CN109053355A - A kind of method of continuous rectification biphenyl purification - Google Patents
A kind of method of continuous rectification biphenyl purification Download PDFInfo
- Publication number
- CN109053355A CN109053355A CN201811150688.6A CN201811150688A CN109053355A CN 109053355 A CN109053355 A CN 109053355A CN 201811150688 A CN201811150688 A CN 201811150688A CN 109053355 A CN109053355 A CN 109053355A
- Authority
- CN
- China
- Prior art keywords
- tower
- biphenyl
- terphenyl
- debenzolizing
- benzene
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/04—Purification; Separation; Use of additives by distillation
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Analytical Chemistry (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Water Supply & Treatment (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The present invention relates to a kind of methods of continuous rectification biphenyl purification, material liquid is passed through into concatenated debenzolizing tower, biphenyl tower and terphenyl tower, material liquid is added in the middle part of debenzolizing tower, a small amount of hydrogen, benzene and biphenyl are produced at the top of debenzolizing tower, tower reactor produces remaining biphenyl, terphenyl mixture and three all tar and enters biphenyl tower；Biphenyl column overhead produces the diphenyl mixture containing benzene on a small quantity and is back to reaction liquid storage tank, side take-off high-purity biphenyl, and tower reactor extraction terphenyl and three all blended tars enter terphenyl tower；Terphenyl column overhead produces the diphenyl mixture containing terphenyl on a small quantity and returns to biphenyl tower feed inlet, side take-off high-purity terphenyl mixture, and tower reactor produces all tar of heavy constituent three.By the way that side take-off is arranged, while being suitble to large-scale production, operating flexibility big, high-purity biphenyl product that mass fraction is 99.9% or more can be obtained, compared with traditional batch technique, energy consumption of unit product can reduce 30-40%, have high economic value.
Description
Technical field
The present invention relates to chemical fields, and in particular to a kind of method of continuous rectification biphenyl purification.
Background technique
Biphenyl is important Organic Ingredients, is widely used in the fields such as medicine, pesticide, dyestuff, liquid crystal material.It can be used to close
At plasticizer, preservative, manufacture fuel, engineering plastics and high-energy fuel etc. can be also used for.Biphenyl is present in coal tar, crude oil
In natural gas.Chemically synthesized biphenyl meeting by-product terphenyl, terphenyl add the available hydrogenated terphenyl of hydrogen, hydrogenation three at present
Biphenyl is widely used in the industries such as petrochemical industry, synthetic fibers, synthetic resin, medicine, printing and dyeing, high temperature heat transfer, heating equipment
System, chemical fibre polymerize (terylene, nylon polymerization, spandex spinning by dry), organic silicon monomer synthesis, trichlorosilane and polysilicon, doctor
The fine chemistry industries such as medicine, pesticide, dyestuff intermediate, biodiesel.
The preparation method of biphenyl, which has, to be pyrolyzed the chemical synthesis of biphenyl processed by benzene and is joined by various coal tar fraction systems
The separation and Extraction method of benzene.Mass fraction of the biphenyl in coal tar is only 0.20%-0.40%, and extraction cost is higher.Chemistry closes
There are process control, superior product quality, the higher advantage of conversion ratio at method.The prevailing technology of chemical synthesis is " tubular type at present
Method ", i.e., be passed through benzene vapour the pipeline (700 DEG C or more) of red heat and respectively lose a hydrogen atom by 2 benzene moleculars and be combined with each other and make
Biphenyl, reaction process process meeting by-product terphenyl and mountain all tar are obtained, tune is mainly passed through using the purification of batch fractionating method at present
Whole produced quantity, operating pressure, reflux ratio obtain corresponding product, and full tower is rectifying section when due to batch fractionating, without stripping
Section, obtains same tower top, tower bottom composition product, and the energy consumption of batch fractionating must be greater than continuous rectification；Meanwhile batch process list
The batch processed time is long, causes production capacity low；Since batch fractionating tower is all stripping section, cuts and be not thorough between component, lead to product
Yield is low, is not suitable for large-scale production.
Chinese patent CN107129422A discloses a kind of continuous fine that high-purity biphenyl is extracted from crude benzol tower first raffinate
Method is evaporated, using the three tower cascade connected technique of high efficiency packing rectifying column, light group of benzene, toluene etc. is extracted to coal tar hydrogenation process crude benzol tower
Raffinate (referred to as first raffinate) further deep processing separation after point, obtains mixed xylenes, naphthalene component, high-purity biphenyl product,
The patent the method can extract biphenyl product, but complex process from the product after coal tar hydrogenating, and control requires high, operation
Elasticity is narrow, cannot get high-purity biphenyl product.
Summary of the invention
The purpose of the present invention is to solve the above-mentioned problems and provides a kind of method of continuous rectification biphenyl purification.
The purpose of the present invention is achieved through the following technical solutions:
Material liquid is passed through three rectifying columns being sequentially connected in series, three rectifying by a kind of method of continuous rectification biphenyl purification
Tower is respectively debenzolizing tower, biphenyl tower and terphenyl tower, and the debenzolizing tower is normal pressure or negative pressure rectifying column, the biphenyl tower and three
Benzene column is high vacuum negative pressure rectifying column, and uses side take-off form, detailed process are as follows:
(1) material liquid is added in the middle part of debenzolizing tower, and a small amount of hydrogen, benzene and biphenyl are produced at the top of debenzolizing tower, and tower reactor extraction is surplus
Remaining biphenyl, terphenyl mixture and three all tar enter biphenyl tower；
(2) biphenyl column overhead produces the diphenyl mixture containing benzene on a small quantity and is back to reaction liquid storage tank, and side take-off is high-purity
Biphenyl is spent, tower reactor extraction terphenyl and three all blended tars enter terphenyl tower；
(3) terphenyl column overhead produces the diphenyl mixture containing terphenyl on a small quantity and returns to biphenyl tower feed inlet, and side line is adopted
High-purity terphenyl mixture out, tower reactor produce all tar of heavy constituent three.
Further, the middle part of the debenzolizing tower is connected with hydrogen gas tank, pushes up with liquid storage tank connection, top gas discharging is reacted
Liquid discharging in portion's is connected with benzene storage tank, and tower reactor discharging is connected to biphenyl tower；
The top extraction pipe of the biphenyl tower is connected to benzene-biphenyl pans, and the benzene-biphenyl pans and reaction solution store up
Tank connection, the side line of biphenyl tower are connected to biphenyl product storage tank, and tower reactor discharging is connected to terphenyl tower；
The top extraction pipe of the terphenyl tower is connected to biphenyl-terphenyl pans, the biphenyl-terphenyl pans
The feed inlet of biphenyl tower is connected, the side line of terphenyl tower is connected to terphenyl product storage tank, and tower reactor discharges and three all tar storage tanks
Connection.
Further, the debenzolizing tower tower top operating pressure is 20-120kPa, preferably 80-101kPa；Biphenyl column overhead behaviour
Making pressure is 0.1-10kPa, preferably 0.5-5kPa；Terphenyl column overhead operating pressure is 0.05-8kPa, preferably 0.1-4kPa.
Further, the debenzolizing tower tower top operation temperature is 60-120 DEG C, and preferably 70-108 DEG C, tower reactor operation temperature is
200-300 DEG C, preferably 265-285 DEG C；
The biphenyl column overhead operation temperature is 80-130 DEG C, and preferably 90-112 DEG C, side line discharge operation temperature is 90-
140 DEG C, preferably 100-122 DEG C, tower reactor operation temperature are 180-350 DEG C, preferably 200-300 DEG C；
The terphenyl column overhead operation temperature be 150-200 DEG C, preferably 165-185 DEG C, side line discharge operation temperature
It is 200-250 DEG C, preferably 215-235 DEG C, tower reactor operation temperature is 280-450 DEG C, preferably 300-400 DEG C.
Further, the reflux ratio of the debenzolizing tower is 0.01-5, preferably 0.02-2；The reflux ratio of biphenyl tower is 0.5-
10, preferably 1-6；The reflux ratio of terphenyl tower is 0.1-8, preferably 1-5.
Further, it counts from top to bottom, biphenyl tower side take-off position is located at the 1/40-2/3 of tower, preferably 1/10-
At 3/5；Terphenyl tower side take-off position is at the 1/30-2/3 of tower, and at preferably 1/15-3/5, side take-off position is necessary
In the range of description, otherwise light component benzene content can be exceeded in biphenyl product, is unable to get high-purity biphenyl product.
Further, the column plate of the debenzolizing tower is 3-30 block, preferably 5-20 block；The column plate of biphenyl tower is 20-90 block, excellent
Select 30-80 block；The column plate of terphenyl tower is 10-60 block, preferably 20-50 block.
Further, the debenzolizing tower, biphenyl tower and terphenyl tower tower are provided with and efficiently separate filler, including Lamb wave
Line, expanded metals, gauze structured packing or efficient random packing.
Further, the tower reactor reboiler of the debenzolizing tower provides steam, the biphenyl tower and three using conventional reboiler
The tower reactor of biphenyl tower is directly heated using heating furnace, and the debenzolizing tower overhead condenser uses water cooling, biphenyl tower and terphenyl tower
Overhead condenser is cold using conduction oil.
Further, the pipe surface in the device for connection winds high temperature heating tape.
The present invention uses continuous three-tower rectification separating-purifying biphenyl, using benzene high-temperature dehydrogenation reaction solution as raw material, by continuous
Precise distillation separation while being suitble to large-scale production, operating flexibility big, can be obtained in conjunction with the form of two tower side take-offs
High-purity biphenyl product that mass fraction is 99.9% or more, and yield is in 93% or more, compared with traditional batch technique, unit
Product energy consumption can reduce 30-40%, have high economic value.
Detailed description of the invention
Fig. 1 is the schematic diagram of continuous rectification biphenyl purification method of the present invention；
Fig. 2 is the schematic diagram of 1 continuous rectification biphenyl purification method of comparative example；
Fig. 3 is the schematic diagram of 2 continuous rectification biphenyl purification method of comparative example；
Fig. 4 is the schematic diagram of 3 continuous rectification biphenyl purification method of comparative example；
In figure, the useless removing liquid storage tank of V101-；The first delivery pump of P1-；The second delivery pump of P2-；P3- third delivery pump；P4-
4th delivery pump；Water in CW1- condensation；Water in CW2- condensation；The hot condensate return of HWS2-；The hot condensate return of HWR2-；T1- takes off benzene
Tower；T2- biphenyl tower；T3- terphenyl tower；E101- debenzolizing tower reboiler；E102- debenzolizing tower condenser；The heating of E103- biphenyl tower
Furnace formula reboiler；E104- biphenyl tower condenser；E105- terphenyl tower heating furnace formula reboiler；E106- terphenyl tower condenser.
Specific embodiment
The present invention is described in detail combined with specific embodiments below.Following embodiment will be helpful to the technology of this field
Personnel further understand the present invention, but the invention is not limited in any way.It should be pointed out that the ordinary skill of this field
For personnel, without departing from the inventive concept of the premise, various modifications and improvements can be made.These belong to the present invention
Protection scope.
A kind of device of continuous rectification biphenyl purification, including three debenzolizing towers being sequentially connected in series, biphenyl tower and terphenyl tower,
Be connected through pipeline with hydrogen gas tank through pipeline with liquid storage tank connection, top of tower gas discharge react in the middle part of debenzolizing tower, liquid discharge and
Benzene storage tank is connected, and tower reactor discharging is connected to through pipeline with biphenyl tower；Biphenyl overhead extraction pipe is connected to benzene-biphenyl pans, in this
Between tank through pipeline with react flow container connection, biphenyl tower side line is connected to biphenyl product storage tank, and tower reactor discharging is through pipeline and terphenyl
Tower connection；Terphenyl overhead extraction pipe is connected to biphenyl-terphenyl pans, the pans through pipeline connection enter biphenyl tower into
Material mouth, terphenyl tower side line are connected to terphenyl product storage tank, and tower reactor discharging is connected to through pipeline with three all tar storage tanks；Biphenyl tower
It is directly heated with terphenyl tower tower reactor using heating furnace.
Debenzolizing tower is normal pressure or negative pressure tower, and tower top operating pressure is 20-120kPa, preferably 80-101kPa, tower top operation temperature
Degree be 60-120 DEG C, preferably 70-108 DEG C, tower reactor operation temperature be 200-300 DEG C, preferably 265-285 DEG C, reflux ratio 0.01-
5, preferably 0.02-2, column plate are 3-30 block, preferably 5-20 block；Biphenyl tower is negative pressure side take-off tower, and tower top operating pressure is
0.1-10kPa, preferably 0.5-5kPa, tower top operation temperature be 80-130 DEG C, preferably 90-112 DEG C, side line discharge operation temperature
It is 90-140 DEG C, preferably 100-122 DEG C, tower reactor operation temperature is 180-350 DEG C, preferably 200-300 DEG C, reflux ratio 0.5-
10, preferably 1-6, column plate are 20-90 block, preferably 30-80 block；Terphenyl tower is negative pressure side take-off tower, and tower top operating pressure is
0.05-8kPa, preferably 0.1-4kPa terphenyl column overhead operation temperature be 150-200 DEG C, preferably 165-185 DEG C, lateral line discharging
Mouth operation temperature is 200-250 DEG C, and preferably 215-235 DEG C, tower reactor operation temperature is 280-450 DEG C, preferably 300-400 DEG C, is returned
Stream is than being 0.1-8, and preferably 1-5, column plate is 10-60 block, preferably 20-50 block.
Debenzolizing tower, biphenyl tower and terphenyl tower tower are provided with and efficiently separate filler, including Lamb wave line, expanded metals, silk screen are regular
Filler or efficient random packing.Biphenyl tower side take-off position is counted at 1/40-2/3 from top to bottom in tower, preferably 1/10-3/5
Place, terphenyl tower side take-off position is counted at 1/30-2/3 from top to bottom in tower, at preferably 1/15-3/5.
Debenzolizing tower tower reactor reboiler provides steam using conventional reboiler, and biphenyl tower and terphenyl tower need to be mentioned using heating furnace
For steam, three tower reboiler heat mediums are all made of high temperature heat conductive oil.Debenzolizing tower overhead condenser uses water cooling, biphenyl tower and three
Biphenyl column overhead condenser is cold using conduction oil.To guarantee to produce energy continuous and steady operation, debenzolizing tower tower reactor extraction pipe, biphenyl tower
Overhead extraction pipe, biphenyl tower tower reactor extraction pipe, terphenyl column overhead extraction pipe, terphenyl tower tower reactor extraction pipe, are both needed to keep the temperature, and
Wind high temperature heating tape.
The method that biphenyl purification is used for using the device are as follows: material liquid is added in the middle part of debenzolizing tower, extraction at the top of debenzolizing tower
A small amount of hydrogen, benzene and biphenyl, tower reactor produce remaining biphenyl, terphenyl mixture and three all tar and enter biphenyl tower；Biphenyl tower
For high vacuum negative pressure rectifying column, using side take-off form, overhead extraction containing the diphenyl mixture of benzene, returns to reaction solution storage on a small quantity
Tank, side take-off high-purity biphenyl, tower reactor extraction terphenyl and three all blended tars enter terphenyl tower；Terphenyl tower is height
Negative pressure of vacuum rectifying column, using side take-off form, overhead extraction on a small quantity containing the diphenyl mixture of terphenyl, return biphenyl tower into
Material mouth, side take-off high-purity terphenyl mixture, tower reactor are all tar of heavy constituent three.
It is more specifical embodiment below.
Embodiment 1
The method of the present invention flow chart is shown in Fig. 1, and material liquid group becomes hydrogen 0.25wt%, benzene 65wt%, biphenyl 25wt%,
Terphenyl 7.75wt%, three all tar 2wt% are mixed, the material liquid being contained in raw material liquid storage tank V101 passes through the first delivery pump
P1 charging in the middle part of debenzolizing tower T1, debenzolizing tower T1 tower top operating pressure are normal pressure, and theoretical stage is 8 pieces, reflux ratio 0.03.It is de-
The tower bottom of benzene column T1 is equipped with debenzolizing tower reboiler E101, and tower top is equipped with debenzolizing tower condenser E102, debenzolizing tower condenser E102 warp
The processing for condensing upper water CW1 and condensate return HW1 is crossed, tower top fixed gas hydrogen is produced from condenser overhead, and condensate liquid part is returned
It flows in debenzolizing tower T1, another part discharge.The mixed liquor that debenzolizing tower T1 tower reactor obtains is delivered to connection by the second delivery pump P2
In the middle part of benzene column T2, biphenyl tower T2 tower top operating pressure is 1kPa, and theoretical stage 50, lateral line discharging position is in the 5th piece of theoretical stage
(counting from top to bottom), reflux ratio 3.It is equipped with directly-fired kiln reboiler E103 in the tower bottom of biphenyl tower T2, tower top is equipped with biphenyl
Tower condenser E104, biphenyl tower condenser E104 condense the processing of upper water HWS2 and hot condensate return HWR2 through overheat, and tower top is cold
Lime set largely returns in biphenyl tower T2, fraction extraction, produces a large amount of high-purity bigeminy benzaldehyde products in side take-off mouth.Biphenyl tower
The mixed liquor of T2 tower reactor is transported in the middle part of terphenyl tower T3 through third delivery pump P3, and terphenyl tower T3 tower top operating pressure is
1kPa, theoretical stage 30, lateral line discharging position (are counted) from top to bottom in the 5th piece of theoretical stage, reflux ratio 2.In terphenyl tower
The tower bottom of T3 is equipped with directly-fired kiln reboiler E105, and tower top is equipped with terphenyl tower condenser E106, terphenyl tower condenser
E106 passes through the processing of thermal conductivity hot oil, and overhead condensation liquid largely returns in terphenyl tower T3, fraction extraction, in side take-off
Mouth produces a large amount of terphenyl products, and three all tar of terphenyl tower T3 tower reactor extraction are delivered in storage tank through the 4th delivery pump P4.
It is separated by three tower continuous rectifications, biphenyl purity reaches 99.99wt%, yield 93%.
Embodiment 2
New method flow chart of the present invention is shown in Fig. 1, and material liquid group becomes hydrogen 0.25wt%, benzene 65wt%, biphenyl
25wt% mixes terphenyl 7.75wt%, and three tar 2wt%, material liquid is by the first delivery pump P1 in the middle part of debenzolizing tower T1
Charging, debenzolizing tower T1 tower top operating pressure are normal pressure, and theoretical stage is 10 pieces, and reflux ratio 0.05, debenzolizing tower T1 tower reactor obtains
Mixed liquor be delivered in the middle part of biphenyl tower T2 by pump, biphenyl tower T2 tower top operating pressure is 3kPa, theoretical stage 60, side line
Unloading position (is counted) from top to bottom in the 15th piece of theoretical stage, reflux ratio 2, and the mixed liquor that biphenyl tower T2 tower reactor obtains is defeated by pumping
It send in the middle part of terphenyl tower T3, terphenyl tower T3 tower top operating pressure is 3kPa, theoretical stage 40, and lateral line discharging position is the
10 pieces of theoretical stages (counting from top to bottom), reflux ratio 1.It is separated by three tower continuous rectifications, biphenyl purity reaches 99.92wt%, receives
Rate is 97%.
Comparative example 1
New method flow chart of the present invention is shown in Fig. 2, and material liquid group becomes hydrogen 0.25wt%, benzene 65wt%, biphenyl
25wt% mixes terphenyl 7.75wt%, and three tar 2wt%, material liquid is by the first delivery pump P1 in the middle part of debenzolizing tower T1
Charging, debenzolizing tower T1 tower top operating pressure are normal pressure, and theoretical stage is 15 pieces, and reflux ratio 0.1, debenzolizing tower T1 tower reactor obtains
Mixed liquor is delivered in the middle part of biphenyl tower T2 by pump, and biphenyl tower T2 tower top operating pressure is 2kPa, theoretical stage 60, reflux ratio
It is 1, the mixed liquor that biphenyl tower T2 tower reactor obtains is delivered in the middle part of terphenyl tower T3 by pump, terphenyl tower T3 tower top operating pressure
For 2kPa, theoretical stage 35, reflux ratio 1.It is separated by three tower continuous rectifications, biphenyl purity reaches 98.21wt%, and yield is
81%.
Comparative example 2
New method flow chart of the present invention is shown in Fig. 3, and material liquid group becomes hydrogen 0.25wt%, benzene 65wt%, biphenyl
25wt% mixes terphenyl 7.75wt%, and three tar 2wt%, material liquid is by the first delivery pump P1 in the middle part of debenzolizing tower T1
Charging, debenzolizing tower T1 tower top operating pressure are normal pressure, and theoretical stage is 25 pieces, and reflux ratio 0.05, debenzolizing tower T1 tower reactor obtains
Mixed liquor be delivered in the middle part of biphenyl tower T2 by pump, biphenyl tower T2 tower top operating pressure is 4kPa, theoretical stage 70, side line
Unloading position (is counted) from top to bottom in the 20th piece of theoretical stage, and reflux ratio 2.5, the mixed liquor that biphenyl tower T2 tower reactor obtains passes through pump
It is delivered in the middle part of terphenyl tower T3, terphenyl tower T3 tower top operating pressure is 4kPa, theoretical stage 50, reflux ratio 1.5.It is logical
The separation of three tower continuous rectifications is crossed, biphenyl purity reaches 99.7wt%, yield 86%.
Comparative example 3
New method flow chart of the present invention is shown in Fig. 4, and material liquid group becomes hydrogen 0.25wt%, benzene 65wt%, biphenyl
25wt% mixes terphenyl 7.75wt%, and three tar 2wt%, material liquid is by the first delivery pump P1 in the middle part of debenzolizing tower T1
Charging, debenzolizing tower T1 tower top operating pressure are normal pressure, and theoretical stage is 25 pieces, and reflux ratio 0.05, debenzolizing tower T1 tower reactor obtains
Mixed liquor be delivered in the middle part of biphenyl tower T2 by pump, biphenyl tower T2 tower top operating pressure is 5kPa, theoretical stage 80, reflux
Than being 4, the mixed liquor that biphenyl tower T2 tower reactor obtains is delivered in the middle part of terphenyl tower T3 by pump, terphenyl tower T3 tower top operation pressure
Power is 8kPa, and theoretical stage 45, lateral line discharging position is in the 20th piece of theoretical stage (meter from top to bottom), reflux ratio 3.Pass through three
Tower continuous rectification separation, biphenyl purity reach 99.03wt%, yield 84%.
The present invention is separated by continuous precision rectifying, and in conjunction with two tower side take-off forms, mass fraction, which can be obtained, is
99.9% or more high-purity biphenyl product, yield is 93% or more.
Specific embodiments of the present invention are described above.It is to be appreciated that the invention is not limited to above-mentioned
Particular implementation, those skilled in the art can make various deformations or amendments within the scope of the claims, this not shadow
Ring substantive content of the invention.
Claims (10)
1. a kind of method of continuous rectification biphenyl purification, which is characterized in that material liquid is passed through into three rectifying columns being sequentially connected in series,
Three rectifying columns are respectively debenzolizing tower, biphenyl tower and terphenyl tower, and the debenzolizing tower is normal pressure or negative pressure rectifying column, the biphenyl
Tower and terphenyl tower are high vacuum negative pressure rectifying column, and use side take-off form, detailed process are as follows:
(1) material liquid is added in the middle part of debenzolizing tower, and a small amount of hydrogen, benzene and biphenyl are produced at the top of debenzolizing tower, and tower reactor extraction is remaining
The all tar of biphenyl, terphenyl mixture and three enters biphenyl tower；
(2) biphenyl column overhead produces the diphenyl mixture containing benzene on a small quantity and is back to reaction liquid storage tank, side take-off high-purity connection
Benzene, tower reactor extraction terphenyl and three all blended tars enter terphenyl tower；
(3) terphenyl column overhead produces the diphenyl mixture containing terphenyl on a small quantity and returns to biphenyl tower feed inlet, and side take-off is high
Purity terphenyl mixture, tower reactor produce all tar of heavy constituent three.
2. a kind of method of continuous rectification biphenyl purification according to claim 1, which is characterized in that in the debenzolizing tower
Portion is connected with liquid storage tank connection, top gas discharging is reacted with hydrogen gas tank, and overhead-liquid discharging is connected with benzene storage tank, tower reactor discharging
It is connected to biphenyl tower；
The top extraction pipe of the biphenyl tower is connected to benzene-biphenyl pans, and the benzene-biphenyl pans connect with liquid storage tank is reacted
Logical, the side line of biphenyl tower is connected to biphenyl product storage tank, and tower reactor discharging is connected to terphenyl tower；
The top extraction pipe of the terphenyl tower is connected to biphenyl-terphenyl pans, the biphenyl-terphenyl pans connection
The side line of the feed inlet of biphenyl tower, terphenyl tower is connected to terphenyl product storage tank, and tower reactor discharging is connected to three all tar storage tanks.
3. a kind of method of continuous rectification biphenyl purification according to claim 1, which is characterized in that the debenzolizing tower tower top
Operating pressure is 20-120kPa, preferably 80-101kPa；Biphenyl column overhead operating pressure is 0.1-10kPa, preferably 0.5-5kPa；
Terphenyl column overhead operating pressure is 0.05-8kPa, preferably 0.1-4kPa.
4. a kind of method of continuous rectification biphenyl purification according to claim 1, which is characterized in that the debenzolizing tower tower top
Operation temperature is 60-120 DEG C, and preferably 70-108 DEG C, tower reactor operation temperature is 200-300 DEG C, preferably 265-285 DEG C；
The biphenyl column overhead operation temperature is 80-130 DEG C, and preferably 90-112 DEG C, side line discharge operation temperature is 90-140
DEG C, preferably 100-122 DEG C, tower reactor operation temperature is 180-350 DEG C, preferably 200-300 DEG C；
The terphenyl column overhead operation temperature is 150-200 DEG C, and preferably 165-185 DEG C, side line discharge operation temperature is
200-250 DEG C, preferably 215-235 DEG C, tower reactor operation temperature are 280-450 DEG C, preferably 300-400 DEG C.
5. a kind of method of continuous rectification biphenyl purification according to claim 1, which is characterized in that the debenzolizing tower returns
Stream is than being 0.01-5, preferably 0.02-2；The reflux ratio of biphenyl tower is 0.5-10, preferably 1-6；The reflux ratio of terphenyl tower is 0.1-
8, preferably 1-5.
6. a kind of method of continuous rectification biphenyl purification according to claim 1, which is characterized in that count, join from top to bottom
Benzene column side take-off position is located at the 1/40-2/3 of tower, at preferably 1/10-3/5；Terphenyl tower side take-off position is in tower
1/30-2/3 at, at preferably 1/15-3/5.
7. a kind of method of continuous rectification biphenyl purification according to claim 1, which is characterized in that the tower of the debenzolizing tower
Plate is 3-30 block, preferably 5-20 block；The column plate of biphenyl tower is 20-90 block, preferably 30-80 block；The column plate of terphenyl tower is 10-60
Block, preferably 20-50 block.
8. a kind of method of continuous rectification biphenyl purification according to claim 1, which is characterized in that the debenzolizing tower, connection
Benzene column and terphenyl tower tower are provided with and efficiently separate filler, including Lamb wave line, expanded metals, gauze structured packing, or efficiently dissipate heap
Filler.
9. a kind of method of continuous rectification biphenyl purification according to claim 1, which is characterized in that the tower of the debenzolizing tower
Kettle reboiler provides steam using conventional reboiler, and the tower reactor of the biphenyl tower and terphenyl tower is directly heated using heating furnace,
The debenzolizing tower overhead condenser uses water cooling, biphenyl tower and terphenyl column overhead condenser cold using conduction oil.
10. a kind of method of continuous rectification biphenyl purification according to claim 1, which is characterized in that be used in the device
The pipe surface of connection winds high temperature heating tape.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811150688.6A CN109053355B (en) | 2018-09-29 | 2018-09-29 | Method for purifying biphenyl by continuous rectification |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811150688.6A CN109053355B (en) | 2018-09-29 | 2018-09-29 | Method for purifying biphenyl by continuous rectification |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109053355A true CN109053355A (en) | 2018-12-21 |
| CN109053355B CN109053355B (en) | 2020-12-25 |
Family
ID=64767040
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811150688.6A Active CN109053355B (en) | 2018-09-29 | 2018-09-29 | Method for purifying biphenyl by continuous rectification |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109053355B (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111018652A (en) * | 2019-12-15 | 2020-04-17 | 江苏曼拓化学有限公司 | Preparation method of high-purity hydrogenated terphenyl heat conduction oil |
| CN111530114A (en) * | 2020-06-16 | 2020-08-14 | 上海化工研究院有限公司 | Rectification system, semi-continuous rectification method and application thereof |
| CN111659149A (en) * | 2020-06-16 | 2020-09-15 | 上海化工研究院有限公司 | Rectifying tower, rectifying system and application thereof |
| CN113144655A (en) * | 2021-04-28 | 2021-07-23 | 安徽金轩科技有限公司 | Jiale musk rectification unit and rectification process thereof |
| CN113636908A (en) * | 2021-08-13 | 2021-11-12 | 涉县津东经贸有限责任公司 | Terphenyl composition and preparation method thereof |
| CN114149299A (en) * | 2021-12-08 | 2022-03-08 | 涉县津东经贸有限责任公司 | Preparation method of biphenyl |
Citations (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3700566A (en) * | 1969-10-13 | 1972-10-24 | Phillips Petroleum Co | Biphenyl purification process by plural stage fractional distillation |
| JPH03106834A (en) * | 1989-09-19 | 1991-05-07 | Osaka Gas Co Ltd | Production of high-purity biphenyl |
| CN101045670A (en) * | 2006-03-29 | 2007-10-03 | 宝山钢铁股份有限公司 | Process for purifying biphenyl |
| CN101182277A (en) * | 2007-12-14 | 2008-05-21 | 鞍钢股份有限公司 | Method for extracting biphenyl from middle washing oil |
| CN100393677C (en) * | 2005-06-30 | 2008-06-11 | 天津大学 | Process for extracting 1-methylnaphthalene and 2-methylnaphthalene from tar |
| CN101245044A (en) * | 2007-02-16 | 2008-08-20 | 宝山钢铁股份有限公司 | Method for extracting biphenyl and indole from coal tar recovered wash oil |
| CN101328105A (en) * | 2007-06-22 | 2008-12-24 | 宝山钢铁股份有限公司 | Process for purifying biphenyl by rectification-emulsification crystallization method |
| CN101516809A (en) * | 2006-10-16 | 2009-08-26 | 东丽精密化学株式会社 | Method for producing biphenyl derivative |
| CN101912693A (en) * | 2010-07-29 | 2010-12-15 | 河南宝硕焦油化工有限公司 | Equipment and method for separating indole and biphenyl from wash oil fraction |
| CN102268273A (en) * | 2011-07-18 | 2011-12-07 | 辽宁科技学院 | Deep processing technology for coking wash oil |
| US20160280616A1 (en) * | 2015-03-25 | 2016-09-29 | Exxonmobil Chemical Patents Inc. | Production of Biphenyl Compounds |
| CN107129422A (en) * | 2016-02-28 | 2017-09-05 | 华东理工大学 | The continuous distillation method of high-purity biphenyl is extracted in a kind of tower first raffinate from crude benzol |
| CN108395362A (en) * | 2017-02-08 | 2018-08-14 | 鞍钢股份有限公司 | A method of extracting biphenyl using heat carrier heating negative pressure rectifying |
-
2018
- 2018-09-29 CN CN201811150688.6A patent/CN109053355B/en active Active
Patent Citations (13)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3700566A (en) * | 1969-10-13 | 1972-10-24 | Phillips Petroleum Co | Biphenyl purification process by plural stage fractional distillation |
| JPH03106834A (en) * | 1989-09-19 | 1991-05-07 | Osaka Gas Co Ltd | Production of high-purity biphenyl |
| CN100393677C (en) * | 2005-06-30 | 2008-06-11 | 天津大学 | Process for extracting 1-methylnaphthalene and 2-methylnaphthalene from tar |
| CN101045670A (en) * | 2006-03-29 | 2007-10-03 | 宝山钢铁股份有限公司 | Process for purifying biphenyl |
| CN101516809A (en) * | 2006-10-16 | 2009-08-26 | 东丽精密化学株式会社 | Method for producing biphenyl derivative |
| CN101245044A (en) * | 2007-02-16 | 2008-08-20 | 宝山钢铁股份有限公司 | Method for extracting biphenyl and indole from coal tar recovered wash oil |
| CN101328105A (en) * | 2007-06-22 | 2008-12-24 | 宝山钢铁股份有限公司 | Process for purifying biphenyl by rectification-emulsification crystallization method |
| CN101182277A (en) * | 2007-12-14 | 2008-05-21 | 鞍钢股份有限公司 | Method for extracting biphenyl from middle washing oil |
| CN101912693A (en) * | 2010-07-29 | 2010-12-15 | 河南宝硕焦油化工有限公司 | Equipment and method for separating indole and biphenyl from wash oil fraction |
| CN102268273A (en) * | 2011-07-18 | 2011-12-07 | 辽宁科技学院 | Deep processing technology for coking wash oil |
| US20160280616A1 (en) * | 2015-03-25 | 2016-09-29 | Exxonmobil Chemical Patents Inc. | Production of Biphenyl Compounds |
| CN107129422A (en) * | 2016-02-28 | 2017-09-05 | 华东理工大学 | The continuous distillation method of high-purity biphenyl is extracted in a kind of tower first raffinate from crude benzol |
| CN108395362A (en) * | 2017-02-08 | 2018-08-14 | 鞍钢股份有限公司 | A method of extracting biphenyl using heat carrier heating negative pressure rectifying |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111018652A (en) * | 2019-12-15 | 2020-04-17 | 江苏曼拓化学有限公司 | Preparation method of high-purity hydrogenated terphenyl heat conduction oil |
| CN111530114A (en) * | 2020-06-16 | 2020-08-14 | 上海化工研究院有限公司 | Rectification system, semi-continuous rectification method and application thereof |
| CN111659149A (en) * | 2020-06-16 | 2020-09-15 | 上海化工研究院有限公司 | Rectifying tower, rectifying system and application thereof |
| CN111659149B (en) * | 2020-06-16 | 2021-10-08 | 上海化工研究院有限公司 | Rectifying tower, rectifying system and application thereof |
| CN113144655A (en) * | 2021-04-28 | 2021-07-23 | 安徽金轩科技有限公司 | Jiale musk rectification unit and rectification process thereof |
| CN113636908A (en) * | 2021-08-13 | 2021-11-12 | 涉县津东经贸有限责任公司 | Terphenyl composition and preparation method thereof |
| CN114149299A (en) * | 2021-12-08 | 2022-03-08 | 涉县津东经贸有限责任公司 | Preparation method of biphenyl |
Also Published As
| Publication number | Publication date |
|---|---|
| CN109053355B (en) | 2020-12-25 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109053355A (en) | A kind of method of continuous rectification biphenyl purification | |
| CN107739300A (en) | A kind of process for producing high-purity isobutene and ethylene glycol mono-tert-butyl ether | |
| CN101225025B (en) | Method for separating catechol/hydroquinone from phenol hydroxylation reaction solution | |
| CN107739301B (en) | Polymethoxy dimethyl ether synthesis system and process | |
| CN110003007A (en) | Coal-ethylene glycol carbonylation dimethyl oxalate rectifying and purifying system and method | |
| CN105399590A (en) | Method for preparing dicyclopentadiene through gas-liquid phase depolymerization of C9 raw material | |
| CN101613248B (en) | Method for preparing cyclopentadiene by thermaldepolymerization of dicyclopentadiene | |
| CN111377802A (en) | Preparation method and system of sec-butyl alcohol | |
| CN109745723B (en) | Double-tower continuous feed rectification system and control method | |
| CN103073437B (en) | Preparation method of N-methyl diethanolamine | |
| CN114380784A (en) | Method and device for preparing electronic grade propylene carbonate by rectification and melt crystallization coupling | |
| CN110280038B (en) | Titanium tetrachloride rectifying device | |
| CN114797145B (en) | Differential pressure thermal coupling rectification process for coal-to-ethylene glycol byproduct | |
| CN101531400B (en) | Method for preparing antimony pentafluoride | |
| CN115779472A (en) | Refining method and rectifying device for crude butanol in 1, 4-butanediol production | |
| CN215886949U (en) | Ultrawhite stearic acid production device with low iodine value | |
| CN110922347B (en) | Method for separating N-methyl pyrrolidone from large-amount chloroform system | |
| CN111807934B (en) | Preparation method of electronic-grade propylene glycol monomethyl ether and product obtained by preparation method | |
| CN210314061U (en) | Rectification and purification device for synthesizing dimethyl oxalate by carbonylation of coal-made ethylene glycol | |
| CN113233982A (en) | Device and method for obtaining high-purity methyl salicylate through continuous rectification and purification | |
| CN209226883U (en) | DMAC, glycerol purifying technique device in a kind of fiber industry waste liquid | |
| CN208776607U (en) | Acetic acid refining and entrainer regenerating unit in polyvinyl alcohol disposing mother liquor unit | |
| CN201981139U (en) | Novel pure benzene producing device | |
| CN112409181A (en) | Dimethyl oxalate rectifying device for coal chemical industry | |
| CN215162247U (en) | Propylene recovery device of epoxypropane styrene coproduction system |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |