CN106431894B - The recyclable device and method of isooctyl acid in a kind of two tricaprylate production process of triethylene glycol - Google Patents
The recyclable device and method of isooctyl acid in a kind of two tricaprylate production process of triethylene glycol Download PDFInfo
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- CN106431894B CN106431894B CN201611082898.7A CN201611082898A CN106431894B CN 106431894 B CN106431894 B CN 106431894B CN 201611082898 A CN201611082898 A CN 201611082898A CN 106431894 B CN106431894 B CN 106431894B
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- isooctyl acid
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- 239000002253 acid Substances 0.000 title claims abstract description 69
- -1 isooctyl Chemical group 0.000 title claims abstract description 65
- ZIBGPFATKBEMQZ-UHFFFAOYSA-N triethylene glycol Chemical compound OCCOCCOCCO ZIBGPFATKBEMQZ-UHFFFAOYSA-N 0.000 title claims abstract description 35
- 238000000034 method Methods 0.000 title claims abstract description 21
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 16
- 238000001816 cooling Methods 0.000 claims abstract description 84
- 238000000926 separation method Methods 0.000 claims abstract description 17
- 238000004064 recycling Methods 0.000 claims abstract description 13
- 238000011084 recovery Methods 0.000 claims abstract description 12
- 238000004148 unit process Methods 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 76
- 239000007788 liquid Substances 0.000 claims description 49
- 239000007789 gas Substances 0.000 claims description 36
- 239000012071 phase Substances 0.000 claims description 35
- 238000001914 filtration Methods 0.000 claims description 25
- 239000007792 gaseous phase Substances 0.000 claims description 20
- 239000000110 cooling liquid Substances 0.000 claims description 18
- 239000002826 coolant Substances 0.000 claims description 16
- 238000010992 reflux Methods 0.000 claims description 14
- 238000006243 chemical reaction Methods 0.000 claims description 9
- 238000000605 extraction Methods 0.000 claims description 9
- 239000011259 mixed solution Substances 0.000 claims description 7
- 238000009833 condensation Methods 0.000 claims description 5
- 230000005494 condensation Effects 0.000 claims description 5
- 239000000470 constituent Substances 0.000 claims description 5
- 230000032050 esterification Effects 0.000 claims description 5
- 238000005886 esterification reaction Methods 0.000 claims description 5
- 239000000243 solution Substances 0.000 claims description 5
- 239000007921 spray Substances 0.000 claims description 5
- 239000000463 material Substances 0.000 claims description 4
- 238000007599 discharging Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 230000003139 buffering effect Effects 0.000 claims description 2
- 239000000706 filtrate Substances 0.000 claims 1
- 238000006386 neutralization reaction Methods 0.000 abstract description 3
- 239000002994 raw material Substances 0.000 abstract description 3
- 239000003344 environmental pollutant Substances 0.000 abstract description 2
- 231100000719 pollutant Toxicity 0.000 abstract description 2
- 239000010865 sewage Substances 0.000 abstract description 2
- 239000003054 catalyst Substances 0.000 description 4
- 230000008901 benefit Effects 0.000 description 3
- 239000004014 plasticizer Substances 0.000 description 3
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 3
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 208000005156 Dehydration Diseases 0.000 description 1
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 235000009508 confectionery Nutrition 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 239000000284 extract Substances 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 238000003754 machining Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000002480 mineral oil Substances 0.000 description 1
- 235000010446 mineral oil Nutrition 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- 239000004800 polyvinyl chloride Substances 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 239000003566 sealing material Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 229920003051 synthetic elastomer Polymers 0.000 description 1
- 239000005061 synthetic rubber Substances 0.000 description 1
Classifications
-
- 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
-
- 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
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Crystallography & Structural Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses the recyclable devices and method of isooctyl acid in a kind of two tricaprylate production process of triethylene glycol, it is characterised in that: recyclable device includes taking off light kettle, literary formula injector, the first cooling tower, the first cooler, dashpot, collecting tank, evaporator, the second cooling tower, the second condenser；Recovery method includes light component separation, light component cooling, isooctyl acid three unit processes of separation.The present invention improves the utilization rate of raw material, reduces production cost by recycling and utilizing to isooctyl acid；The processes such as subsequent neutralization, sewage treatment are also eliminated simultaneously, reduce pollutant discharge amount；Recyclable device of the invention is simple, easy to implement, and implementation by the method for the invention is, it can be achieved that the rate of recovery of isooctyl acid is up to 98% or more, and the purity for recycling isooctyl acid is greater than 99.5%.
Description
Technical field
The present invention relates to the recyclable devices and method of isooctyl acid in two tricaprylate production process of triethylene glycol.
Background technique
Two tricaprylate of triethylene glycol is kind of a colourless, slightly odorous liquid, has good durability, UV resistant and resists
Antistatic property, not soluble in water and mineral oil dissolve in a variety of organic solvents, are the special efficacys of polyvinyl butyral and synthetic rubber
Plasticizer, so that product is generated low-temperature characteristics and low volatility feature, molecular structure can make machining object possess the good transparency
And coloration.Two tricaprylate of triethylene glycol can also be used for binder and sealing material, be polyvinyl chloride, cellulosics and styrene
Equal products plasticizer.Its speciality plasticizer as polyvinyl butyral film, is indispensable in film process
Raw material, thus be used widely in the field of polyvinyl butyral intermediate coat.
The main method of synthesis two tricaprylate of triethylene glycol is divided into the progress of two steps both at home and abroad at present: the first step is a molecule
The isooctyl acid of triethylene glycol and a molecule sloughs a molecular water under the action of catalyst, generates triethylene glycol list tricaprylate；And then
Second step reaction is carried out, a molecule triethylene glycol list tricaprylate and a molecule isooctyl acid slough a molecule again under the action of catalyst
Water generates two tricaprylate of triethylene glycol.The reaction influence factor includes that catalyst type, reaction time, reaction temperature and three are sweet
Alcohol and isooctyl acid ratio etc. are typical esterification dehydrations.
Production two tricaprylate of triethylene glycol both at home and abroad, the isooctyl acid of selection is excessive, in triethylene glycol and isooctyl acid through being esterified
After reaction, in gained reaction solution in addition to product and catalyst, also containing a large amount of remaining isooctyl acids；Coarse filtration after reaction solution coarse filtration
After liquid passes through neutralisation treatment, direct emission not only increases processing cost, has an effect on environment.The recovery method of isooctyl acid is studied,
It realizes that the selective recovery of isooctyl acid utilizes, reduces discharge, be not only able to reduce the production cost of two tricaprylate of triethylene glycol, mention
The market competitiveness of high product, moreover it is possible to play the role of protecting environment.
Summary of the invention
The purpose of the present invention is to provide a kind of recovery method of isooctyl acid in two tricaprylate production process of triethylene glycol and
Device mainly extracts isooctyl acid from through esterification, filtered coarse filtration liquid.In two tricaprylate production process of triethylene glycol
Isooctyl acid excess 5-20% not only had an economic benefit if can be carried out recycling, but also had environmental benefit.
The present invention solves technical problem, adopts the following technical scheme that
Present invention firstly provides a kind of recyclable device of isooctyl acid in two tricaprylate production process of triethylene glycol, feature exists
In: the recyclable device includes taking off light kettle, literary formula injector, the first cooling tower, the first cooler, dashpot, collecting tank, evaporation
Device, the second cooling tower, the second condenser.
In the collet for taking off and being provided with outside light kettle for being passed through steam, it is described take off to be provided on light kettle take off light kettle coarse filtration
Liquid entrance takes off light kettle material outlet, takes off light kettle gaseous phase outlet and takes off light kettle coolant liquid refluxing opening；It is provided on the collet de-
Light kettle jacket steam entrance is exported with light kettle jacket steam is taken off；
The text formula injector setting takes off middle and lower part in light kettle, including literary formula injector steam inlet, literary formula spray described
Emitter coarse filtration liquid entrance and spray head；
The first cooling tower gas phase entrance, the first cooling tower gaseous phase outlet, first cold is provided on first cooling tower
But tower overflowing liquid entrance, the first cooling tower coolant liquid refluxing opening.
The first condenser gas phase entrance, the first condenser cooling liquid outlet, first are provided on first condenser
Condenser recycles water inlet, the first condenser circulating water outlet, the first condenser vacuum system connector.
Dashpot overflow port, dashpot drain hole and dashpot feed inlet are provided on the dashpot；
Collecting tank feed inlet and collecting tank drain hole are provided on the collecting tank；
Evaporator entry to mixed solution, evaporator isooctyl acid extraction mouth and evaporator gas phase is provided on the evaporator to go out
Mouthful
The second condenser gas phase entrance, the second condenser cooling liquid outlet, second are provided on second condenser
Condenser recycles water inlet, the second condenser circulating water outlet, the second condenser vacuum system connector；
The de- light kettle gaseous phase outlet for taking off light kettle and take off first of light kettle coolant liquid refluxing opening respectively with the first cooling tower
Cooling tower gas phase entrance and the first cooling tower coolant liquid refluxing opening are connected；
The cooling tower gaseous phase outlet of first cooling tower is connected with the first condenser gas phase entrance of the first condenser, and first is cold
But tower overflowing liquid entrance is connected with the dashpot overflow port of dashpot；
First condenser condensate outlet of the first condenser is connected with the dashpot feed inlet of dashpot, the first condenser
Vacuum system connector is connected with pumped vacuum systems, and the first condenser recycles water inlet and the first condenser circulating water outlet difference
It is connected with water on recirculated water and return water system；
The dashpot drain hole of the buffering trench bottom is connected with the collecting tank feed inlet at the top of the collecting tank；
The collecting tank drain hole for collecting trench bottom is connected with the evaporator entry to mixed solution of the evaporator；
Evaporator gaseous phase outlet at the top of the evaporator is connected with the second cooling tower bottom inlet；
Gaseous phase outlet is connected with the second condenser gas phase entrance of second condenser at the top of second cooling tower；
Second condenser vacuum system connector of second condenser is connected with pumped vacuum systems, and the second condenser follows
Ring water inlet and the second condenser circulating water outlet are connected with water on recirculated water and return water system respectively.
It is to utilize invention further provides the recovery method of isooctyl acid in two tricaprylate production process of triethylene glycol
Above-mentioned recyclable device, including light component separation, light component cooling, isooctyl acid three unit processes of separation.Specific steps are as follows:
Step 1, light component separation
The reaction solution of triethylene glycol and isooctyl acid after esterification is subjected to coarse filtration, to remove granule foreign；Gained coarse filtration
Liquid is taken off light kettle coarse filtration liquid entrance addition and is taken off in light kettle, by the control of temperature and pressure, makes light, heavy constituent separation, described heavy
Component includes most two tricaprylate of triethylene glycol；The light component is mainly isooctyl acid and water, carries a small amount of triethylene glycol two secretly
Tricaprylate；
Step 2, light component are cooling
Light component from the first cooling tower gas phase entrance of the first cooling tower cooling tower lower part enter the first cooling tower, by with
Contact of the phegma with column plate, sloughs two tricaprylate of triethylene glycol carried secretly in light component, and isooctyl acid and water vapour constitute light
Component continues to rise, by the first condenser gas phase entrance enter in the first condenser it is cooling after, be formed by isooctyl acid and water
Mixed liquor enters dashpot by the first condenser cooling liquid outlet；By the control to dashpot overflow port spillway discharge, to control
The temperature of first cooling tower, and by the control to dashpot liquid level, and then control its discharging rate；
Step 3, isooctyl acid separation
The mixed liquor of isooctyl acid and water in collecting tank is added in evaporator, by the control of temperature and pressure, makes water
It carries a small amount of isooctyl acid secretly and is detached from mixed liquor into the second cooling tower, be back to the isooctyl acid of entrainment again by the second cooling tower
In evaporator, after water vapour enters the condensation of the second condenser by the second condenser gas phase entrance, through the second condenser coolant liquid
It collects outlet；Isooctyl acid collects recycling from the extraction mouth extraction of evaporator isooctyl acid.
The operating pressure that light kettle is taken off described in step 1 is 8-10Kpa, temperature is 160-170 DEG C.
Gas temperature control is 155-165 DEG C in first cooling tower described in step 2, is mixed at the first condenser cooling liquid outlet
Close 40-50 DEG C of liquid temperature；
The operating pressure of evaporator described in step 3 is 30-40Kpa, temperature is 75-85 DEG C；Second condenser coolant liquid goes out
Water temperature is 40-50 DEG C at mouthful.
The heat source that light kettle is taken off described in step 1 is provided by steam jacket and Wen Shi injector；Steam is from literary formula injector steam
Entrance enters, and sucks coarse filtration liquid by literary formula injector coarse filtration liquid entrance, sprays, is atomized after mixing；Take off light kettle pressure by with
The connected pumped vacuum systems control of first condenser vacuum system connector.
First cooling tower described in step 2 is mainly used for recycling two tricaprylate of triethylene glycol；The cold source of first condenser
For recirculated water, temperature is 28-32 DEG C.
The pressure of evaporator described in step 3 is by the pumped vacuum systems control that is connected with the second condenser vacuum system connector
System；Described second is used for cooling tower in recycling isooctyl acid；The cold source of second cooler is recirculated water, and temperature is 28-32 DEG C.
Compared with prior art, the invention has the advantages that:
1, the present invention improves raw material by recycling and utilizing to isooctyl acid in two tricaprylate production process of triethylene glycol
Utilization rate reduces production cost；The processes such as subsequent neutralization, sewage treatment are also eliminated simultaneously, reduce pollutant discharge amount.
2, recyclable device of the invention is simple, easy to implement, and implementation by the method for the invention is, it can be achieved that isooctyl acid returns
Yield is up to 98% or more, and the purity for recycling isooctyl acid is greater than 99.5%.
Detailed description of the invention
Fig. 1 is the recyclable device of isooctyl acid in two tricaprylate production process of present invention side's triethylene glycol；
Figure label: 1 takes off light kettle；1a takes off light kettle coarse filtration liquid entrance；1b takes off light kettle material outlet；1c takes off light kettle jacket steam
Entrance；1d takes off light kettle jacket steam outlet；1e takes off light kettle gaseous phase outlet；1f takes off light kettle coolant liquid refluxing opening；2 literary formula injectors；
2a text formula injector steam inlet；2b text formula injector coarse filtration liquid entrance；3 first cooling towers；3a the first cooling tower gas phase entrance；
3b the first cooling tower gaseous phase outlet；3c the first cooling tower overflowing liquid entrance；3d the first cooling tower coolant liquid refluxing opening；4 first is cold
Condenser；4a the first condenser gas phase entrance；4b the first condenser cooling liquid outlet；The first condenser of 4c recycles water inlet；4d
One condenser circulating water outlet；The solidifying but device vacuum system connector of 4e first；5 dashpots；5a dashpot overflow port；5b dashpot
Drain hole；5c dashpot feed inlet；6 collecting tanks；6a collecting tank feed inlet；6b collecting tank drain hole；7 evaporators；7a evaporator
Entry to mixed solution；7b evaporator isooctyl acid produces mouth；7c evaporator gaseous phase outlet；8 second cooling towers；9 second condensers；9a
Two condenser gas phase entrances；9b the second condenser cooling liquid outlet；The second condenser of 9c recycles water inlet；The second condenser of 9d follows
Ring water out；9e the second condenser vacuum system connector.
Specific embodiment
As shown in Figure 1, following recyclable device is arranged in the present embodiment first: cold including taking off light kettle 1, literary formula injector 2, first
But tower 3, the first cooler 4, dashpot 5, collecting tank 6, evaporator 7, the second cooling tower 8 and the second cooler 9.
The collet being provided with outside light kettle 1 for being passed through steam is being taken off, is being provided on taking off light kettle 1 and takes off light kettle coarse filtration liquid entrance
1a, light kettle material outlet 1b is taken off, light kettle gaseous phase outlet 1e is taken off and takes off light kettle coolant liquid refluxing opening 1f；It is provided on collet de- light
Kettle jacket steam entrance 1c exports 1d with light kettle jacket steam is taken off；
The literary setting of formula injector 2 is taking off middle and lower part in light kettle 1, including literary formula injector steam inlet 2a and Wen Shi injector
Coarse filtration liquid entrance 2b；
The first cooling tower gas phase entrance 3a, the first cooling tower gaseous phase outlet 3b, are provided on first cooling tower 3
One cooling tower overflowing liquid entrance 3c and the first cooling tower coolant liquid refluxing opening 3d.
The first condenser gas phase entrance 4a, the first condenser cooling liquid outlet 4b, first are provided on the first condenser 4
Condenser recycles water inlet 4c, the first condenser circulating water outlet 4d and the first condenser vacuum system connector 4e.
Dashpot overflow port 5a, dashpot drain hole 5b and dashpot feed inlet 5c are provided on dashpot 5；
Collecting tank feed inlet 6a and collecting tank drain hole 6b are provided on collecting tank 6；
Evaporator entry to mixed solution 7a, evaporator isooctyl acid extraction mouth 7b and evaporator gas phase are provided on evaporator 7
Export 7c；
The second condenser gas phase entrance 9a, the second condenser cooling liquid outlet 9b, second are provided on the second condenser 9
Condenser recycles water inlet 9c, the second condenser circulating water outlet 9d, the second condenser vacuum system connector 9e；
It takes off the de- light kettle gaseous phase outlet 1e of light kettle 1 and takes off of light kettle coolant liquid refluxing opening 1f respectively with the first cooling tower 3
One cooling tower gas phase entrance 3a and the first cooling tower coolant liquid refluxing opening 3d is connected；
The cooling tower gaseous phase outlet 3b of first cooling tower is connected with the first condenser gas phase entrance 4a of the first condenser 4,
First cooling tower overflowing liquid entrance 3c is connected with the dashpot overflow port 5a of dashpot 5；
First condenser condensate outlet 4b of the first condenser 4 is connected with the dashpot feed inlet 5c of dashpot 5, and first
Condenser vacuum system connector 4e is connected with pumped vacuum systems, and the first condenser recycles water inlet 4c and the first condenser circulation
Water out 4d is connected with water on recirculated water and return water system respectively；
The dashpot drain hole of 5 bottom of dashpot is connected with the collecting tank feed inlet 6a at 6 top of collecting tank；
The collecting tank drain hole 6b of 6 bottom of collecting tank is connected with the evaporator entry to mixed solution 7a of evaporator 7；
The evaporator gaseous phase outlet 7c at 7 top of evaporator is connected with 8 bottom inlet of the second cooling tower；
The outlet of second cooling tower, 8 top gas phase is connected with the second condenser gas phase entrance 9a of the second condenser 9；
Second condenser vacuum system connector 9e of the second condenser 9 is connected with pumped vacuum systems, and the second condenser follows
Ring water inlet 9c and the second condenser circulating water outlet 9d are connected with water on recirculated water and return water system respectively.
Using above-mentioned recyclable device, to the method that isooctyl acid in two tricaprylate production process of triethylene glycol is recycled, packet
Include light component separation, light component cooling, isooctyl acid three unit processes of separation, specific steps are as follows:
Step 1, light component separation
The reaction solution of triethylene glycol and isooctyl acid after esterification is subjected to coarse filtration；Gained coarse filtration liquid is taken off light kettle coarse filtration liquid
Entrance 1a addition takes off in light kettle (1), takes off the temperature adjusting and the pressure control of pumped vacuum systems of light kettle collet and Wen Shi injector 2
System, makes light, heavy constituent separation, and heavy constituent includes most two tricaprylate of triethylene glycol；Light component is mainly isooctyl acid and water,
Carry a small amount of two tricaprylate of triethylene glycol secretly；
Step 2, light component are cooling
Light component enters the first cooling tower 3 from the first cooling tower gas phase entrance 3a, sloughs the triethylene glycol carried secretly in light component
Two tricaprylates, isooctyl acid and water vapour continue to be entered by the first condenser gas phase entrance 4a in the first condenser 4 after cooling, institute
The isooctyl acid of formation and the mixed liquor of water enter dashpot 5 by the first condenser cooling liquid outlet 4b, subsequently into collecting tank 6；
By the control to dashpot overflow port 5a spillway discharge, to control the temperature of the first cooling tower 3, and by dashpot liquid level
Control, and then control its discharging rate；
Step 3, isooctyl acid separation
The mixed liquor of isooctyl acid and water in collecting tank 6 is added in evaporator 7, by the control of temperature and pressure, is made
Water carries a small amount of isooctyl acid secretly and is detached from mixed liquor into the second cooling tower 8, returns the isooctyl acid of entrainment again by the second cooling tower 8
It flow in evaporator 7, after water vapour enters the condensation of the second condenser 9 by the second condenser gas phase entrance 9a, through the second condensation
Device cooling liquid outlet 9b is collected；Isooctyl acid collects recycling from the extraction mouth 7b extraction of evaporator isooctyl acid.
The operating pressure that light kettle 1 is taken off in step 1 is 8-10KPa, and temperature is 160-170 DEG C.
Gas temperature control is 155-165 DEG C in first cooling tower of step 2, mixed liquor at the first condenser cooling liquid outlet
40-50 DEG C of temperature；
The operating pressure of step 3 evaporator is 30-40Kpa, temperature is 75-85 DEG C；At second condenser cooling liquid outlet
Water temperature is 40-50 DEG C.
Steam enters from literary formula injector steam inlet 2a in step 1, and is inhaled by text formula injector coarse filtration liquid entrance 2b
Enter coarse filtration liquid, sprays, is atomized after mixing；Light kettle pressure is taken off by vacuumizing with what the first condenser vacuum system connector 4e was connected
System control.
Step 2 first is used for cooling tower in recycling two tricaprylate of triethylene glycol；The cold source of first condenser 4 is recirculated water, temperature
Degree is 28-32 DEG C.
The pressure of step 3 evaporator 7 is controlled by the pumped vacuum systems being connected with the second condenser vacuum system connector 9e；
Second cooling tower 8 is mainly used for recycling isooctyl acid；The cold source of second condenser 9 is recirculated water, and temperature is 28-32 DEG C.
Repeated measurement, the rate of recovery of isooctyl acid is up to 98% or more, and the purity for recycling isooctyl acid is greater than 99.5%.
Claims (4)
1. the recovery method of isooctyl acid in a kind of two tricaprylate production process of triethylene glycol, it is characterised in that: utilize isooctyl acid
Recyclable device carries out, including light component separation, light component cooling, isooctyl acid three unit processes of separation；
The recyclable device includes taking off light kettle (1), literary formula injector (2), the first cooling tower (3), the first condenser (4), buffering
Slot (5), collecting tank (6), evaporator (7), the second cooling tower (8) and the second condenser (9)；
In the collet for taking off and being provided with outside light kettle (1) for being passed through steam, it is provided with that take off light kettle thick on light kettle (1) in described take off
Filtrate inlet (1a) takes off light kettle material outlet (1b), takes off light kettle gaseous phase outlet (1e) and takes off light kettle coolant liquid refluxing opening (1f)；?
It is provided with to take off light kettle jacket steam entrance (1c) and take off light kettle jacket steam on the collet and exports (1d)；
The text formula injector (2), which is arranged, takes off light kettle (1) interior middle and lower part described, including literary formula injector steam inlet (2a) and
Literary formula injector coarse filtration liquid entrance (2b)；
Be provided on first cooling tower (3) the first cooling tower gas phase entrance (3a), the first cooling tower gaseous phase outlet (3b),
First cooling tower overflowing liquid entrance (3c) and the first cooling tower coolant liquid refluxing opening (3d)；
The first condenser gas phase entrance (4a), the first condenser cooling liquid outlet are provided on first condenser (4)
(4b), the first condenser recycle water inlet (4c), the first condenser circulating water outlet (4d) and the first condenser vacuum system and connect
Interface (4e)；
Dashpot overflow port (5a), dashpot drain hole (5b) and dashpot feed inlet are provided on the dashpot (5)
(5c)；
Collecting tank feed inlet (6a) and collecting tank drain hole (6b) are provided on the collecting tank (6)；
It is provided with evaporator entry to mixed solution (7a), evaporator isooctyl acid extraction mouth (7b) on the evaporator (7) and evaporates
Device gaseous phase outlet (7c)；
The second condenser gas phase entrance (9a), the second condenser cooling liquid outlet are provided on second condenser (9)
(9b), the second condenser recycle water inlet (9c), the second condenser circulating water outlet (9d), the connection of the second condenser vacuum system
Mouth (9e)；
The de- light kettle gaseous phase outlet (1e) for taking off light kettle (1) and take off light kettle coolant liquid refluxing opening (1f) respectively with the first cooling tower
(3) the first cooling tower gas phase entrance (3a) is connected with the first cooling tower coolant liquid refluxing opening (3d)；
First condenser gas phase entrance (4a) phase of the cooling tower gaseous phase outlet (3b) of first cooling tower and the first condenser (4)
Even, the first cooling tower overflowing liquid entrance (3c) is connected with the dashpot overflow port (5a) of dashpot (5)；
First condenser condensate outlet (4b) of the first condenser (4) is connected with the dashpot feed inlet (5c) of dashpot (5),
First condenser vacuum system connector (4e) is connected with pumped vacuum systems, and the first condenser recycles water inlet (4c) and first cold
Condenser circulating water outlet (4d) is connected with water on recirculated water and return water system respectively；
The dashpot drain hole of dashpot (5) bottom is connected with the collecting tank feed inlet (6a) at the top of the collecting tank (6)；
The collecting tank drain hole (6b) of collecting tank (6) bottom and the evaporator entry to mixed solution (7a) of the evaporator (7)
It is connected；
Evaporator gaseous phase outlet (7c) at the top of the evaporator (7) is connected with the second cooling tower (8) bottom inlet；
Second condenser gas phase entrance (9a) of the second cooling tower (8) top gas phase outlet and second condenser (9)
It is connected；
Second condenser vacuum system connector (9e) of second condenser (9) is connected with pumped vacuum systems, the second condensation
Device circulating water intake (9c) and the second condenser circulating water outlet (9d) are connected with water on recirculated water and return water system respectively；
The specific steps of the recovery method are as follows:
Step 1, light component separation
The reaction solution of triethylene glycol and isooctyl acid after esterification is subjected to coarse filtration；Gained coarse filtration liquid is taken off light kettle coarse filtration liquid entrance
(1a) addition takes off in light kettle (1), by the control of temperature and pressure, makes light, heavy constituent separation, the heavy constituent includes most of
Two tricaprylate of triethylene glycol；The light component is mainly isooctyl acid and water, carries a small amount of two tricaprylate of triethylene glycol secretly；
The heat source for taking off light kettle is provided by steam jacket and Wen Shi injector (2)；Steam is from literary formula injector steam inlet
(2a) enters, and sucks coarse filtration liquid by literary formula injector coarse filtration liquid entrance (2b), sprays, is atomized after mixing；Take off light kettle pressure
By the pumped vacuum systems control being connected with the first condenser vacuum system connector (4e)；
Step 2, light component are cooling
Light component enters the first cooling tower (3) from the first cooling tower gas phase entrance (3a), sloughs the triethylene glycol carried secretly in light component
Two tricaprylates, isooctyl acid and water vapour continue to be entered by the first condenser gas phase entrance (4a) cooling in the first condenser (4)
Afterwards, the mixed liquor for being formed by isooctyl acid and water enters dashpot (5) by the first condenser cooling liquid outlet (4b), subsequently into
Collecting tank (6)；By the control to dashpot overflow port (5a) spillway discharge, to control the temperature of the first cooling tower (3), and pass through
Control to dashpot liquid level, and then control its discharging rate；
Step 3, isooctyl acid separation
The mixed liquor of isooctyl acid and water in collecting tank (6) is added in evaporator (7), by the control of temperature and pressure, is made
Water carries a small amount of isooctyl acid secretly and is detached from mixed liquor into the second cooling tower (8), and the isooctyl acid of entrainment is made by the second cooling tower (8)
It is back in evaporator (7) again, after water vapour enters the second condenser (9) condensation by the second condenser gas phase entrance (9a),
It is collected through the second condenser cooling liquid outlet (9b)；Isooctyl acid collects recycling from evaporator isooctyl acid extraction mouth (7b) extraction.
2. recovery method according to claim 1, it is characterised in that:
The operating pressure that light kettle is taken off described in step 1 is 8-10Kpa, temperature is 160-170 DEG C.
Gas temperature control is 155-165 DEG C in first cooling tower described in step 2, mixed liquor at the first condenser cooling liquid outlet
40-50 DEG C of temperature；
The operating pressure of evaporator described in step 3 is 30-40Kpa, temperature is 75-85 DEG C；At second condenser cooling liquid outlet
Water temperature is 40-50 DEG C.
3. recovery method according to claim 1 or 2, it is characterised in that: the cold source of first condenser (4) is circulation
Water, temperature are 28-32 DEG C.
4. recovery method according to claim 1 or 2, it is characterised in that: the pressure of evaporator described in step 3 (7) by with
The connected pumped vacuum systems control of second condenser vacuum system connector (9e)；The cold source of second condenser (9) is to follow
Ring water, temperature are 28-32 DEG C.
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Denomination of invention: A device and method for recovering isooctanoic acid in the production process of triethylene glycol diisooctyl ester Effective date of registration: 20231129 Granted publication date: 20190101 Pledgee: Chaohu Branch of China Construction Bank Co.,Ltd. Pledgor: Chaohu Kimcheon wanwei Industry Co.,Ltd. Registration number: Y2023980068457 |