CN108976115A - A kind of method and system of separating benzene-cyclohexane and acetic acid - Google Patents
A kind of method and system of separating benzene-cyclohexane and acetic acid Download PDFInfo
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- CN108976115A CN108976115A CN201710416969.0A CN201710416969A CN108976115A CN 108976115 A CN108976115 A CN 108976115A CN 201710416969 A CN201710416969 A CN 201710416969A CN 108976115 A CN108976115 A CN 108976115A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/43—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
- C07C51/44—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation by distillation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C51/00—Preparation of carboxylic acids or their salts, halides or anhydrides
- C07C51/42—Separation; Purification; Stabilisation; Use of additives
- C07C51/43—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation
- C07C51/44—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation by distillation
- C07C51/46—Separation; Purification; Stabilisation; Use of additives by change of the physical state, e.g. crystallisation by distillation by azeotropic distillation
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- 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
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/04—Purification; Separation; Use of additives by distillation
- C07C7/05—Purification; Separation; Use of additives by distillation with the aid of auxiliary compounds
- C07C7/06—Purification; Separation; Use of additives by distillation with the aid of auxiliary compounds by azeotropic distillation
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Abstract
The present invention relates to a kind of methods of separating benzene-cyclohexane and acetic acid, by the heating of the mixed solution of hexamethylene and acetic acid, make its azeotropic；To adding water in the azeotropic system of hexamethylene and acetic acid, and the temperature of system is controlled at 69.4~69.6 DEG C；Hexamethylene-water forms azeotropic mixture and separated from acetic acid；Collect hexamethylene-water azeotropic mixture and cooling, isolated hexamethylene.The invention also discloses the systems of a kind of separating benzene-cyclohexane and acetic acid.The present invention is used using water as entrainer, the separation of hexamethylene and acetic acid is completed in rectifying column, tower top water phase returns to rectifying column and hexamethylene carries out circulation azeotropic, reduce or eliminate the azeotropic of hexamethylene and acetic acid, tower top obtains the hexamethylene of 1~100ppm of acetic acid content, and tower reactor obtains the acetic acid that mass concentration is greater than 99.5%.Present invention process is simple, and energy and material consumption is low.
Description
Technical field
The present invention relates to the method and devices of a kind of separating benzene-cyclohexane and acetic acid；Belong to petrochemical technology development field.
Background technique
Cyclohexanol, cyclohexanone, adipic acid be the raw material for preparing nylon 6 and nylon66 fiber, cyclohexanol, cyclohexanone, adipic acid
In production process, generally use benzene for raw material, by adding hydrogen to obtain the intermediate products such as hexamethylene, cyclohexene, hexamethylene using
Oxidation obtains the products such as cyclohexanol, cyclohexanone, adipic acid, and cyclohexene adds hydrogen to obtain cyclohexanol through over-churning.
In above-mentioned production process, there are problems that the isolation technics of hexamethylene and acetic acid, since hexamethylene and acetic acid distill
When generate azeotropic, conventional distil-lation technology is difficult to separate.
In order to solve the separation problem of hexamethylene and acetic acid, the general method using washing or extractive distillation, using washing
When separation, the acetic acid diluted of a large amount of low values is generated；When using extractive distillation, it is long that there are separation process, and energy and material consumption is high.
Patent CN104829408B relates to the separation method of a kind of hexamethylene and ethyl acetate, uses phenol as extraction
Ethyl acetate is extracted to common distillation column distillation separation by the extractant of destilling tower, and tower reactor extractant phenol is recycled.The skill
Art is typical extractive distillation separating technology.
Patent CN1270578A be related to it is a kind of by hexamethylene direct oxidation be adipic acid during, removed from hexamethylene
The method and apparatus of acetic acid.It is washed using second level or three-level, removes the acetic acid in hexamethylene, aqueous acetic acid passes through azeotropic distillation
Remove water.The process flow is long, and energy consumption is high.
Summary of the invention
In view of the deficiencies of the prior art, the present invention provides a kind of methods of separating benzene-cyclohexane and acetic acid.
In addition, the present invention also provides the separation systems of a kind of method described in implementation.
A kind of method of separating benzene-cyclohexane and acetic acid by the heating of the mixed solution of hexamethylene and acetic acid, makes its azeotropic；Xiang Huan
Add water in the azeotropic system of hexane and acetic acid, and by the control of the temperature of system the azeotropic temperature 69.4 of water and hexamethylene~
69.6℃；Hexamethylene-water forms azeotropic mixture and separated from acetic acid；Collect hexamethylene-water azeotropic mixture and cooling, isolated hexamethylene
Alkane.
In the method for the present invention, water is added in the azeotropic system of hexamethylene and acetic acid, and temperature is strict controlled in described
At a temperature of, the azeotropic system of hexamethylene and acetic acid is transformed into the azeotropic system of hexamethylene and water, thus, make acetic acid and hexamethylene
Alkane separation.It collects the azeotropic system of hexamethylene and water and obtains oily phase, as hexamethylene by water-oil separating after cooling.Using this hair
Bright method, it is only necessary to which the separation of hexamethylene and acetic acid can be realized in a set of equipment with heating function.The method of the present invention is simple, sets
Standby investment is small；Compared to existing separation method, avoids such as prior art emulsification that may be present, third phase, separation occurs
A series of problems, such as low efficiency, water consumption are big, restored acid concentration is low, reuse effect is poor.
The inventors discovered that temperature is controlled in water with 69.4~69.6 DEG C of hexamethylene azeotropic temperature after adding water, not only
The acetic acid content for helping to reduce isolated hexamethylene can also reduce the water content of isolated acetic acid, improve recycling
Acetic acid quality.
Further preferably, described 69.4~69.5 DEG C of temperature are controlled.
The method of the present invention can theoretically handle the hexamethylene of any mass ratio and the mixed solution of acetic acid.
Preferably, the initial concentration of acetic acid is 10~95% in the mixed solution of hexamethylene and acetic acid.Acetic acid
In the raw material of initial concentration finger ring hexane and acetic acid, the mass percent of acetic acid.
Preferably, the initial concentration of acetic acid is 10~50% in the mixed solution of hexamethylene and acetic acid.
Preferably, the water recycled that the azeotropic system of hexamethylene, water is obtained through refrigerated separation.
Preferably, the mass concentration of the water added is 98~99.9%.
Preferably, the oil phase part that hexamethylene-water azeotropic system condenses divides recycled.In this way, can further mention
High rectification effect.
Preferably, oily phase reflux ratio is less than or equal to 30 (being also 0~30).The reflux ratio are as follows: by hexamethylene-
Ratio between hexamethylene derived from water azeotropic mixture and the hexamethylene of reuse.When oily phase reflux ratio is 0, it is believed that will not
Oily phase recycled.
Further preferably, oily phase reflux ratio is 1~10；It is still more preferably 1~2.
Hexamethylene-water of the separation process of hexamethylene and acetic acid of the present invention preferably described in it can be warming up to is total to
It is carried out under container at a temperature of boiling.
Preferably, the separation process of hexamethylene of the present invention and acetic acid carries out in rectifying column.
In the present invention, the raw material of hexamethylene, acetic acid is placed in rectifying column, heating makes hexamethylene, acetic acid in rectifying column
Hexamethylene-acetic acid azeotropic system (atmosphere) is formed on top, and water is added into the azeotropic system, and controls at the top of rectifying column
Temperature in water and 69.4~69.6 DEG C of hexamethylene azeotropic temperature, the azeotropic system of hexamethylene, acetic acid is transformed into hexamethylene, water
Azeotropic system.Hexamethylene, water azeotropic system by exporting at the top of rectifying column and condensing, isolated hexamethylene.Rectifying column is surplus
Remaining solution is acetic acid.
By the method for the invention, the separation of hexamethylene, acetic acid can be completed using a set of equipment；Compared to the prior art,
The method of the present invention is not necessarily to a large amount of water, and cost is lower；In addition, also achieving hexamethylene by rectifying column top and separated from acetic acid.
The present invention adopts water as entrainer, and the separation of hexamethylene and acetic acid is completed in rectifying column, and tower top water phase returns to essence
Evaporate tower and hexamethylene carry out circulation azeotropic, reduce or eliminate the azeotropic of hexamethylene and acetic acid, tower top obtain acetic acid content 1~
The hexamethylene of 100ppm, tower reactor obtain the acetic acid that mass concentration is greater than 99.5%；The purity energy of the isolated water of tower top water phase
It is positively retained at 98~99.9%；The method of the present invention has the separating effect of excellent hexamethylene and acetic acid.
The present invention also provides the systems of a kind of separating benzene-cyclohexane and acetic acid, including rectifying column, overhead condenser, grease point
Phase tank, tower top water phase reflux pump, overhead oil phase reflux pump, tower bottom cooler；
The rectifying column includes rectifying section and stripping section, and the bottom of rectifying column is connected with tower bottom reboiler；The essence
It evaporates tower and is provided with feed inlet, hexamethylene-water azeotropic mixture outlet is provided at the top of rectifying column, bottom is provided with acetic acid outlet, rectifying
Section is additionally provided with reflux inlet；
The hexamethylene-water azeotropic mixture outlet is connect with the azeotropic mixture entrance of grease phase separation tank, is set on the connecting line
It is equipped with overhead condenser；
Grease phase separation tank is additionally provided with water filling port, water out and mutually exports with oil；The reflux of the water out and rectifying column
Entrance connection, mutually outlet is connect the oil with hexamethylene storage tank.
The acetic acid outlet of rectifying column is connect with acetic acid storage tank, and tower bottom condenser is provided on the connecting line.
Preferably, the feed inlet of the rectifying column is arranged between rectifying section and stripping section.
Preferably, reflux inlet of the water out of grease phase separation tank by tower top water phase reflux pump and the rectifying column
Perforation connection.
Preferably, mutually outlet is connected oil by the perforation of the reflux inlet of overhead oil phase reflux pump and rectifying column.
Preferably, being filled with Titanium θ ring in the rectifying section and stripping section of the rectifying column.
The present invention also provides the systematic difference methods of the separating benzene-cyclohexane and acetic acid, include the following steps:
Step 1: under normal pressure, hexamethylene, vinegar stock are added from rectifying column feed inlet, in grease phase separation tank water phase area
Water is added；
Step 2: tower bottom reboiler heat temperature raising when tower top discharges, starts tower top water phase reflux pump, adjusts aqueous-phase reflux
Flow, the upper temp for controlling the rectifying section of rectifying column is water and 69.4~69.6 DEG C of hexamethylene azeotropic temperature；Start overhead oil
Phase reflux pump controls oily phase reflux ratio and is less than or equal to 30；
Step 3: constantly from the oil of grease phase separation tank, mutually outlet produces hexamethylene；Extraction second is exported from the acetic acid of rectifying column
Acid.
Preferably, controlling tower bottom of rectifying tower liquid level 50-60% in step 1；Water in the water phase area of grease phase separation tank
Phase liquid level 30~50%.
Preferably, the water phase liquid level water phase liquid level in the water phase area of grease phase separation tank is controlled by water supplement.
Preferably, the mass concentration of water is 98~99.9% in water phase in grease phase separation tank.
Preferably, the rectifying section upper temp for controlling rectifying column is 69.4~69.6 DEG C in step 2；Further preferably
It is 69.4~69.5 DEG C.
It that is to say, control is 69.4~69.6 DEG C by the temperature of hexamethylene-water azeotropic mixture outlet output material.
Preferably, in step 2, the return flow of water is that overhead oil mutually flows back and discharges the 9.0 of the sum of mass flow
~11.0%；Further preferably 9.5~10.0%.
Preferably, it is still more preferably 1~2 that oily phase reflux ratio, which is 1~10, in step 2.
A kind of systematic difference method of preferred separating benzene-cyclohexane and acetic acid of the present invention, includes the following steps:
Step 1:
Under normal pressure, hexamethylene, vinegar stock are added from rectifying column feed inlet, tower reactor liquid level 50-60% are established, in grease
Water is added in phase separation tank (4) water phase area, establishes water phase liquid level 30~50%；
Step 2:
Tower bottom reboiler (8) heat temperature raising when tower top discharges, starts tower top water phase reflux pump (5), adjusts aqueous-phase reflux stream
Amount, control rectifying tower top temperature are water and 69.4~69.6 DEG C of hexamethylene azeotropic temperature；Gradually establish overhead oil water phase separation tank (4)
Oil phase liquid position 60-80%, start overhead oil phase reflux pump (6), oily phase reflux ratio control is 1~2；
Step 3:
Constantly from the oil of grease phase separation tank, mutually outlet produces hexamethylene；Extraction acetic acid is exported from the acetic acid of rectifying column；Water phase
Liquid level is controlled by water supplement.
In industrial applications, the mixture of hexamethylene and acetic acid is by entering rectifying between stripping section (1) and rectifying section (2)
Tower, under the action of tower reactor reboiler (8), hexamethylene and acetic acid rectifying and azeotropic to tower top, with the oil of overhead reflux mutually and
Water phase carries out mass transfer and heat exchange, gradually forms the azeotropic mixture outflow tower top of water and hexamethylene, and about 69.4 DEG C of tower top temperature, tower top
1~100ppm of acid content in discharging hexamethylene, about 118 DEG C of bottom temperature, the mass concentration of tower reactor discharging acetic acid is greater than
99.5%.
Beneficial effect
The present invention uses in rectifying column in rectifying section, is that hexamethylene, water are total to by hexamethylene, acetic acid azeotropic gas phase transition
Gas phase is boiled, the latent heat of phase change of acetic acid is made full use of, reduces the separating energy consumption of hexamethylene and acetic acid, shorten separation process, is dropped
Low investment cost and operating cost.
In the present invention, water is added into hexamethylene-acetic acid azeotropic system (atmosphere), and control the temperature, can divided
From the acetic acid of high-purity is obtained, the water content of the acetic acid of recycling can be controlled in 0.5% or less；And the purity of the hexamethylene of recycling
Height, the study found that the acetic acid amount of isolated hexamethylene is can be controlled within 100ppm.
Detailed description of the invention
Fig. 1 is that designed reactive distillation prepares cyclohexyl acetate cyclohexane removing acetic acid process in the preferred solution of the invention
Schematic diagram.
In Fig. 1,1 it is stripping section, 2 is rectifying section, 3 is overhead condenser, 4 is grease phase separation tank, 5 is tower top aqueous-phase reflux
Pump, 6 be overhead oil phase reflux pump, 7 be tower bottom cooler, 8 be tower bottom reboiler.
Specific embodiment
The present invention is illustrated below with reference to embodiment, but embodiment is not construed as limiting the invention.
Device therefor technique is as shown in Figure 1 in the embodiment of the present invention；Its specific parameter and material are as follows:
Divide two sections in the reactive distillation column of DN100 × 6000, upper section is the rectifying section of 4000mm equipped with 5mm Titanium θ
Ring, lower section are the stripping sections of 2000mm equipped with 5mm Titanium θ ring.Tower top is equipped with condenser, grease phase separation tank, oil phase and water phase
There is water supply pipe in reflux pump, grease phase separation tank water phase area.Material inlet port is between rectifying section 2 and stripping section 1.Tower reactor is using electricity
Heating, kettle material are sent after cooling to product bucket.
The system of separating benzene-cyclohexane and acetic acid of the present invention, including rectifying column, overhead condenser 3, grease phase separation tank
4, tower top water phase reflux pump 5, overhead oil phase reflux pump 6, tower bottom cooler 7；
The rectifying column includes rectifying section 2 and stripping section 1, and the bottom of rectifying column is connected with tower bottom reboiler 8；Described
Rectifying column is provided with feed inlet, which is arranged between rectifying section 2 and stripping section 1.Hexamethylene-is provided at the top of rectifying column
The outlet of water azeotropic mixture, bottom are provided with acetic acid outlet, and rectifying section 2 is additionally provided with reflux inlet；
The hexamethylene-water azeotropic mixture outlet is connect with the azeotropic mixture entrance of grease phase separation tank 4, is set on the connecting line
It is equipped with overhead condenser 3；
Grease phase separation tank 4 is additionally provided with water filling port, water out and mutually exports with oil；The water out with oil mutually distinguish by outlet
Or it is connect after merging with the reflux inlet of rectifying column；Wherein, the water out of grease phase separation tank 4 by tower top water phase reflux pump 5 with
The reflux inlet of the rectifying column penetrates through connection.Oily mutually outlet passes through the reflux inlet of overhead oil phase reflux pump 6 and rectifying column
Perforation connection.
Mutually outlet is also connect with hexamethylene storage tank the oil.
The acetic acid outlet of rectifying column and acetic acid storage tank (product bucket, Fig. 1 in be not shown) connection are provided on the connecting line
Tower bottom condenser.
Embodiment 1
Step 1
Under normal pressure, mass fraction is fed with 5kg/h flow from rectifying column for the mixture of 90% hexamethylene and 10% acetic acid
Mouth is added, and establishes tower reactor liquid level 60%；Water is added in grease phase separation tank (4) water phase area, establishes water phase liquid level 30~50%.
Step 2
Tower bottom reboiler (8) heat temperature raising when tower top discharges, starts tower top water phase reflux pump (5), adjusts aqueous-phase reflux stream
Amount 0.81kg/h or so (backflow water yield is that overhead oil mutually flows back and discharges the 9% of the sum of mass flow), controls rectifying tower top temperature
Degree is water and 69.4 DEG C of hexamethylene azeotropic temperature；Overhead oil water phase separation tank (4) oil phase liquid position 60-80% is gradually established, tower is started
Oily phase reflux pump (6) is pushed up, oily phase reflux ratio control is 1, after stable operation, and the mass concentration of water is 99.9% in water phase, tower top
Discharging hexamethylene acid content is 1ppm, and bottom temperature is 118 DEG C or so, and tower reactor discharging quality of acetic acid concentration is 99.5%.
Embodiment 2
Step 1
Under normal pressure, mass fraction is the mixture of 5% hexamethylene and 95% acetic acid with 5kg/h flow from rectifying column feed inlet
It is added, establishes tower reactor liquid level 60%；Water is added in grease phase separation tank (4) water phase area, establishes water phase liquid level 30~50%.
Step 2
Tower bottom reboiler (8) heat temperature raising when tower top discharges, starts tower top water phase reflux pump (5), adjusts aqueous-phase reflux stream
Amount 0.76kg/h or so (backflow water yield is that overhead oil mutually flows back and discharges the 10% of the sum of mass flow), controls rectifying tower top
Temperature is 69.6 DEG C；Overhead oil water phase separation tank (4) oil phase liquid position 60-80% is gradually established, is started overhead oil phase reflux pump (6),
Oily phase reflux ratio control is 30, after stable operation, and the mass concentration of water is 95% in water phase, and tower top discharging hexamethylene acid content is
100ppm, bottom temperature are 118 DEG C or so, and tower reactor discharging quality of acetic acid concentration is 99.8%.
Embodiment 3
Step 1
Under normal pressure, mass fraction is fed with 5kg/h flow from rectifying column for the mixture of 50% hexamethylene and 50% acetic acid
Mouth is added, and establishes tower reactor liquid level 60%；Water is added in grease phase separation tank (4) water phase area, establishes water phase liquid level 30~50%.
Step 2
Tower bottom reboiler (8) heat temperature raising when tower top discharges, starts tower top water phase reflux pump (5), adjusts aqueous-phase reflux stream
Amount 0.275kg/h or so (backflow water yield is that overhead oil mutually flows back and discharges the 11% of the sum of mass flow), controls rectifying tower top
Temperature is water and 69.4 DEG C of hexamethylene azeotropic temperature；Overhead oil water phase separation tank (4) oil phase liquid position 60-80% is gradually established, is not opened
Dynamic overhead oil phase reflux pump (6), oily phase reflux ratio control is 0, after stable operation, and the mass concentration of water is 98% in water phase, tower
Ejection material hexamethylene acid content is 60ppm, and bottom temperature is 118 DEG C or so, and tower reactor discharging quality of acetic acid concentration is 99.6%.
Comparative example 1
Such as embodiment 3, under normal pressure, mass fraction is the mixture of 50% hexamethylene and 50% acetic acid with 5kg/h rectifying column
Feed inlet is added, and establishes tower reactor liquid level 60%, and tower reactor heating is established overhead oil water phase separation tank (4) oil phase liquid position 60-80%, opened
Dynamic overhead oil phase reflux pump (6), oily phase reflux ratio control is 1；After stable operation, rectifying tower top temperature is 78 DEG C；Overhead oil phase
Hexamethylene acid content is 16wt%, can not separating benzene-cyclohexane and acetic acid.
Comparative example 2
Such as embodiment 3, under normal pressure, mass fraction is the mixture of 50% hexamethylene, 25% acetic acid and 25% water with 5kg/h
Rectifying column feed inlet is added, and establishes tower reactor liquid level 60%, and overhead oil water phase separation tank (4) oil phase liquid position 60- is established in tower reactor heating
80%, start overhead oil phase reflux pump (6), oily phase reflux ratio control is 1；After stable operation, rectifying tower top temperature is 69.4 DEG C；
Overhead oil phase hexamethylene acid content is 1ppm, and tower reactor discharging quality of acetic acid concentration is 63%, is unable to get qualified acetic acid.
From above embodiments and comparative example can be seen that separating benzene-cyclohexane of the present invention with acetic acid process simple, energy and material consumption
It is low, it is suitble to industrialization.
Claims (14)
1. a kind of method of separating benzene-cyclohexane and acetic acid, which is characterized in that by the heating of the mixed solution of hexamethylene and acetic acid, make it
Azeotropic；To adding water in the azeotropic system of hexamethylene and acetic acid, and the temperature of system is controlled at 69.4~69.6 DEG C；Hexamethylene
Alkane-water forms azeotropic mixture and separated from acetic acid；Collect hexamethylene-water azeotropic mixture and cooling, isolated hexamethylene.
2. the method for separating benzene-cyclohexane as described in claim 1 and acetic acid, which is characterized in that the mixing of hexamethylene and acetic acid is molten
In liquid, the initial concentration of acetic acid is 10~95%.
3. the method for separating benzene-cyclohexane as described in claim 1 and acetic acid, which is characterized in that the mixing of hexamethylene and acetic acid is molten
In liquid, the initial concentration of acetic acid is 10~50%.
4. the method for separating benzene-cyclohexane as described in claim 1 and acetic acid, which is characterized in that the azeotropic system of hexamethylene, water
The water recycled obtained through refrigerated separation.
5. the method for separating benzene-cyclohexane as described in claim 1 and acetic acid, which is characterized in that hexamethylene-water azeotropic system is cold
Solidifying obtained oil phase part divides recycled；Oily phase reflux ratio is less than or equal to 30.
6. the method for separating benzene-cyclohexane as claimed in claim 1 or 5 and acetic acid, which is characterized in that the quality of the water added is dense
Degree is 98~99.9%.
7. a kind of system of claim 1~6 described in any item separating benzene-cyclohexanes and acetic acid, which is characterized in that including rectifying
Tower, overhead condenser, grease phase separation tank, tower top water phase reflux pump, overhead oil phase reflux pump, tower bottom cooler；
The rectifying column includes rectifying section and stripping section, and the bottom of rectifying column is connected with tower bottom reboiler；The rectifying column
It is provided with feed inlet, hexamethylene-water azeotropic mixture outlet is provided at the top of rectifying column, bottom is provided with acetic acid outlet, and rectifying section is also
It is provided with reflux inlet；
The hexamethylene-water azeotropic mixture outlet is connect with the azeotropic mixture entrance of grease phase separation tank, is arranged on the pipeline of the connection
There is overhead condenser；
Grease phase separation tank is additionally provided with water filling port, water out and mutually exports with oil；The reflux inlet of the water out and rectifying column
Connection, mutually outlet is connect the oil with hexamethylene storage tank.
8. the system of separating benzene-cyclohexane as claimed in claim 7 and acetic acid, which is characterized in that the described oil mutually outlet also with essence
Evaporate the reflux inlet connection of tower.
9. the system of separating benzene-cyclohexane as claimed in claim 8 and acetic acid, which is characterized in that mutually outlet passes through overhead oil phase to oil
The perforation connection of the reflux inlet of reflux pump and rectifying column.
10. the system of separating benzene-cyclohexane as claimed in claim 7 and acetic acid, which is characterized in that the outlet of the acetic acid of rectifying column with
Acetic acid storage tank connects, and is provided with tower bottom condenser on the connecting line.
11. the system of separating benzene-cyclohexane as claimed in claim 7 and acetic acid, which is characterized in that the water out of grease phase separation tank
It is penetrated through and is connected by the reflux inlet of tower top water phase reflux pump and the rectifying column.
12. a kind of systematic difference of claim 7~11 described in any item separating benzene-cyclohexanes and acetic acid, which is characterized in that
Include the following steps:
Step 1: under normal pressure, hexamethylene, vinegar stock are added from rectifying column feed inlet, are added in grease phase separation tank water phase area
Water；
Step 2: tower bottom reboiler heat temperature raising when tower top discharges, starts tower top water phase reflux pump, adjusts aqueous-phase reflux flow,
The temperature for controlling the rectifying section of rectifying column is 69.4~69.6 DEG C of azeotropic temperature of hexamethylene and water；Starting overhead oil mutually flows back
Pump controls oily phase reflux ratio and is less than or equal to 30；
Step 3: constantly from the oil of grease phase separation tank, mutually outlet produces hexamethylene；Extraction acetic acid is exported from the acetic acid of rectifying column.
13. the systematic difference of separating benzene-cyclohexane as claimed in claim 12 and acetic acid, which is characterized in that control rectifying column
Rectifying section upper temp is 69.4~69.6 DEG C.
14. the systematic difference of separating benzene-cyclohexane as claimed in claim 12 and acetic acid, which is characterized in that the return flow of water
Mutually flow back for overhead oil with discharging the sum of mass flow 9.0~11.0%.
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| CN201710416969.0A CN108976115B (en) | 2017-06-05 | 2017-06-05 | Method and system for separating cyclohexane and acetic acid |
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| CN201710416969.0A CN108976115B (en) | 2017-06-05 | 2017-06-05 | Method and system for separating cyclohexane and acetic acid |
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| CN101172941A (en) * | 2006-11-02 | 2008-05-07 | 中国石油化工股份有限公司 | Method for recycling acetic acid in dilute acetic acid |
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| JPS63255244A (en) * | 1987-04-14 | 1988-10-21 | Daicel Chem Ind Ltd | Method for separating organic acid |
| CN101172941A (en) * | 2006-11-02 | 2008-05-07 | 中国石油化工股份有限公司 | Method for recycling acetic acid in dilute acetic acid |
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| CN102267889A (en) * | 2011-06-03 | 2011-12-07 | 华东理工大学 | Method for recovering spirit of vinegar by combining extraction with azeotropic distillation |
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