CN109053355B - Method for purifying biphenyl by continuous rectification - Google Patents
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Abstract
The invention relates to a method for purifying biphenyl by continuous rectification, which comprises the steps of enabling a raw material liquid to pass through a debenzolization tower, a biphenyl tower and a terphenyl tower which are connected in series, adding the raw material liquid from the middle part of the debenzolization tower, extracting a small amount of hydrogen, benzene and biphenyl from the top of the debenzolization tower, and extracting the residual biphenyl, a terphenyl mixture and trinitrol from a tower kettle to enter the biphenyl tower; a small amount of biphenyl mixture containing benzene is extracted from the top of the biphenyl tower and returned to the reaction liquid storage tank, high-purity biphenyl is extracted from the side line, and terphenyl and Sandu tar mixture extracted from the tower bottom enters the terphenyl tower; a small amount of biphenyl mixture containing terphenyl is extracted from the top of the terphenyl tower and returns to the feed inlet of the biphenyl tower, a high-purity terphenyl mixture is extracted from the side line, and a heavy component Sandu tar is extracted from the bottom of the terphenyl tower. By arranging side line extraction, the high-purity biphenyl product with the mass fraction of more than 99.9 percent can be obtained while being suitable for large-scale production and high in operation elasticity, and compared with the traditional intermittent process, the high-purity biphenyl product has the advantages that the energy consumption per unit product can be reduced by 30-40 percent, and the high-purity biphenyl product has extremely high economic value.
Description
Technical Field
The invention relates to the field of chemical industry, in particular to a method for purifying biphenyl by continuous rectification.
Background
Biphenyl is an important organic raw material and is widely used in the fields of medicines, pesticides, dyes, liquid crystal materials and the like. Can be used for synthesizing plasticizer and antiseptic, and can also be used for producing fuel, engineering plastics and high-energy fuel, etc. Biphenyl is present in coal tar, crude oil, and natural gas. The biphenyl synthesized chemically at present can produce a byproduct of terphenyl, hydrogenated terphenyl can be obtained by hydrogenation of the terphenyl, and the hydrogenated terphenyl is widely applied to industries such as petrochemical industry, synthetic fibers, synthetic resins, medicines, printing and dyeing and the like, high-temperature heat conduction and heat supply equipment systems, chemical fiber polymerization (terylene, chinlon polymerization and dry spandex spinning), organic silicon monomer synthesis, fine chemical industry such as trichlorosilane, polysilicon, medicines, pesticides and dye intermediates and biodiesel.
The biphenyl is prepared by a chemical synthesis method for preparing biphenyl by benzene pyrolysis and a separation and extraction method for preparing biphenyl by various coal tar fractions. The mass fraction of biphenyl in coal tar is only 0.20-0.40%, and the extraction cost is high. The chemical synthesis method has the advantages of controllable process, good product quality and higher conversion rate. The mainstream technology of the existing chemical synthesis method is a 'tubular method', namely benzene steam is introduced into a red hot pipeline (above 700 ℃) to prepare biphenyl by combining 2 benzene molecules with each other without a hydrogen atom, the reaction process can generate by-products of terphenyl and santa tar, the existing chemical synthesis method mainly adopts an intermittent rectification method for purification, corresponding products are obtained by adjusting the extraction amount, the operation pressure and the reflux ratio, and because all the towers are rectification sections during intermittent rectification and do not have a stripping section, the same products consisting of the tower top and the tower bottom are obtained, and the energy consumption of the intermittent rectification is larger than that of the continuous rectification; meanwhile, the batch method has long single batch processing time, which leads to low productivity; because the batch distillation tower is a stripping section, the components are not cut thoroughly, so that the product yield is low, and the batch distillation tower is not suitable for large-scale production.
Chinese patent CN107129422A discloses a continuous rectification method for extracting high-purity biphenyl from crude benzene tower A raffinate, which adopts a three-tower series process of high-efficiency filler rectification towers to further deeply process and separate raffinate (called as A raffinate) after extracting light components such as benzene, toluene and the like from a crude benzene tower in a coal tar hydrogenation process to obtain mixed xylene, naphthalene components and high-purity biphenyl products.
Disclosure of Invention
The invention aims to solve the problems and provide a method for purifying biphenyl by continuous rectification.
The purpose of the invention is realized by the following technical scheme:
a method for purifying biphenyl by continuous rectification comprises the following steps of enabling a raw material liquid to pass through three rectifying towers which are sequentially connected in series, wherein the three rectifying towers are a debenzolization tower, a biphenyl tower and a terphenyl tower respectively, the debenzolization tower is a normal-pressure or negative-pressure rectifying tower, the biphenyl tower and the terphenyl tower are high-vacuum negative-pressure rectifying towers, a side line extraction mode is adopted, and the specific process comprises the following steps:
(1) raw material liquid is added from the middle part of the debenzolization tower, a small amount of hydrogen, benzene and biphenyl are extracted from the top of the debenzolization tower, and the rest biphenyl, terphenyl mixture and santa tar oil extracted from the tower kettle enter a biphenyl tower;
(2) a small amount of biphenyl mixture containing benzene is extracted from the top of the biphenyl tower and returned to the reaction liquid storage tank, high-purity biphenyl is extracted from the side line, and terphenyl and Sandu tar mixture extracted from the tower bottom enters the terphenyl tower;
(3) a small amount of biphenyl mixture containing terphenyl is extracted from the top of the terphenyl tower and returns to the feed inlet of the biphenyl tower, a high-purity terphenyl mixture is extracted from the side line, and a heavy component Sandu tar is extracted from the bottom of the terphenyl tower.
Further, the middle part of the debenzolization tower is communicated with a reaction liquid storage tank, a top gas discharge is connected with a hydrogen tank, a top liquid discharge is connected with a benzene storage tank, and a tower kettle discharge is communicated with a biphenyl tower;
a top extraction pipe of the biphenyl tower is communicated with a benzene-biphenyl intermediate tank, the benzene-biphenyl intermediate tank is communicated with a reaction liquid storage tank, a side line of the biphenyl tower is communicated with a biphenyl product storage tank, and a tower kettle discharge is communicated with the terphenyl tower;
the top extraction pipe of the terphenyl tower is communicated with a biphenyl-terphenyl intermediate tank, the biphenyl-terphenyl intermediate tank is connected with a feed inlet of the terphenyl tower, the lateral line of the terphenyl tower is communicated with a terphenyl product storage tank, and the tower kettle discharge is communicated with a Sandu tar storage tank.
Further, the operation pressure of the top of the debenzolization tower is 20-120kPa, preferably 80-101 kPa; the operation pressure of the top of the biphenyl tower is 0.1-10kPa, preferably 0.5-5 kPa; the pressure at the top of the terphenyl column is in the range of 0.05 to 8kPa, preferably 0.1 to 4 kPa.
Further, the operation temperature of the top of the debenzolization tower is 60-120 ℃, preferably 70-108 ℃, the operation temperature of the bottom of the debenzolization tower is 200-300 ℃, preferably 265-285 ℃;
the operation temperature of the top of the biphenyl tower is 80-130 ℃, preferably 90-112 ℃, the operation temperature of the lateral line discharge port is 90-140 ℃, preferably 100-;
the top operating temperature of the terphenyl tower is 150-200 ℃, preferably 165-185 ℃, the side outlet operating temperature is 200-250 ℃, preferably 215-235 ℃, and the bottom operating temperature is 280-450 ℃, preferably 300-400 ℃.
Further, the reflux ratio of the debenzolization tower is 0.01-5, preferably 0.02-2; the reflux ratio of the biphenyl tower is 0.5-10, preferably 1-6; the reflux ratio of the terphenyl column is from 0.1 to 8, preferably from 1 to 5.
Further, the side line production position of the biphenyl tower is located at 1/40-2/3, preferably 1/10-3/5 of the tower from top to bottom; the side-draw position of the terphenyl tower is 1/30-2/3, preferably 1/15-3/5 of the tower, the side-draw position must be in the described range, otherwise, the content of light component benzene in the biphenyl product exceeds the standard, and the high-purity biphenyl product cannot be obtained.
Further, the number of trays of the debenzolization tower is 3 to 30, preferably 5 to 20; the number of the trays of the biphenyl tower is 20-90, preferably 30-80; the trays of the terphenyl column are 10 to 60, preferably 20 to 50.
Furthermore, efficient separation packing is filled in the debenzolization tower, the biphenyl tower and the terphenyl tower, and comprises plate corrugations, plate nets, wire mesh regular packing or efficient random packing.
Further, the reboiler of the tower kettle of the debenzolization tower adopts a conventional reboiler to provide steam, the tower kettles of the biphenyl tower and the terphenyl tower adopt a heating furnace to directly heat, the condenser at the top of the debenzolization tower adopts water cooling, and the condenser at the top of the biphenyl tower and the terphenyl tower adopts heat conduction oil cooling.
Further, the surfaces of the pipelines for connection in the device are wound with high-temperature heat tracing bands.
The invention adopts continuous three-tower rectification to separate and purify biphenyl, takes benzene high-temperature dehydrogenation reaction liquid as a raw material, combines the mode of two-tower side line extraction through continuous precise rectification separation, is suitable for large-scale production, has large operation flexibility, can obtain a high-purity biphenyl product with the mass fraction of more than 99.9 percent, has the yield of more than 93 percent, and has extremely high economic value because the energy consumption of unit product can be reduced by 30 to 40 percent compared with the traditional intermittent process.
Drawings
FIG. 1 is a schematic diagram of a continuous rectification method for purifying biphenyl according to the present invention;
FIG. 2 is a schematic diagram of a process for purifying biphenyl by continuous rectification in comparative example 1;
FIG. 3 is a schematic diagram of a process for purifying biphenyl by continuous rectification in comparative example 2;
FIG. 4 is a schematic diagram of a process for purifying biphenyl by continuous rectification in comparative example 3;
in the figure, V101-waste stripping solution storage tank; p1-first delivery pump; p2-second delivery pump; p3-third transfer pump; p4-fourth delivery pump; CW 1-condensation of water; CW 2-condensation of water; HWS 2-hot condensate return water; HWR 2-hot condensate return water; t1-debenzolization column; t2-biphenyl column; t3-terphenyl column; e101-a reboiler of a debenzolization column; e102-a debenzolization tower condenser; e103-biphenyl tower heating furnace type reboiler; e104-biphenyl tower condenser; e105-terphenyl tower heating furnace reboiler; e106-terphenyl column condenser.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.
A device for purifying biphenyl by continuous rectification comprises three debenzolization towers, a biphenyl tower and a terphenyl tower which are sequentially connected in series, wherein the middle part of the debenzolization tower is communicated with a reaction liquid storage tank through a pipeline, a gas discharge material at the top of the tower is connected with a hydrogen tank through a pipeline, a liquid discharge material is connected with the benzene storage tank, and a tower kettle discharge material is communicated with the biphenyl tower through a pipeline; the extraction pipe at the top of the biphenyl tower is communicated with a benzene-biphenyl intermediate tank, the intermediate tank is communicated with a reaction liquid tank through a pipeline, the lateral line of the biphenyl tower is communicated with a biphenyl product storage tank, and the discharge of the tower kettle is communicated with the terphenyl tower through a pipeline; the top extraction pipe of the terphenyl tower is communicated with a biphenyl-terphenyl intermediate tank, the intermediate tank is connected with a feed inlet of the biphenyl tower through a pipeline, the lateral line of the terphenyl tower is communicated with a terphenyl product storage tank, and the discharge of the tower kettle is communicated with a Sandu tar storage tank through a pipeline; the biphenyl tower and the kettle of the terphenyl tower are directly heated by a heating furnace.
The debenzolization tower is an atmospheric pressure tower or a negative pressure tower, the operation pressure at the top of the tower is 20-120kPa, preferably 80-101kPa, the operation temperature at the top of the tower is 60-120 ℃, preferably 70-108 ℃, the operation temperature at the bottom of the tower is 200-300 ℃, preferably 265-285 ℃, the reflux ratio is 0.01-5, preferably 0.02-2, and the number of tower plates is 3-30, preferably 5-20; the biphenyl tower is a negative pressure side-draw tower, the operation pressure at the top of the tower is 0.1-10kPa, preferably 0.5-5kPa, the operation temperature at the top of the tower is 80-130 ℃, preferably 90-112 ℃, the operation temperature at a side-draw discharge port is 90-140 ℃, preferably 100-; the terphenyl tower is a negative pressure side-draw tower, the operation pressure at the top of the terphenyl tower is 0.05-8kPa, the preferable 0.1-4kPa that the operation temperature at the top of the terphenyl tower is 150-.
The high-efficiency separation packing is filled in the debenzolization tower, the biphenyl tower and the terphenyl tower, and comprises plate corrugation, plate mesh, silk screen regular packing or high-efficiency random packing. The side-draw of the biphenyl column is from 1/40 to 2/3, preferably from 1/10 to 3/5, from top to bottom of the column, and the side-draw of the terphenyl column is from 1/30 to 2/3, preferably from 1/15 to 3/5, from top to bottom of the column.
A reboiler of a tower kettle of the debenzolization tower adopts a conventional reboiler to provide steam, a heating furnace is needed to provide steam for the biphenyl tower and the terphenyl tower, and heating media of the reboiler of the three towers all adopt high-temperature heat conduction oil. The condenser at the top of the debenzolization tower is cooled by water, and the condensers at the tops of the biphenyl tower and the terphenyl tower are cooled by heat-conducting oil. In order to ensure continuous and stable operation of production, the extraction pipe of the tower kettle of the debenzolization tower, the extraction pipe of the tower top of the biphenyl tower, the extraction pipe of the tower kettle of the biphenyl tower, the extraction pipe of the tower top of the terphenyl tower and the extraction pipe of the tower kettle of the terphenyl tower are all required to be insulated and wound with a high-temperature tracing band.
The method for purifying biphenyl by adopting the device comprises the following steps: raw material liquid is added from the middle part of the debenzolization tower, a small amount of hydrogen, benzene and biphenyl are extracted from the top of the debenzolization tower, and the rest biphenyl, terphenyl mixture and santa tar oil extracted from the tower kettle enter a biphenyl tower; the biphenyl tower is a high vacuum negative pressure rectifying tower, a side line extraction mode is adopted, a small amount of biphenyl mixture containing benzene is extracted from the tower top and returns to a reaction liquid storage tank, high-purity biphenyl is extracted from the side line, and a mixture of terphenyl and trinary tar oil extracted from the tower bottom enters the terphenyl tower; the terphenyl tower is a high vacuum negative pressure rectifying tower, a side line extraction mode is adopted, a small amount of biphenyl mixture containing terphenyl is extracted from the top of the tower and returns to a feed inlet of the terphenyl tower, a high-purity terphenyl mixture is extracted from the side line, and the bottom of the tower is heavy component Sandu tar.
The following are more specific embodiments.
Example 1
The flow chart of the method is shown in figure 1, the raw material liquid comprises 0.25 wt% of hydrogen, 65 wt% of benzene, 25 wt% of biphenyl, 7.75 wt% of mixed terphenyl and 2 wt% of santal tar, the raw material liquid contained in a raw material liquid storage tank V101 is fed from the middle part of a debenzolization tower T1 through a first conveying pump P1, the operation pressure at the top of the debenzolization tower T1 is normal pressure, the theoretical stages are 8, and the reflux ratio is 0.03. The bottom of the debenzolization tower T1 is provided with a debenzolization tower reboiler E101, the top of the tower is provided with a debenzolization tower condenser E102, the debenzolization tower condenser E102 is treated by condensed upper water CW1 and condensed return water HW1, the top of the tower is extracted with non-condensable gas hydrogen from the top of the condenser, part of the condensed liquid reflows to the debenzolization tower T1, and the other part is discharged. The mixed liquid obtained from the bottom of the debenzolization tower T1 is conveyed to the middle part of a biphenyl tower T2 through a second conveying pump P2, the operation pressure at the top of the biphenyl tower T2 is 1kPa, the theoretical stage number is 50, the side line discharging position is at the 5 th theoretical stage (from top to bottom), and the reflux ratio is 3. A direct heating furnace reboiler E103 is arranged at the bottom of the biphenyl tower T2, a biphenyl tower condenser E104 is arranged at the top of the biphenyl tower, the biphenyl tower condenser E104 is treated by hot condensed upper water HWS2 and hot condensed return water HWR2, most of the condensed liquid at the top of the biphenyl tower returns to the biphenyl tower T2, a small part of the condensed liquid at the top of the biphenyl tower is extracted, and a large amount of high-purity biphenyl products are extracted at a side line extraction port. The mixed liquid at the bottom of the terphenyl tower T2 is conveyed to the middle part of a terphenyl tower T3 through a third conveying pump P3, the operation pressure at the top of the terphenyl tower T3 is 1kPa, the theoretical stage number is 30, the side line discharging position is at the 5 th theoretical stage (from top to bottom), and the reflux ratio is 2. A direct heating furnace reboiler E105 is arranged at the bottom of the terphenyl tower T3, a terphenyl tower condenser E106 is arranged at the top of the terphenyl tower, the terphenyl tower condenser E106 is treated by heat conduction hot oil, most of condensate liquid at the top of the terphenyl tower returns to the terphenyl tower T3, a small part of condensate liquid is extracted, a large amount of terphenyl products are extracted at a side line extraction outlet, and the trinary tar oil extracted from the bottom of the terphenyl tower T3 is conveyed to a storage tank through a fourth conveying pump P4. Through three-tower continuous rectification separation, the purity of biphenyl reaches 99.99 wt%, and the yield is 93%.
Example 2
The flow chart of the new method is shown in figure 1, the raw material liquid comprises 0.25 wt% of hydrogen, 65 wt% of benzene, 25 wt% of biphenyl, 7.75 wt% of mixed terphenyl and 2 wt% of santal tar, the raw material liquid is fed from the middle of a debenzolization tower T1 through a first conveying pump P1, the operation pressure of the top of the debenzolization tower T1 is normal pressure, the theoretical stage number is 10, the reflux ratio is 0.05, the mixed liquid obtained from the bottom of the debenzolization tower T1 is conveyed to the middle of the biphenyl tower T2 through a pump, the operation pressure of the top of the biphenyl tower T2 is 3kPa, the theoretical stage number is 60, the side line discharge position is 15 theoretical stage (counted from top to bottom), the reflux ratio is 2, the mixed liquid obtained from the bottom of the biphenyl tower T2 is conveyed to the middle of the terphenyl tower T3 through a pump, the operation pressure of the top of the terphenyl tower T3 is 3kPa, the theoretical stage number is 40, the side line discharge position is. Through three-tower continuous rectification separation, the purity of biphenyl reaches 99.92 wt%, and the yield is 97%.
Comparative example 1
The new method of the invention is shown in a flow chart of a figure 2, raw material liquid comprises 0.25 wt% of hydrogen, 65 wt% of benzene, 25 wt% of biphenyl, 7.75 wt% of mixed terphenyl and 2 wt% of tar, the raw material liquid is fed from the middle part of a debenzolization tower T1 through a first conveying pump P1, the operation pressure of the top of a debenzolization tower T1 is normal pressure, the theoretical stage number is 15, the reflux ratio is 0.1, mixed liquid obtained from the bottom of a debenzolization tower T1 is conveyed to the middle part of a biphenyl tower T2 through a pump, the operation pressure of the top of a biphenyl tower T2 is 2kPa, the theoretical stage number is 60, the reflux ratio is 1, the mixed liquid obtained from the bottom of a biphenyl tower T2 is conveyed to the middle part of a terphenyl tower T3 through a pump, the operation pressure of the top of a terphenyl tower T3. Through three-tower continuous rectification separation, the purity of biphenyl reaches 98.21 wt%, and the yield is 81%.
Comparative example 2
The flow chart of the novel method is shown in figure 3, the raw material liquid comprises 0.25 wt% of hydrogen, 65 wt% of benzene, 25 wt% of biphenyl, 7.75 wt% of mixed terphenyl and 2 wt% of santal tar, the raw material liquid is fed from the middle of a debenzolization tower T1 through a first conveying pump P1, the operation pressure of the top of the debenzolization tower T1 is normal pressure, the theoretical stage number is 25, the reflux ratio is 0.05, the mixed liquid obtained from the bottom of the debenzolization tower T1 is conveyed to the middle of the biphenyl tower T2 through a pump, the operation pressure of the top of the biphenyl tower T2 is 4kPa, the theoretical stage number is 70, the side-draw discharging position is 20 theoretical stages (counted from top to bottom), the reflux ratio is 2.5, the mixed liquid obtained from the bottom of the biphenyl tower T2 is conveyed to the middle of the terphenyl tower T3 through a pump, the operation pressure of the top of the terphenyl tower T3 is 4 kPa. Through three-tower continuous rectification separation, the purity of biphenyl reaches 99.7 wt%, and the yield is 86%.
Comparative example 3
The flow chart of the novel method is shown in figure 4, the raw material liquid comprises 0.25 wt% of hydrogen, 65 wt% of benzene, 25 wt% of biphenyl, 7.75 wt% of mixed terphenyl and 2 wt% of santal tar, the raw material liquid is fed from the middle of a debenzolization tower T1 through a first conveying pump P1, the operation pressure of the top of the debenzolization tower T1 is normal pressure, the theoretical stage number is 25, the reflux ratio is 0.05, the mixed liquid obtained from the bottom of the debenzolization tower T1 is conveyed to the middle of the biphenyl tower T2 through a pump, the operation pressure of the top of the biphenyl tower T2 is 5kPa, the theoretical stage number is 80, the reflux ratio is 4, the mixed liquid obtained from the bottom of the biphenyl tower T2 is conveyed to the middle of the terphenyl tower T3 through a pump, the operation pressure of the top of the terphenyl tower T3 is 8kPa, the theoretical stage number is 45, the side line discharging position is the. Through three-tower continuous rectification separation, the purity of biphenyl reaches 99.03 wt%, and the yield is 84%.
According to the invention, through continuous precise rectification separation and combination of a two-tower side-line extraction form, a high-purity biphenyl product with the mass fraction of more than 99.9% can be obtained, and the yield is more than 93%.
The foregoing description of specific embodiments of the present invention has been presented. It is to be understood that the present invention is not limited to the specific embodiments described above, and that various changes and modifications may be made by one skilled in the art within the scope of the appended claims without departing from the spirit of the invention.
Claims (15)
1. The method for purifying biphenyl by continuous rectification is characterized in that a raw material liquid passes through three rectifying towers which are sequentially connected in series, wherein the three rectifying towers are a debenzolization tower, a biphenyl tower and a terphenyl tower respectively, the debenzolization tower is a normal-pressure or negative-pressure rectifying tower, the biphenyl tower and the terphenyl tower are high-vacuum negative-pressure rectifying towers, a side line extraction mode is adopted, and the specific process is as follows:
(1) raw material liquid is added from the middle part of the debenzolization tower, a small amount of hydrogen, benzene and biphenyl are extracted from the top of the debenzolization tower, and the rest biphenyl, terphenyl mixture and santa tar oil extracted from the tower kettle enter a biphenyl tower;
(2) a small amount of biphenyl mixture containing benzene is extracted from the top of the biphenyl tower and returned to the reaction liquid storage tank, high-purity biphenyl is extracted from the side line, and terphenyl and Sandu tar mixture extracted from the tower bottom enters the terphenyl tower;
(3) a small amount of biphenyl mixture containing terphenyl is extracted from the top of the terphenyl tower and returns to the feed inlet of the biphenyl tower, a high-purity terphenyl mixture is extracted from the side line, and a heavy component Sandu tar is extracted from the bottom of the terphenyl tower.
2. The method for purifying biphenyl by continuous rectification according to claim 1, wherein the middle part of the debenzolization tower is communicated with a reaction liquid storage tank, the top gas discharge is connected with a hydrogen tank, the top liquid discharge is connected with a benzene storage tank, and the tower bottom discharge is communicated with the biphenyl tower;
a top extraction pipe of the biphenyl tower is communicated with a benzene-biphenyl intermediate tank, the benzene-biphenyl intermediate tank is communicated with a reaction liquid storage tank, a side line of the biphenyl tower is communicated with a biphenyl product storage tank, and a tower kettle discharge is communicated with the terphenyl tower;
the top extraction pipe of the terphenyl tower is communicated with a biphenyl-terphenyl intermediate tank, the biphenyl-terphenyl intermediate tank is connected with a feed inlet of the terphenyl tower, the lateral line of the terphenyl tower is communicated with a terphenyl product storage tank, and the tower kettle discharge is communicated with a Sandu tar storage tank.
3. The method for purifying biphenyl by continuous distillation according to claim 1, wherein the operating pressure of the top of the debenzolization tower is 20-120 kPa; the operation pressure at the top of the biphenyl tower is 0.1-10 kPa; the operation pressure at the top of the terphenyl tower is 0.05-8 kPa.
4. The method for purifying biphenyl by continuous distillation according to claim 3, wherein the operation pressure of the top of the debenzolization tower is 80-101 kPa; the operation pressure at the top of the biphenyl tower is 0.5-5 kPa; the top operating pressure of the terphenyl tower is 0.1-4 kPa.
5. The method for purifying biphenyl by continuous distillation as claimed in claim 1, wherein the tower top operating temperature of the debenzolization tower is 60-120 ℃, the tower bottom operating temperature is 200-300 ℃;
the operation temperature of the top of the biphenyl tower is 80-130 ℃, the operation temperature of the lateral line discharge port is 90-140 ℃, and the operation temperature of the tower kettle is 180-;
the top operating temperature of the terphenyl tower is 150-200 ℃, the side line discharge port operating temperature is 200-250 ℃, and the tower kettle operating temperature is 280-450 ℃.
6. The method for purifying biphenyl by continuous distillation as claimed in claim 5, wherein the tower top operating temperature of the debenzolization tower is 70-108 ℃, and the tower bottom operating temperature is 265-285 ℃;
the operation temperature of the top of the biphenyl tower is 90-112 ℃, the operation temperature of the lateral line discharge port is 100-122 ℃, and the operation temperature of the bottom of the biphenyl tower is 200-300 ℃;
the top operating temperature of the terphenyl tower is 165-185 ℃, the side line discharge port operating temperature is 215-235 ℃, and the tower kettle operating temperature is 300-400 ℃.
7. The method for purifying biphenyl by continuous distillation as claimed in claim 1, wherein the reflux ratio of the debenzolization tower is 0.01-5; the reflux ratio of the biphenyl tower is 0.5-10; the reflux ratio of the terphenyl tower is 0.1-8.
8. The method for purifying biphenyl by continuous distillation as claimed in claim 7, wherein the reflux ratio of the debenzolization tower is 0.02-2; the reflux ratio of the biphenyl tower is 1-6; the reflux ratio of the terphenyl tower is 1-5.
9. The continuous rectification purification method for biphenyl according to claim 1, wherein the side line extraction position of the biphenyl tower is 1/40-2/3 from top to bottom; the side draw of the terphenyl column is at 1/30-2/3 of the column.
10. The continuous rectification purification method for biphenyl according to claim 9, wherein the side line extraction position of the biphenyl tower is 1/10-3/5 from top to bottom; the side draw of the terphenyl column is at 1/15-3/5 of the column.
11. The method for purifying biphenyl by continuous distillation according to claim 1, wherein the number of the tower plates of the debenzolization tower is 3-30; the number of the tower plates of the biphenyl tower is 20-90; the terphenyl tower has 10-60 trays.
12. The method for purifying biphenyl by continuous distillation according to claim 11, wherein the number of the tower plates of the debenzolization tower is 5-20; the number of the tower plates of the biphenyl tower is 30-80; the terphenyl tower has 20-50 trays.
13. The method for purifying biphenyl by continuous distillation as claimed in claim 1, wherein the debenzolization tower, the biphenyl tower and the terphenyl tower are filled with high-efficiency separation packing comprising plate corrugation, plate mesh, wire mesh structured packing or high-efficiency random packing.
14. The method for continuous distillation purification of biphenyl according to claim 1, wherein a reboiler at the bottom of the debenzolization tower is provided with steam by using a conventional reboiler, the bottoms of the biphenyl tower and the terphenyl tower are directly heated by using a heating furnace, a condenser at the top of the debenzolization tower is water-cooled, and condensers at the top of the biphenyl tower and the terphenyl tower are cold by using heat conducting oil.
15. The method for purifying biphenyl by continuous distillation as claimed in claim 1, wherein the surfaces of the pipes for connection are wound with high temperature heat tracing band.
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| 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 |
| CN113559817B (en) * | 2020-06-16 | 2022-10-14 | 上海化工研究院有限公司 | Corrugated wire mesh sheet for forming structured packing, structured packing and rectifying tower |
| 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 |
| CN113144655B (en) * | 2021-04-28 | 2022-06-21 | 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 |
| CN114149299B (en) * | 2021-12-08 | 2023-07-11 | 涉县津东经贸有限责任公司 | Preparation method of biphenyl |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| CN100473631C (en) * | 2006-03-29 | 2009-04-01 | 宝山钢铁股份有限公司 | Process for purifying biphenyl |
| JP5210639B2 (en) * | 2006-10-16 | 2013-06-12 | 民生 林 | Method for producing biphenyl derivative |
| CN101245044B (en) * | 2007-02-16 | 2011-01-19 | 宝山钢铁股份有限公司 | Method for extracting biphenyl and indole from coal tar recovered wash oil |
| CN101328105B (en) * | 2007-06-22 | 2011-07-20 | 宝山钢铁股份有限公司 | Process for purifying biphenyl by rectification-emulsification crystallization method |
| CN101182277B (en) * | 2007-12-14 | 2010-04-14 | 鞍钢股份有限公司 | Method for extracting biphenyl from medium wash oil |
| CN101912693B (en) * | 2010-07-29 | 2012-08-22 | 河南宝硕焦油化工有限公司 | Equipment and method for separating indole and biphenyl from wash oil fraction |
| CN102268273B (en) * | 2011-07-18 | 2013-09-11 | 辽宁科技学院 | Deep processing technology for coking wash oil |
| US9708230B2 (en) * | 2015-03-25 | 2017-07-18 | 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 | Method for extracting biphenyl by heating heat carrier and performing negative pressure rectification |
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