through the 19th pipeline 19, the water that cold flow body is 72 DEG C that condenser E5 uses, the steam of 2.9atm is obtained after heat exchange, discharged by the 22nd pipeline 22, heat energy produces for downstream, C18 product is through the 20th pipeline 20 extraction.Condensed water inlet pipeline i.e. the 21st pipeline 21 is provided with flow control valve, controls the produced quantity of C18 by controlling the flow of condensed water, and then controls the opposing steam flow amount in the 17th pipeline 17.Restructuring lease making the 23rd pipeline 23 and the 3rd pump 24 in storage tank S2 enter luwa evaporator E6, luwa evaporator E6 uses the steam of 285 DEG C to be hot fluid, and the tower reactor of luwa evaporator E6 discharges the impurity such as remaining high boiling component, non-saponifiable matter, non-volatile component by the 27th pipeline 27；Gas-liquid material in luwa evaporator E6 is delivered in rectifying column (i.e. erucic acid treating column T2), pressure in erucic acid treating column T2 is 1.8kPa, column bottom temperature is about 283 DEG C, tower top passes through the 26th pipeline 26 extraction C18 (linoleic acid, oleic acid, stearic acid) mixture, through the 25th pipeline 25 extraction C22 erucic acid at the bottom of tower, purity is about 99.3%.
Obtaining through metering and accounting, adopt this method with device separating mixed fatty acid compared with existing Technology, yield can improve 5.2%, and energy consumption of unit product can save 40.6%, and the investment of ton material equipment saves more than 42%.
Above-described embodiment utilizes the fatty acid component of vacuum rectification tower continuous separating refining C12～C22.Tower top adopts direct condensation by contact mode efficiently to cool down upflowing vapor, and bottom product, after demister processes, condenses extraction product, and connect luwa evaporator and erucic acid rectifying column to process still residual, it is thus achieved that high-purity erucic acid.In subtractive process, the heat consumption being made production process by thermal coupling cascade utilization is minimum, it is achieved that energy-saving and emission-reduction, reduces cost, the purpose increased economic efficiency.
Although an embodiment of the present invention has been shown and described, it will be understood by those skilled in the art that: these embodiments can being carried out multiple change, amendment, replacement and modification when without departing from principles of the invention and objective, the scope of the present invention is limited by claim and equivalent thereof.
Claims (3)
1. a low-cost separation method for fatty acid mixed, is characterized in that it comprises the following steps:
Step 1, fatty acid mixed feedstock transportation to be separated is easily separated to vacuum rectification tower (T1)；The theoretical cam curve of described vacuum rectification tower (T1) is 50-80 block, described mixing-in fat acid starting material is the hydrolyzate of C12-C18 Petiolus Trachycarpi wet goods Vegetable oil lipoprotein and the fatty acid mixed being mixed to form by different proportion with Animal fat hydrolyzate thereof, and its carbon atom substantially forms and with content is: C12-C14:5-15%；C16:20-30%；C18:55-65%；C22:1-3%；Heavy constituent ≯ 1%, the feeding temperature of described vacuum rectification tower (T1) is 40-160 DEG C, operation pressure is 0.08-0.3MPa, vacuum rectification tower overhead vapours condensation rear portion is as backflow, reflux ratio is between 3-20, extraction part is the fatty acid of the first products C 12-C14, and the temperature of condensed water is heated to 85-120 DEG C, and the first order for raw material heats；
Step 2, side line output C16 fatty acid between the rectifying section 10-30 block column plate of described vacuum rectification tower (T1), with the waste heat of the C16 fatty acid of output, raw material is carried out second level heating, being then input to storage tank, the purity of C16 fatty acid reaches 99.2%；
Step 3, vacuum rectification tower (T1) bottom temperature is 230-250 DEG C, kettle material pumps into falling-film reboiler (E4), described falling-film reboiler (E4) uses the conduction oil of 260-300 DEG C or the steam heating higher than 260 DEG C, the operation pressure of vacuum rectification tower is 1-3kPa, liquid-vapor mixture enters storage tank (S2) and separates, a gaseous phase materials part in storage tank (S2) returns to vacuum rectification tower (T1), after being partly into demister (D1) process, enter the 4th heat exchanger (E5), output C18 fatty acid after heat exchange condensation, the water that cold flow body is 60-80 DEG C that 4th heat exchanger (E5) uses produces the steam of 2-3atm after heat exchange, heat energy produces for downstream；
Liquid phase part in step 4, above-mentioned storage tank (S2) is pumped to luwa evaporator (E6), vapour-liquid material in luwa evaporator (E6) is delivered to erucic acid rectifying column (T2), pressure in erucic acid rectifying column (T2) is 0.5-2.5kPa, column bottom temperature is 270-300 DEG C, overhead extraction C18 fatty acid mixt, extraction C22 erucic acid at the bottom of tower；
Wherein step 2, step 3 and step 4 are without time order and function order.
2. the low-cost separation method of fatty acid mixed according to claim 1, it is characterized in that: the high-temperature material of described rectification under vacuum top of tower and side take-off is each through the direct or indirect heat exchange of waste heat boiler, producing temperature is the low-pressure steam of 110-130 DEG C, heat source or the preheating and pipe insulation etc. as raw material of fatty acid is provided for other user.
null3. the vacuum rectification tower for the low-cost separation method of the fatty acid mixed described in claim 1，It is characterized in that: it is a filler and the mixing rectifying column of valve plate composition，Its rectifying section arranges 10000-18000mm without the regular wire packing of wall stream,It is divided into 2-3 section，Liquid distribution adopts LQ-II without point of accumulation liquid distribution trough,Overhead reflux part adopts sprinkling equipment，Stripping section arranges the 20-40 super valve plate of block STV，It can also be other metal structured packing，It is highly 10000-20000mm,Rectification under vacuum column overhead has a dividing plate，Dividing plate has multiple riser 4 communicated with rectifying section under dividing plate，Each riser 4 there is a cover cap，Cover cap can allow the rising gas of riser (4) enter above dividing plate，It is avoided that the liquid that tower top sprays enters riser (4) simultaneously，So，Described dividing plate constitutes liquid trap (3)，Liquid trap (3) has the 5th pipeline (5) and valve that the liquid in liquid trap (3) is imported surge tank (S1)，And separately have pipeline to be guided into by the liquid in liquid trap (3) liquid distributor under dividing plate makes backflow；The tower reactor of vacuum rectification tower is funnel type, and wherein tubule section diameter is 200-800mm, and tubule Partial Height is 500-3000mm, and reducing part height in funnel top is 300-1000mm.
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| CN109011676A (en) * | 2018-08-21 | 2018-12-18 | 浙江工业大学 | A kind of achievable material is rapidly heated the rectifying column of vaporization |
| CN109806607A (en) * | 2017-11-21 | 2019-05-28 | 辽宁海德新化工有限公司 | A kind of device that material purity can be improved |
| CN110041998A (en) * | 2019-05-16 | 2019-07-23 | 南安市蒂巧工艺品有限公司 | A kind of fatty acid refining plant |
| CN110433519A (en) * | 2019-08-30 | 2019-11-12 | 中冶焦耐(大连)工程技术有限公司 | A kind of return-flow system and method for distilling tower top |
| CN112827204A (en) * | 2021-02-07 | 2021-05-25 | 吉林凯莱英医药化学有限公司 | Vacuum purification device and purification system |
| CN113105949A (en) * | 2021-04-01 | 2021-07-13 | 河北隆海生物能源股份有限公司 | Equipment and process for producing high-purity octadecyl methyl ester by using waste animal and vegetable oil |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109806607A (en) * | 2017-11-21 | 2019-05-28 | 辽宁海德新化工有限公司 | A kind of device that material purity can be improved |
| CN109011676A (en) * | 2018-08-21 | 2018-12-18 | 浙江工业大学 | A kind of achievable material is rapidly heated the rectifying column of vaporization |
| CN109011676B (en) * | 2018-08-21 | 2021-06-04 | 浙江工业大学 | Rectifying tower capable of realizing rapid temperature rise and vaporization of materials |
| CN110041998A (en) * | 2019-05-16 | 2019-07-23 | 南安市蒂巧工艺品有限公司 | A kind of fatty acid refining plant |
| CN110433519A (en) * | 2019-08-30 | 2019-11-12 | 中冶焦耐(大连)工程技术有限公司 | A kind of return-flow system and method for distilling tower top |
| CN112827204A (en) * | 2021-02-07 | 2021-05-25 | 吉林凯莱英医药化学有限公司 | Vacuum purification device and purification system |
| CN113105949A (en) * | 2021-04-01 | 2021-07-13 | 河北隆海生物能源股份有限公司 | Equipment and process for producing high-purity octadecyl methyl ester by using waste animal and vegetable oil |
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