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 PDF

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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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condenser
cooling tower
inlet
outlet
gas phase
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CN106431894A (en
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吴福胜
胡安宁
刘帮柱
潘晓明
王平林
朱宝华
陈争艳
陈建旭
王家东
童祎
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Chaohu Kimcheon Wanwei Industry Co ltd
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ANHUI WANWEI GROUP Co Ltd
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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
    • 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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Abstract

本发明公开了一种三甘醇二异辛酸酯生产过程中异辛酸的回收装置及方法，其特征在于：回收装置包括脱轻釜、文式喷射器、第一冷却塔、第一冷却器、缓冲槽、收集槽、蒸发器、第二冷却塔、第二冷凝器；回收方法包括轻组分分离、轻组分冷却、异辛酸分离三个单元过程。本发明通过对异辛酸回收和利用，提高了原料的利用率，降低了生产成本；同时也省去了后续中和、污水处理等工序，减少了污染物排放量；本发明的回收装置简单、易于实施，通过本发明方法的实施，可实现异辛酸的回收率达98％以上，且回收异辛酸的纯度大于99.5％。

The invention discloses a recovery device and method for isooctanoic acid in the production process of triethylene glycol diisooctanoate, which is characterized in that the recovery device comprises a delighting kettle, a Wen-type ejector, a first cooling tower and a first cooler , buffer tank, collection tank, evaporator, second cooling tower, second condenser; the recovery method includes three unit processes of light component separation, light component cooling, and iso-octanoic acid separation. By recycling and utilizing isooctanoic acid, the invention improves the utilization rate of raw materials and reduces the production cost; meanwhile, processes such as subsequent neutralization and sewage treatment are omitted, and the discharge amount of pollutants is reduced; the recovery device of the invention is simple, It is easy to implement, and through the implementation of the method of the present invention, the recovery rate of isooctanoic acid can reach more than 98%, and the purity of the recovered isooctanoic acid is greater than 99.5%.

Description

The recyclable device and method of isooctyl acid in a kind of two tricaprylate production process of triethylene glycol
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)

1.一种三甘醇二异辛酸酯生产过程中异辛酸的回收方法，其特征在于：利用异辛酸的回收装置进行，包括轻组分分离、轻组分冷却、异辛酸分离三个单元过程；1. the recovery method of isooctanoic acid in a triethylene glycol diisocaprylate production process, is characterized in that: utilize the recovery device of isooctanoic acid to carry out, comprises three units of light component separation, light component cooling, isooctanoic acid separation process; 所述回收装置包括脱轻釜(1)、文式喷射器(2)、第一冷却塔(3)、第一冷凝器(4)、缓冲槽(5)、收集槽(6)、蒸发器(7)、第二冷却塔(8)和第二冷凝器(9)；The recovery device comprises a delighting kettle (1), a Wen-type ejector (2), a first cooling tower (3), a first condenser (4), a buffer tank (5), a collection tank (6), an evaporator (7), the second cooling tower (8) and the second condenser (9); 在所述脱轻釜(1)外设置有用于通入蒸汽的夹套，在所述脱轻釜(1)上设置有脱轻釜粗滤液入口(1a)、脱轻釜物料出口(1b)、脱轻釜气相出口(1e)和脱轻釜冷却液回流口(1f)；在所述夹套上设置有脱轻釜夹套蒸汽入口(1c)和脱轻釜夹套蒸汽出口(1d)；A jacket for introducing steam is arranged outside the delighting still (1), and a delighting still coarse filtrate inlet (1a) and a delighting still material outlet (1b) are arranged on the delighting still (1). , the gas phase outlet (1e) of the delighting kettle and the cooling liquid return port (1f) of the dehydrating kettle; the jacket is provided with a dehydrating kettle jacket steam inlet (1c) and a dehydrating kettle jacket steam outlet (1d) ; 所述文式喷射器(2)设置在所述脱轻釜(1)内中下部，包括文式喷射器蒸汽入口(2a)和文式喷射器粗滤液入口(2b)；The Wen-style ejector (2) is arranged in the middle and lower part of the delighting kettle (1), and includes a Wen-style ejector steam inlet (2a) and a Wen-style ejector coarse filtrate inlet (2b); 在所述第一冷却塔(3)上设置有第一冷却塔气相入口(3a)、第一冷却塔气相出口(3b)、第一冷却塔溢流液入口(3c)和第一冷却塔冷却液回流口(3d)；The first cooling tower (3) is provided with a first cooling tower gas phase inlet (3a), a first cooling tower gas phase outlet (3b), a first cooling tower overflow liquid inlet (3c) and a first cooling tower cooling tower Liquid return port (3d); 在所述第一冷凝器(4)上设置有第一冷凝器气相入口(4a)、第一冷凝器冷却液出口(4b)、第一冷凝器循环水入口(4c)、第一冷凝器循环水出口(4d)和第一冷凝器真空系统连接口(4e)；The first condenser (4) is provided with a first condenser gas phase inlet (4a), a first condenser cooling liquid outlet (4b), a first condenser circulating water inlet (4c), a first condenser circulation a water outlet (4d) and a first condenser vacuum system connection port (4e); 在所述缓冲槽(5)上设置有缓冲槽溢流口(5a)、缓冲槽放料口(5b)和缓冲槽进料口(5c)；The buffer tank (5) is provided with a buffer tank overflow port (5a), a buffer tank discharge port (5b) and a buffer tank feed port (5c); 在所述收集槽(6)上设置有收集槽进料口(6a)和收集槽放料口(6b)；The collection tank (6) is provided with a collection tank feed port (6a) and a collection tank discharge port (6b); 在所述蒸发器(7)上设置有蒸发器混合液入口(7a)、蒸发器异辛酸采出口(7b)和蒸发器气相出口(7c)；The evaporator (7) is provided with an evaporator mixed liquid inlet (7a), an evaporator isooctanoic acid extraction outlet (7b) and an evaporator gas phase outlet (7c); 在所述第二冷凝器(9)上设置有第二冷凝器气相入口(9a)、第二冷凝器冷却液出口(9b)、第二冷凝器循环水入口(9c)、第二冷凝器循环水出口(9d)、第二冷凝器真空系统连接口(9e)；The second condenser (9) is provided with a second condenser gas phase inlet (9a), a second condenser cooling liquid outlet (9b), a second condenser circulating water inlet (9c), and a second condenser circulation Water outlet (9d), second condenser vacuum system connection port (9e); 所述脱轻釜(1)的脱轻釜气相出口(1e)和脱轻釜冷却液回流口(1f)分别与第一冷却塔(3)的第一冷却塔气相入口(3a)和第一冷却塔冷却液回流口(3d)相连；The gas phase outlet (1e) of the delighting kettle and the cooling liquid reflux port (1f) of the delighting kettle (1) are respectively connected with the first cooling tower gas phase inlet (3a) and the first cooling tower gas phase inlet (3a) of the first cooling tower (3). The cooling tower coolant return port (3d) is connected; 第一冷却塔的冷却塔气相出口(3b)与第一冷凝器(4)的第一冷凝器气相入口(4a)相连，第一冷却塔溢流液入口(3c)与缓冲槽(5)的缓冲槽溢流口(5a)相连；The cooling tower gas phase outlet (3b) of the first cooling tower is connected with the first condenser gas phase inlet (4a) of the first condenser (4), and the first cooling tower overflow liquid inlet (3c) is connected to the buffer tank (5). The overflow port (5a) of the buffer tank is connected; 第一冷凝器(4)的第一冷凝器冷凝液出口(4b)与缓冲槽(5)的缓冲槽进料口(5c)相连，第一冷凝器真空系统连接口(4e)与抽真空系统相连，第一冷凝器循环水入口(4c)和第一冷凝器循环水出口(4d)分别与循环水上水和回水系统相连；The first condenser condensate outlet (4b) of the first condenser (4) is connected to the buffer tank feed port (5c) of the buffer tank (5), and the first condenser vacuum system connection port (4e) is connected to the vacuum pumping system connected, the first condenser circulating water inlet (4c) and the first condenser circulating water outlet (4d) are respectively connected with the circulating water and the return water system; 所述缓冲槽(5)底部的缓冲槽放料口与所述收集槽(6)顶部的收集槽进料口(6a)相连；The buffer tank discharge port at the bottom of the buffer tank (5) is connected with the collection tank feed port (6a) at the top of the collection tank (6); 所述收集槽(6)底部的收集槽放料口(6b)与所述蒸发器(7)的蒸发器混合液入口(7a)相连；The collection tank discharge port (6b) at the bottom of the collection tank (6) is connected to the evaporator mixed liquid inlet (7a) of the evaporator (7); 所述蒸发器(7)顶部的蒸发器气相出口(7c)与所述第二冷却塔(8)底部入口相连；The evaporator gas phase outlet (7c) at the top of the evaporator (7) is connected to the bottom inlet of the second cooling tower (8); 所述第二冷却塔(8)顶部气相出口与所述第二冷凝器(9)的第二冷凝器气相入口(9a)相连；The gas phase outlet at the top of the second cooling tower (8) is connected with the second condenser gas phase inlet (9a) of the second condenser (9); 所述第二冷凝器(9)的第二冷凝器真空系统连接口(9e)与抽真空系统相连，第二冷凝器循环水进口(9c)和第二冷凝器循环水出口(9d)分别与循环水上水和回水系统相连；The second condenser vacuum system connection port (9e) of the second condenser (9) is connected to the vacuum pumping system, and the second condenser circulating water inlet (9c) and the second condenser circulating water outlet (9d) are respectively connected to the vacuum pumping system. The circulating water is connected to the return water system; 所述回收方法的具体步骤为：The concrete steps of the recovery method are: 步骤1、轻组分分离Step 1. Light component separation 将三甘醇与异辛酸经酯化反应后的反应液进行粗滤；所得粗滤液经脱轻釜粗滤液入口(1a)加入脱轻釜(1)中，通过温度和压力的控制，使轻、重组分分离，所述重组分包含大部分的三甘醇二异辛酸酯；所述轻组分主要为异辛酸和水，夹带少量三甘醇二异辛酸酯；The reaction solution after the esterification reaction of triethylene glycol and isooctanoic acid is subjected to coarse filtration; the obtained coarse filtrate is added to the delighting still (1) through the crude filtrate inlet (1a) of the delighting still, and the light is controlled by temperature and pressure. , the heavy component is separated, and the heavy component comprises most of triethylene glycol diisooctanoate; the light component is mainly isooctanoic acid and water, and a small amount of triethylene glycol diisooctanoate is entrained; 所述脱轻釜的热源由蒸汽夹套和文式喷射器(2)提供；蒸汽从文式喷射器蒸汽入口(2a)进入，并通过文式喷射器粗滤液入口(2b)吸入粗滤液，混合后喷出、雾化；脱轻釜压力由与第一冷凝器真空系统连接口(4e)相连的抽真空系统控制；The heat source of the delighting kettle is provided by the steam jacket and the Wen-style ejector (2); the steam enters from the steam inlet (2a) of the Wen-style ejector, and sucks the crude filtrate through the crude filtrate inlet (2b) of the Wen-style ejector, and mixes After spraying and atomizing; the pressure of the light-removing kettle is controlled by the vacuum system connected to the first condenser vacuum system connection port (4e); 步骤2、轻组分冷却Step 2. Light component cooling 轻组分从第一冷却塔气相入口(3a)进入第一冷却塔(3)，脱去轻组分中夹带的三甘醇二异辛酸酯，异辛酸和水蒸汽继续由第一冷凝器气相入口(4a)进入第一冷凝器(4)中冷却后，所形成的异辛酸和水的混合液由第一冷凝器冷却液出口(4b)进入缓冲槽(5)，然后进入收集槽(6)；通过对缓冲槽溢流口(5a)溢流量的控制，来控制第一冷却塔(3)的温度，并通过对缓冲槽液位的控制，进而控制其放料速率；The light component enters the first cooling tower (3) from the first cooling tower gas phase inlet (3a) to remove the triethylene glycol diisooctanoate entrained in the light component, and the isooctanoic acid and water vapor continue to pass through the first condenser. After the gas phase inlet (4a) enters the first condenser (4) for cooling, the formed mixture of isooctanoic acid and water enters the buffer tank (5) from the first condenser cooling liquid outlet (4b), and then enters the collection tank ( 6); Control the temperature of the first cooling tower (3) by controlling the overflow flow of the buffer tank overflow port (5a), and then control its discharge rate by controlling the liquid level of the buffer tank; 步骤3、异辛酸分离Step 3. Isooctanoic acid separation 将收集槽(6)中的异辛酸和水的混合液加入蒸发器(7)中，通过温度和压力的控制，使水夹带少量的异辛酸脱离混合液进入第二冷却塔(8)，经过第二冷却塔(8)使夹带的异辛酸再回流至蒸发器(7)中，水蒸汽通过第二冷凝器气相入口(9a)进入第二冷凝器(9)冷凝后，经第二冷凝器冷却液出口(9b)收集；异辛酸从蒸发器异辛酸采出口(7b)采出，收集回收。The mixed solution of isooctanoic acid and water in the collecting tank (6) is added to the evaporator (7), and through the control of temperature and pressure, the water is entrained with a small amount of isooctanoic acid and leaves the mixed solution and enters the second cooling tower (8), and passes through the second cooling tower (8). The second cooling tower (8) recirculates the entrained isooctanoic acid to the evaporator (7), and the water vapor enters the second condenser (9) through the second condenser gas phase inlet (9a) for condensation, and passes through the second condenser. The cooling liquid outlet (9b) is collected; the isooctanoic acid is extracted from the isooctanoic acid extraction outlet (7b) of the evaporator, and collected and recovered. 2.根据权利要求1所述的回收方法，其特征在于：2. recovery method according to claim 1, is characterized in that: 步骤1所述脱轻釜的操作压力为8-10Kpa、温度为160-170℃。The operating pressure of the light-removing kettle described in step 1 is 8-10Kpa, and the temperature is 160-170°C. 步骤2所述第一冷却塔中气体温度控制为155-165℃，第一冷凝器冷却液出口处混合液温度40-50℃；The temperature of the gas in the first cooling tower described in step 2 is controlled to be 155-165 °C, and the temperature of the mixed liquid at the cooling liquid outlet of the first condenser is 40-50 °C; 步骤3所述蒸发器的操作压力为30-40Kpa、温度为75-85℃；第二冷凝器冷却液出口处水温为40-50℃。The operating pressure of the evaporator in step 3 is 30-40Kpa, and the temperature is 75-85°C; the water temperature at the cooling liquid outlet of the second condenser is 40-50°C. 3.根据权利要求1或2所述的回收方法，其特征在于：所述第一冷凝器(4)的冷源为循环水，温度为28-32℃。3. The recovery method according to claim 1 or 2, characterized in that: the cold source of the first condenser (4) is circulating water, and the temperature is 28-32°C. 4.根据权利要求1或2所述的回收方法，其特征在于：步骤3所述蒸发器(7)的压力由与第二冷凝器真空系统连接口(9e)相连的抽真空系统控制；所述第二冷凝器(9)的冷源为循环水，温度为28-32℃。4. The recovery method according to claim 1 or 2, characterized in that: the pressure of the evaporator (7) described in step 3 is controlled by a vacuum system connected to the second condenser vacuum system connection port (9e); The cold source of the second condenser (9) is circulating water, and the temperature is 28-32°C.
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