CN116272713A - Device and method for recycling alpha-methylstyrene by cracking phenol tar - Google Patents
Device and method for recycling alpha-methylstyrene by cracking phenol tar Download PDFInfo
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- CN116272713A CN116272713A CN202211104505.3A CN202211104505A CN116272713A CN 116272713 A CN116272713 A CN 116272713A CN 202211104505 A CN202211104505 A CN 202211104505A CN 116272713 A CN116272713 A CN 116272713A
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- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
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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
- B01D3/009—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping in combination with chemical reactions
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C1/00—Preparation of hydrocarbons from one or more compounds, none of them being a hydrocarbon
- C07C1/20—Preparation of hydrocarbons from one or more compounds, none of them being a hydrocarbon starting from organic compounds containing only oxygen atoms as heteroatoms
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- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/005—Processes comprising at least two steps in series
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- 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
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10C—WORKING-UP PITCH, ASPHALT, BITUMEN, TAR; PYROLIGNEOUS ACID
- C10C1/00—Working-up tar
- C10C1/04—Working-up tar by distillation
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- C—CHEMISTRY; METALLURGY
- C10—PETROLEUM, GAS OR COKE INDUSTRIES; TECHNICAL GASES CONTAINING CARBON MONOXIDE; FUELS; LUBRICANTS; PEAT
- C10C—WORKING-UP PITCH, ASPHALT, BITUMEN, TAR; PYROLIGNEOUS ACID
- C10C1/00—Working-up tar
- C10C1/20—Refining by chemical means inorganic or organic compounds
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Abstract
The invention relates to a device and a method for recycling alpha-methylstyrene by cracking phenol tar, wherein the device comprises a cracking reaction unit for carrying out cracking reaction on a phenol tar raw material, a crude product condenser with a feeding port connected with a gas phase discharge of the cracking reaction unit, a negative pressure heavy removal rectifying tower with a feeding port connected with a liquid phase discharge of the crude product condenser, and a negative pressure rectifying AMS product tower with a feeding port connected with a top discharge of the negative pressure heavy removal rectifying tower, wherein the top of the negative pressure rectifying AMS product tower is used for producing alpha-methylstyrene. Compared with the prior art, the invention adopts a method of controlling the reaction residence time by continuous direct thermal cracking, increases the reaction directionality and increases the recovery rate of the target product; on the other hand, the negative pressure rectification method is adopted, so that the continuous cracking of heavy components can be avoided, isopropylbenzene, AMS and the like can be separated from the heavy components by two towers, and the process flow is simple.
Description
Technical Field
The invention belongs to the technical field of petrochemical industry, and relates to a device and a method for recycling alpha-methylstyrene by cracking phenol tar.
Background
Phenol tar is a byproduct of the reaction for preparing phenol and acetone by taking cumene as a raw material, and is distillation residue after separating phenol and acetone from reaction products, and belongs to hazardous waste. The composition of phenol tar was approximately as follows: phenol 19.6%, acetophenone 12%, cumylphenol 21.6% and some other heavy components 48.8%. From the composition point of view, phenol tar contains more fine chemicals, and the fine chemicals have higher application value. However, the treatment of phenol tar in the current market does not maximize the value, and many phenol factories burn phenol tar, so that when the phenol tar is burnt, the phenol tar not only causes environmental pollution, but also wastes resources. Therefore, a method that maximizes recovery of useful products such as cumene, phenol, acetophenone, alpha-methylstyrene, etc. from phenol tar and reduces the amount of tar removed by combustion would be of great value.
Document CN1154399 discloses a phenol tar treatment process. The phenolic tar is thermally cracked under controlled conditions in the presence of polyphosphoric acid to recover valuable products. Adding phenol tar into a cylindrical reactor for thermal cracking treatment, heating the bottom of the reactor to 200-360 ℃, maintaining the reactor pressure at 0.1-5 atm, and dehydrating and polymerizing the pyrolysis tar into a non-volatile polyphosphoric acid analog by the added phosphoric acid in the presence of phosphoric acid preheated to 50-180 ℃ and having a weight percentage of 0.1-1.0, preferably 0.1-0.2%. Bisphenol A tar can be optionally used for mixing and cracking with tar under the condition, so that the product yield is improved. The literature is compared and analyzed, and the process adopts a catalytic cracking mode of the catalyst to obtain useful recoverable components, but the catalyst phosphoric acid is easy to polymerize to generate solid, and the bottom heavy component is easy to coke after catalytic cracking to influence the operation of equipment. The recovery process of the useful components is not described in the patent.
Document CN1137033 discloses co-cracking of bisphenol a and phenol process tar, and relates to a process for working up a tar mixture produced in the production of phenol and bisphenol by heating a column bottoms liquid obtained from the bisphenol a process and a phenol tar obtained from the cumene phenol process in a mass ratio of 1 (1) to (10) in a distillation column thermal cracking reaction at 290 ℃ to 360 ℃. The process is carried out by feeding into the middle of the column and withdrawing the valuable product from the top of the column. The literature was analyzed for comparison, the process is directed to phenol tar and bisphenol a tar obtained in the cumene phenol production process or a mixture of the two in any ratio, the valuable products (phenol, alpha-methylstyrene and cumene) that can be recycled are obtained by thermal cracking, phenol tar obtained by the cumene process route is not mentioned, and no recycling method or apparatus is mentioned in the patent.
Disclosure of Invention
The invention aims at solving the problem that phenol tar produced by a device for producing phenol by taking cumene as a raw material is difficult to treat, and provides a device and a method for recycling valuable substances alpha-methylstyrene by cracking the phenol tar.
The aim of the invention can be achieved by the following technical scheme:
a device for recycling alpha-methylstyrene by cracking phenol tar comprises
The cracking reaction unit is used for carrying out cracking reaction on the phenol tar raw material;
the feed inlet of the crude product condenser is connected with the gas phase discharge of the cracking reaction unit and is used for condensing to obtain a liquid phase crude product;
the feeding port of the negative pressure heavy removal rectifying tower is connected with the liquid phase discharging port of the crude product condenser, and the heavy removal rectifying liquid phase is extracted from the top of the negative pressure heavy removal rectifying tower; and
the feeding port of the negative pressure rectifying AMS product tower is connected with the discharging port of the top of the negative pressure heavy removal rectifying tower, and the alpha-methylstyrene is produced from the top of the negative pressure rectifying AMS product tower.
Further, the cracking reaction unit comprises a cracking reactor, an external circulation pump, a heater and a gas-liquid separator, wherein the external circulation pump, the heater and the gas-liquid separator are sequentially connected with a liquid phase discharge port of the cracking reactor;
the gas phase outlet of the gas-liquid separator is connected with the feed inlet of the crude product condenser, and the liquid phase outlet is connected with the cracking reactor.
Further, a pyrolysis liquid phase discharge port is also arranged on the connecting pipeline between the external circulation pump and the heater.
Further, a crude product collecting tank and a heavy-removal tower feeding pump are sequentially arranged between the crude product condenser and the negative pressure heavy-removal rectifying tower along the material flow direction;
the crude product collecting tank is provided with a crude product discharging port.
Further, a heavy component recovery pump is arranged between the tower bottom discharge port of the negative pressure heavy removal rectifying tower and the crude product condenser, and the tower bottom discharge of the negative pressure heavy removal rectifying tower returns to the cracking reaction unit after heat exchange between the crude product condenser and the gas phase discharge of the cracking reaction unit.
Further, a top condenser of the de-heavy rectifying tower and a top collecting tank of the de-heavy rectifying tower are connected in sequence at the top discharge port of the negative pressure de-heavy rectifying tower,
and a discharge hole of the top collecting tank of the de-weight tower is connected with a negative pressure rectifying AMS product tower.
Further, an AMS product tower feeding pump is arranged between the top collecting tank of the de-weight tower and the negative pressure rectifying AMS product tower.
A method for recovering alpha-methylstyrene by phenol tar cracking, comprising using the apparatus as described above, and comprising:
the phenol tar raw material is sent to a cracking reaction unit, the gas phase discharge is condensed by a crude product condenser and then sent to a negative pressure heavy removal rectifying tower, the gas phase discharge at the top of the tower is condensed and then sent to a negative pressure rectifying AMS product tower, and the product alpha-methyl styrene is obtained at the bottom of the tower.
Further, the method for recycling the alpha-methylstyrene by cracking the phenol tar comprises the following steps:
sending the phenol tar raw material to a cracking reactor, separating liquid phase discharge into two parts after passing through an external circulating pump, wherein one part is extracted, the other part is heated by a heater and then enters a gas-liquid separator, the liquid phase discharge of the gas-liquid separator returns to the cracking reactor, and after the gas phase discharge is mixed with the gas phase discharge of the cracking reactor, the gas phase discharge is condensed by a crude product condenser and then enters a crude product collecting tank;
the liquid phase discharge of the crude product collecting tank is pumped to a negative pressure heavy removal rectifying tower through a heavy component recovery pump, the liquid phase discharge at the bottom of the tower is pumped to a crude product condenser to exchange heat with the mixed gas phase discharge, and the discharge is returned to the cracking reactor; condensing the top discharge of the negative pressure heavy removal rectifying tower through a condenser at the top of the heavy removal rectifying tower, entering a collecting tank at the top of the heavy removal rectifying tower, pumping into a negative pressure rectifying AMS product tower through an AMS product tower feeding pump, and obtaining the product alpha-methyl styrene at the top of the tower.
Further, the liquid phase discharged from the cracking reactor is heated by an external circulating pump and a heater, and the residence time of the materials in the cracking reaction unit can be controlled to be 1-6h.
Further, the operating pressure of the negative pressure heavy removal rectifying tower is 10-90kPa (preferably 40-60 kPa), and the operating pressure of the negative pressure rectifying AMS product tower is 1-50kPa (preferably 5-20 kPa). The operating pressures in the present invention are all absolute pressures.
Further, the mass content of the alpha-methyl styrene in the tower bottom of the negative pressure rectification AMS product tower is not less than 99.0 percent.
Compared with the prior art, the invention has the following characteristics:
1) Compared with the phenol tar cracking scheme, the invention adopts a negative pressure rectification method, can avoid continuous cracking of heavy components, can separate cumene, AMS and the like from two towers, and has simple process flow;
2) Compared with the common direct thermal cracking method, the method for controlling the reaction residence time by adopting the continuous direct thermal cracking method increases the reaction directionality and increases the recovery rate of the target product.
Drawings
FIG. 1 is a schematic structural diagram of an apparatus for recovering alpha-methylstyrene by phenol tar cracking in example 1;
the figure indicates:
1-cracking reactor, 2-external circulation pump, 3-heater, 4-gas-liquid separator, 5-crude product condenser, 6-crude product collecting tank, 7-heavy-removal tower feeding pump, 8-negative pressure heavy-removal rectifying tower, 9-heavy component recovery pump, 10-heavy-removal tower top condenser, 11-heavy-removal tower top collecting tank, 12-AMS product feeding pump and 13-negative pressure rectifying AMS product tower.
Detailed Description
The invention will now be described in detail with reference to the drawings and specific examples. The present embodiment is implemented on the premise of the technical scheme of the present invention, and a detailed implementation manner and a specific operation process are given, but the protection scope of the present invention is not limited to the following examples.
Example 1:
the device for recycling the alpha-methylstyrene by cracking the phenol tar as shown in figure 1 comprises a cracking reaction unit, a crude product condenser 5, a negative pressure heavy removal rectifying tower 8 and a negative pressure rectifying AMS product tower 13.
The cracking reaction unit comprises a cracking reactor 1, an external circulation pump 2, a heater 3 and a gas-liquid separator 4, wherein the external circulation pump 2, the heater 3 and the gas-liquid separator 4 are sequentially connected with a liquid phase discharge port of the cracking reactor 1, a gas phase outlet of the cracking reactor 1 and the gas-liquid separator 4 is connected with a feed inlet of a crude product condenser 5, and a liquid phase outlet of the gas-liquid separator 4 is connected with the cracking reactor 1. In addition, a pyrolysis liquid phase discharge port is also arranged on the connecting pipeline between the external circulation pump 2 and the heater 3.
The cracking reaction unit is used for carrying out cracking reaction on the phenol tar raw material, and after the liquid phase discharge of the cracking reactor 1 passes through the external circulation pump 2, part of the liquid phase discharge is extracted, and the other part of the liquid phase discharge is gasified by the heater 3 and then enters the gas-liquid separator 4; the liquid phase discharge of the gas-liquid separator 4 is returned to the cracking reactor 1 for cracking reaction circulation, and the gas phase discharge is mixed with the gas phase discharge of the cracking reactor 1 and enters the crude product condenser 5.
The crude product condenser 5 is used for condensing the pyrolysis gas phase discharge to obtain a liquid phase crude product, and a crude product collecting tank 6 and a heavy-removal tower feed pump 7 are sequentially arranged at the discharge port. Part of liquid phase materials in the crude product collecting tank 6 are extracted and collected through a crude product discharging port, and the other part of liquid phase materials are sent into a negative pressure heavy removal rectifying tower 8 through a heavy removal tower feeding pump 7.
The discharge port of the tower kettle of the negative pressure heavy removal rectifying tower 8 is connected with a heavy component recovery pump 9, the tower kettle discharge is sent to a crude product condenser 5 through the heavy component recovery pump 9, and exchanges heat with the gas phase discharge of the cracking reaction unit, and then returns to the cracking reactor 1 for cracking reaction. The top discharge port of the negative pressure heavy removal rectifying tower 8 is sequentially connected with a heavy removal tower top condenser 10, a heavy removal tower top collecting tank 11 and an AMS product tower feeding pump, and heavy removal rectifying liquid phase extracted from the top of the tower is sequentially fed into a negative pressure rectifying AMS product tower 13 after passing through the heavy removal tower top condenser 10, the heavy removal tower top collecting tank 11 and the AMS product tower feeding pump. The high-purity alpha-methyl styrene is produced from the top of the AMS product tower 13 through negative pressure rectification.
Example 2:
a method for recycling alpha-methylstyrene by phenol tar cracking adopts the device in the embodiment 1, and specifically comprises the following steps:
phenol tar of a device for producing phenol acetone by using isopropylbenzene is taken as a raw material, the flow is 100kg/h, and the mass composition of the phenol tar is 19.9% of phenol, 10.3% of acetophenone, 0.1% of dimethylphenol, 21.7% of cumylphenol and 48.0% of other heavy components. The phenol tar raw material enters a cracking reactor 1 (phi 300 multiplied by 1000 mm), and the pressure is controlled to be 300kPa and the temperature is controlled to be 320 ℃. The materials at the bottom of the cracking reactor 1 are extracted by an external circulating pump 2, the extraction amount is 20kg/h, a part of the materials are heated by a heater 3 and then are delivered to a gas-liquid separator 4, the pressure of the gas-liquid separator 4 is controlled to 300kPa, and the gas-phase materials of the gas-liquid separator 4 and the gas-phase materials of the cracking reactor 1 are condensed to 50 ℃ by a crude product condenser 5 and then enter a crude product collecting tank 6 (normal pressure and normal temperature).
Part of the materials in the crude product collecting tank 6 are extracted, the other part is conveyed to the negative pressure heavy removal rectifying tower 8 through the heavy removal tower feeding pump 7, the control pressure is 10kPa, tower bottom materials enter the cracking reactor 1 after heat exchange at the crude product condenser 5 through the heavy component recovery pump 9, tower top materials enter the heavy removal tower top collecting tank 11 after condensation through the heavy removal tower top condenser 10, and then are conveyed to the negative pressure rectifying AMS product tower 13 through the AMS product tower feeding pump 12. The pressure of the tower top of the tower 13 of the AMS product is 10kPa, the AMS product is obtained at the tower top, the flow is 30kg/h, and the purity of the AMS product is 99.4%. The components obtained from the tower bottom are returned to a main device for producing phenol acetone by isopropylbenzene to carry out rectification and purification of isopropylbenzene, phenol and the like.
Example 3:
the process for recovering alpha-methylstyrene by cracking phenol tar differs from example 2 only in that:
the reaction temperature of the cracking reactor 1 is 350 ℃, the operating pressure is 150kPa, and the top discharge flow of the negative pressure rectification AMS product tower 13 is 35kg/h. The procedure is as in example 2.
The purity of the AMS product obtained was 99.2%.
Example 4:
the process for recovering alpha-methylstyrene by cracking phenol tar differs from example 2 only in that:
the reaction temperature of the cracking reactor 1 is 350 ℃, the operating pressure is 250kPa, and the top discharge flow of the negative pressure rectification AMS product tower 13 is 33kg/h. The procedure is as in example 2.
The purity of the AMS product obtained was 99.3%.
In the phenol recovery method, phenol tar is subjected to high-temperature pyrolysis and rectification purification to obtain an alpha-methylstyrene product, wherein the pyrolysis reaction adopts a mode of controlling the residence time by external circulation heating. The device and the method for recycling the alpha-methylstyrene by cracking the phenol tar can control the residence time of the tar cracking reaction, reduce the production of byproducts and improve the recycling rate of the alpha-methylstyrene.
The previous description of the embodiments is provided to facilitate a person of ordinary skill in the art in order to make and use the present invention. It will be apparent to those skilled in the art that various modifications can be readily made to these embodiments and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above-described embodiments, and those skilled in the art, based on the present disclosure, should make improvements and modifications without departing from the scope of the present invention.
Claims (10)
1. A device for recycling alpha-methylstyrene by cracking phenol tar is characterized by comprising
The cracking reaction unit is used for carrying out cracking reaction on the phenol tar raw material;
the raw product condenser (5) is connected with the gas phase discharge of the cracking reaction unit at the feed inlet and is used for condensing to obtain a liquid phase raw product;
the feeding port of the negative pressure heavy removal rectifying tower (8) is connected with the liquid phase discharging port of the crude product condenser (5), and a heavy removal rectifying liquid phase is extracted from the top of the negative pressure heavy removal rectifying tower (8); and
the feeding port of the negative pressure rectifying AMS product tower (13) is connected with the discharging port of the top of the negative pressure heavy removal rectifying tower (8), and the alpha-methylstyrene is produced from the top of the negative pressure rectifying AMS product tower (13).
2. The device for recycling alpha-methylstyrene by cracking phenol tar according to claim 1, wherein the cracking reaction unit comprises a cracking reactor (1), an external circulation pump (2), a heater (3) and a gas-liquid separator (4) which are sequentially connected with a liquid phase discharge port of the cracking reactor (1);
the gas phase outlet of the gas-liquid separator (4) is connected with the feed inlet of the crude product condenser (5), and the liquid phase outlet is connected with the cracking reactor (1).
3. The device for recycling alpha-methylstyrene by phenol tar cracking of claim 2, wherein a cracking liquid phase discharge port is arranged on the connecting pipeline between the external circulating pump (2) and the heater (3).
4. The device for recycling alpha-methylstyrene by phenol tar cracking according to claim 1, wherein a crude product collecting tank (6) and a de-weight tower feeding pump (7) are arranged between the crude product condenser (5) and the negative pressure de-weight rectifying tower (8) in sequence along the material flow direction;
the crude product collecting tank (6) is provided with a crude product discharging port.
5. The device for recycling alpha-methylstyrene by phenol tar cracking according to claim 1, wherein a heavy component recycling pump (9) is further arranged between a tower bottom discharge port of the negative pressure heavy removal rectifying tower (8) and the crude product condenser (5), and the tower bottom discharge of the negative pressure heavy removal rectifying tower (8) is returned to the cracking reaction unit after heat exchange between the crude product condenser (5) and the gas phase discharge of the cracking reaction unit.
6. The device for recycling alpha-methylstyrene by phenol tar cracking according to claim 1, wherein the top discharge port of the negative pressure de-heavy rectifying tower (8) is sequentially connected with a de-heavy tower top condenser (10) and a de-heavy tower top collecting tank (11),
the discharge port of the top collecting tank (11) of the de-weight tower is connected with a negative pressure rectifying AMS product tower (13).
7. The device for recovering alpha-methylstyrene by phenol tar cracking of claim 6, wherein an AMS product tower feed pump (12) is further arranged between the top collection tank (11) of the de-weight tower and the negative pressure rectifying AMS product tower (13).
8. A method for recovering α -methylstyrene by phenol tar cracking, comprising using the apparatus according to any one of claims 1 to 7, and comprising:
the phenol tar raw material is sent to a cracking reaction unit, the gas phase discharge is sent to a negative pressure heavy removal rectifying tower (8) after being condensed by a crude product condenser (5), the gas phase discharge at the top of the tower is sent to a negative pressure rectifying AMS product tower (13) after being condensed, and the product alpha-methylstyrene is produced at the bottom of the tower.
9. The method for recovering α -methylstyrene from a phenolic tar cracking process of claim 8, comprising:
sending the phenol tar raw material to a cracking reactor (1), separating liquid phase discharge into two parts after passing through an external circulating pump (2), extracting one part, heating the other part by a heater (3), then entering a gas-liquid separator (4), returning the liquid phase discharge of the gas-liquid separator (4) to the cracking reactor (1), mixing the gas phase discharge with the gas phase discharge of the cracking reactor (1), condensing by a crude product condenser (5), and then entering a crude product collecting tank (6);
the liquid phase discharged material of the crude product collecting tank (6) is sent to a negative pressure heavy removal rectifying tower (8) through a heavy removal tower feeding pump (7), the liquid phase discharged material at the bottom of the tower is sent to a crude product condenser (5) through a heavy component recovery pump (9) to exchange heat with the mixed gas phase discharged material, and the discharged material is returned to the cracking reactor (1); the tower top discharge of the negative pressure heavy removal rectifying tower (8) is condensed by a tower top condenser (10) of the heavy removal tower and then enters a tower top collecting tank (11) of the heavy removal tower, and then is sent into a negative pressure rectifying AMS product tower (13) by an AMS product tower feeding pump (12), and the product alpha-methyl styrene is produced at the tower top.
10. The method for recovering α -methylstyrene by phenol tar cracking according to claim 8 or 9, wherein the operating pressure of said negative pressure heavy-duty removal rectifying column (8) is 10 to 90kPa, and the operating pressure of said negative pressure rectifying AMS product column (13) is 1 to 50kPa.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211104505.3A CN116272713A (en) | 2022-09-09 | 2022-09-09 | Device and method for recycling alpha-methylstyrene by cracking phenol tar |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202211104505.3A CN116272713A (en) | 2022-09-09 | 2022-09-09 | Device and method for recycling alpha-methylstyrene by cracking phenol tar |
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| CN116272713A true CN116272713A (en) | 2023-06-23 |
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| CN202211104505.3A Pending CN116272713A (en) | 2022-09-09 | 2022-09-09 | Device and method for recycling alpha-methylstyrene by cracking phenol tar |
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| CN (1) | CN116272713A (en) |
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- 2022-09-09 CN CN202211104505.3A patent/CN116272713A/en active Pending
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