CN110292786A - A kind of isooctyl thioglycolate continuous rectification apparatus and technique - Google Patents
A kind of isooctyl thioglycolate continuous rectification apparatus and technique Download PDFInfo
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- CN110292786A CN110292786A CN201910691088.9A CN201910691088A CN110292786A CN 110292786 A CN110292786 A CN 110292786A CN 201910691088 A CN201910691088 A CN 201910691088A CN 110292786 A CN110292786 A CN 110292786A
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- rectifying column
- isooctyl thioglycolate
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D1/00—Evaporating
- B01D1/22—Evaporating by bringing a thin layer of the liquid into contact with a heated surface
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
- B01D3/14—Fractional distillation or use of a fractionation or rectification column
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C319/00—Preparation of thiols, sulfides, hydropolysulfides or polysulfides
- C07C319/26—Separation; Purification; Stabilisation; Use of additives
- C07C319/28—Separation; Purification
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of isooctyl thioglycolate continuous rectification apparatus, it is related to organic chemical industry's technical field of rectification, including falling film evaporator, purification rectifying column, finished product rectifying column and high boiling rectifying column, the liquid-phase outlet of falling film evaporator is connect with the entrance of purification rectifying column, the liquid-phase outlet of purification rectifying column is connect with the entrance of finished product rectifying column, the liquid-phase outlet of finished product rectifying column is connect with the entrance of high boiling rectifying column, and falling film evaporator, the gaseous phase outlet for purifying rectifying column, finished product rectifying column and high boiling rectifying column are all connected to condenser system.The problem of present invention solves in the prior art that isooctyl thioglycolate residence time in distillation system is long, and side reaction is more, and it is high to discharge high boiling middle isooctyl thioglycolate content, and is difficult to realize continuous rectification production.The present invention realizes isooctyl thioglycolate serialization rectifying, reduces isooctyl thioglycolate residence time in distillation system, reduces side reaction, recycles to the further rectification and purification of high boiling product.
Description
Technical field
The present invention relates to organic chemical industry's technical field of rectification, in particular to a kind of isooctyl thioglycolate continuous rectification apparatus
And the technique using the rectifier unit.
Background technique
Isooctyl thioglycolate mainly occurs esterification by thioacetic acid and isooctanol under the action of catalyst and generates.
Isooctanol is largely excessive in reaction process, and can be with a little side reaction, and washing is needed to remove catalyst after esterification, therefore
Contain the components such as isooctanol, water, high boiling substance during isooctyl thioglycolate is thick.Conventional espresso mainly based on distillation still, uses
Batch technology, distillation sequence is complicated, and distillation time is long, and discharges high boiling middle thioacetic acid content height, and finished product distillation yield is low.Especially
Its isooctyl thioglycolate rests in Distallation systm for a long time as heat-sensitive substance, more aggravates side reaction.
Patent CN204246861U discloses a kind of isooctyl thioglycolate continuous rectification apparatus, including vacuum system and essence
Evaporate system.Vacuum system is connected to distillation system evaporator overhead condenser gas outlet by surge tank, and charging in the middle part of rectifying column, top is equipped with
Flow back dispensing section, and reflux dispensing section is equipped with light fraction outlet, and tower bottom provides heat with reboiler external circulation heating.The patented technology
In, isooctyl thioglycolate residence time in distillation system is long, and side reaction is more, discharges high boiling middle isooctyl thioglycolate content
Height, and it is difficult to realize continuous rectification production.
Summary of the invention
For disadvantages described above, the object of the present invention is to provide a kind of isooctyl thioglycolate continuous rectification apparatus and technique,
Aim to solve the problem that in the prior art isooctyl thioglycolate residence time in distillation system it is long, side reaction is more, discharges high boiling middle mercapto
The different monooctyl ester content of guanidine-acetic acid is high, and is difficult to realize the problem of continuous rectification produces.
In order to solve the above technical problems, the technical scheme is that
A kind of isooctyl thioglycolate continuous rectification apparatus, including falling film evaporator, purification rectifying column, finished product rectifying column with
And high boiling rectifying column, the entrance of falling film evaporator are connected with thick ester tank, liquid-phase outlet and the purification rectifying column of falling film evaporator
Entrance connection, the liquid-phase outlet for purifying rectifying column are connect with the entrance of finished product rectifying column, the liquid-phase outlet and height of finished product rectifying column
The entrance for boiling rectifying column connects, and the outlet of set finished product material is connected to finished product receiving tank, falling film evaporation on high boiling rectifying tower side
Device, the gaseous phase outlet for purifying rectifying column, finished product rectifying column and high boiling rectifying column are all connected to condenser system.
Wherein, the outlet at bottom of high boiling destilling tower is connected to the entrance of scraper evaporator, the outlet connection of scraper evaporator
In high boiling product receiving tank.
Wherein, condenser system includes condenser and condensation receiving tank, is connected to the condenser system and connection of falling film evaporator
Same condensation receiving tank is shared in the condenser system of purification rectifying column.
Wherein, condenser system further includes being connected to the vacuum system of condenser, is connected to the condenser system of purification destilling tower
Same vacuum system is shared with the condenser system for being connected to finished product destilling tower.
Wherein, it purifies and is equipped with return-flow structure on rectifying column, finished product rectifying column and high boiling rectifying column and boils structure again.
Wherein, it purifies in rectifying column, finished product rectifying column and high boiling rectifying column and is equipped with filled layer, the filler in filled layer
For one of silk screen, Lamb wave line, Raschig ring and Pall ring or any several combination.
Wherein, the material of filler is ceramics or 316L stainless steel or titanium.
Kind isooctyl thioglycolate continuous rectificating technique, comprising the following steps:
S1, isooctyl thioglycolate crude product are transported in falling film evaporator via thick ester tank, by falling film evaporator certain
The moisture having in crude product is removed under temperature, pressure；
Isooctyl thioglycolate crude product after S2, water removal enters in purification rectifying column, removes low boiling component；
Isooctyl thioglycolate crude product after S3, removing low boiling component enters in finished product rectifying column, carries out rectification and purification,
And distill out isooctyl thioglycolate first product；
S4, isooctyl thioglycolate first product enter high boiling rectifying column in, further purification be isooctyl thioglycolate at
Product；
S5, high boiling rectifying tower bottom high-boiling components enter scraper evaporator further purify recycling thioacetic acid finished product, and
High-boiling components after purification are transported to out-of-bounds.
Wherein, the temperature and pressure of falling film evaporator is respectively 70~100 DEG C in S1, -0.07~-0.1MPa；It is mentioned in S2
The tower top temperature of pure rectifying column is 70~110 DEG C, and column bottom temperature is 120~160 DEG C, and the pressure of tower top and tower bottom is -0.1MPa；
The tower top temperature of finished product rectifying column is 90~120 DEG C in S3, and column bottom temperature is 130~170 DEG C, the pressure of tower top and tower bottom is-
0.1MPa；The tower top temperature of high boiling rectifying column is 100~120 DEG C in S4, and column bottom temperature is 150~180 DEG C, tower top and tower bottom pressure
Power is -0.1MPa.
After above-mentioned technical proposal, the beneficial effects of the present invention are:
Due to isooctyl thioglycolate continuous rectification apparatus include falling film evaporator, purification rectifying column, finished product rectifying column with
And high boiling rectifying column, raw material take the lead in being removed water by falling film evaporator, then in turn through purification rectifying column, finished product rectifying column with
And high boiling rectifying column is repeatedly purified, to realize the stage continuous rectification of raw material, distillation process is changed by different level accurate
It carries out, effectively reduces the rectifying time in each level, reduce the incidence of side reaction, improve the efficiency of rectifying,
Reduce the time of entire rectification process.
Since the outlet at bottom of high boiling destilling tower is connected to scraper evaporator, by scraper evaporator to the mercapto in high boiling product
The different monooctyl ester of guanidine-acetic acid is purified and is flowed back, to reduce the content of isooctyl thioglycolate in high boiling product.
Since the gaseous phase outlet of falling film evaporator, purification rectifying column, finished product rectifying column and high boiling rectifying column is all connected to
Condenser system guarantees that the by-product during purification can quickly be discharged, and effectively prevents by-product to rectification process speed
The influence of rate.
It shares due to being connected to the condenser system of falling film evaporator with the condenser system for being connected to purification rectifying column same cold
Solidifying receiving tank is shared due to being connected to the condenser system of purification destilling tower with the condenser system for being connected to finished product destilling tower same true
Empty set system, so that the structure of entire Distallation systm is more compact, reduces system to effectively simplify entire Distallation systm
Cause this.
In conclusion the present invention solves in the prior art, isooctyl thioglycolate residence time in distillation system is long,
The problem of side reaction is more, and it is high to discharge high boiling middle isooctyl thioglycolate content, and is difficult to realize continuous rectification production.The present invention is real
Isooctyl thioglycolate serialization rectifying is showed, has reduced isooctyl thioglycolate residence time in distillation system, has reduced secondary anti-
It should occur, the further rectification and purification of high boiling product is recycled, improve isooctyl thioglycolate yield.
Detailed description of the invention
Fig. 1 is a kind of structural schematic diagram of isooctyl thioglycolate continuous rectification apparatus of the present invention.
In figure, the thick ester tank of 1-, 2- falling film evaporator, the first condenser of 20-, the first vacuum system of 21-, 3- purification rectifying
Tower, the second condenser of 4-, the second vacuum system of 31-, the first receiving tank of 32-, 4- finished product rectifying column, 40- third condenser, 41-
Second receiving tank, the high boiling rectifying column of 5-, the 4th condenser of 50-, 51- third vacuum system, 52- third receiving tank, 6- scraper plate steam
Hair device, the high boiling product receiving tank of 60-, 7- finished product receiving tank, 80- dnockout pumps, 81- return-flow structure, 82- boil structure again.
Specific embodiment
With reference to the accompanying drawing, the present invention is further explained.
The orientation being related in this specification is with a kind of normal work of isooctyl thioglycolate continuous rectification apparatus of the present invention
Subject to orientation when making, orientation when its storage and transport is not limited, opposite positional relationship is only represented, does not represent absolute position
Set relationship.
As shown in Figure 1, a kind of isooctyl thioglycolate continuous rectification apparatus, including thick ester tank 1, falling film evaporator 2, purification
Rectifying column 3, finished product rectifying column 4, high boiling rectifying column and scraper evaporator 6, thick ester tank 1, falling film evaporator 2, purification rectifying column
3, finished product rectifying column 4, high boiling rectifying column and scraper evaporator 6 are sequentially connected in series, i.e., the discharge port of thick ester tank 1 passes through pipeline
It is connected in the feeding inlet of falling film evaporator 2, the liquid-phase outlet of falling film evaporator 2 is connected to purification rectifying column 3 by pipeline
The liquid-phase outlet of feeding inlet, purification rectifying column 3 is connected to the feeding inlet of finished product rectifying column 4, the liquid of finished product rectifying column 4 by pipeline
Mutually outlet is connected to the feeding inlet of high boiling rectifying column, and the outlet at bottom of high boiling destilling tower 5 is connected to the pan feeding of scraper evaporator 6
Mouthful, the outlet of scraper evaporator 6 is connected to high boiling product receiving tank 60.Dnockout pumps 80 are respectively mounted on each segment pipe.
As shown in Figure 1, thick ester tank 1 is used for the storage of isooctyl thioglycolate crude product, falling film evaporator 2 is used for thioacetic acid
The mechanism of the water removal of different monooctyl ester crude product, purification rectifying column 3, finished product rectifying column 4 and high boiling rectifying column three tower body is identical, three
The difference is that the difference of reaction condition (tower interior reaction temperature and pressure).It purifies rectifying column 3 and is used for preliminary purification, go
Except the low boiling component after dehydration in isooctyl thioglycolate crude product.After finished product rectifying column 4 and 5 pairs of high boiling destilling tower purifications
Product is further deeply purified, and steps up the finished product content in product, and being exported by the finished product material of high boiling destilling tower 5 will
Finished product materials are transported to finished product receiving tank 7, and the high boiling product in high boiling destilling tower 5 go out to enter in scraper evaporator 6 by bottom
It is purified, into high boiling alembic, the high boiling product after purification enter in high boiling product receiving tank 60 product reflux of purification.
As shown in Figure 1, falling film evaporator 2, purification rectifying column 3, finished product rectifying column 4, high boiling rectifying column and scraper plate evaporation
The gaseous phase outlet of device 6 is all connected to condenser system.Condenser system includes the first condenser 20, the second condenser 30, third condensation
Device 40 and the 4th condenser 50；First vacuum system 21, the second vacuum system 31 and third vacuum system 51；First receives
Tank 32, the second receiving tank 41 and third receiving tank 52.The gaseous phase outlet of falling liquid film generator is connected on the first condenser 20, the
One condenser 20 is connect with the first vacuum system 21, the first receiving tank 32；It is cold that the gaseous phase outlet of purification rectifying column 3 is connected to second
Condenser 30, the second condenser 30 are connect with the second vacuum system 31 and the first receiving tank 32；The gaseous phase outlet of finished product rectifying column 4
It is connected to third condenser 40, third condenser 40 is connect with the second vacuum system 31 and the second receiving tank 41, high boiling rectifying
The gaseous phase outlet of tower is connected to the 4th condenser 50, and the 4th condenser 50 connects with third vacuum system 51 and third receiving tank 52
It connects.
As shown in Figure 1, being equipped with return-flow structure on the tower body of purification rectifying column 3, finished product rectifying column 4 and high boiling rectifying column
81 and structure 82 is boiled again, return-flow structure 81 is that the outlet of each condenser passes through the upper return mouth of branch tieback to tower body
On, then it boils the outlet that structure 82 is tower body bottom and is connected to the entrance of reboiler by branch, the outlet tieback of reboiler to tower
The lower return mouth of body.Return-flow structure 81 contacts the intracorporal gas-liquid two-phase of tire inversely with structure 82 is boiled again, the gas of uplink
Middle heavy constituent condenses, and the light component in the liquid of downlink, which is absorbed heat, to be vaporized, and condensation vaporization repeatedly further increases product point
From precision.
As shown in Figure 1, being equipped with filled layer, filled layer in purification rectifying column 3, finished product rectifying column 4 and high boiling rectifying column
Two layers of preferential setting, the filler in filled layer are one of silk screen, Lamb wave line, Raschig ring and Pall ring or any several
Combination, the material of filler is ceramics or 316L stainless steel or titanium.
A kind of isooctyl thioglycolate continuous rectificating technique, comprising the following steps:
The first step, isooctyl thioglycolate crude product is transported in falling film evaporator 2 via thick ester tank 1, by falling film evaporator 2
The moisture having in crude product is removed under certain temperature and pressure；
Second step, the isooctyl thioglycolate crude product after water removal enter in purification rectifying column 3, remove low boiling component；
Third step, the isooctyl thioglycolate crude product after removing low boiling component enter in finished product rectifying column 4, carry out preliminary
Rectification and purification, and distill out isooctyl thioglycolate finished product；
4th step, isooctyl thioglycolate first product enter high boiling rectifying column in, purification recycling isooctyl thioglycolate at
Product；
5th step, the high-boiling components at high boiling rectifying tower bottom enter scraper evaporator 6 further purification recycling thioacetic acid at
Product, and the high-boiling components after purification are transported to out-of-bounds.
Wherein, the temperature and pressure of falling film evaporator 2 is respectively 70~100 DEG C in step 1, -0.07~-0.1MPa；Step
It is 70~110 DEG C that 3 tower top temperature of rectifying column is purified in rapid 2, and column bottom temperature is 120~160 DEG C, the pressure of tower top and tower bottom is-
0.1MPa；The tower top temperature of finished product rectifying column 4 is 90~120 DEG C in step 3, and column bottom temperature is 130~170 DEG C, tower top and tower
The pressure at bottom is -0.1MPa；100~120 DEG C of the tower top temperature of high boiling rectifying column in step 4, column bottom temperature are 150~180 DEG C,
Tower top and tower bottom pressure are -0.1MPa.
Specifically, the isooctyl thioglycolate crude product that water content is 0.5wt% enters in falling film evaporator 2, falling film evaporation
2 operating condition of device is 80 DEG C, -0.09MPa, and water content is 0 in isooctyl thioglycolate crude product after falling film evaporator 2.
Isooctyl thioglycolate crude product after water removal enters in purification rectifying column 3, and purification 3 operating condition of rectifying column is tower bottom
120 DEG C, -0.09MPa, 90 DEG C of tower top, -0.09MPa, reflux ratio 2, after purified rectifying column 3 in isooctyl thioglycolate crude product
Isooctyl thioglycolate content reaches 90wt%.
Purification 3 materials at bottom of tower of rectifying column enters in finished product rectifying column 4, and operating condition is 135 DEG C of tower bottom, -0.1MPa, tower top
100 DEG C, -0.1MPa, reflux ratio 4, finished product content is 99.5% or more.
4 materials at bottom of tower of finished product rectifying column enters in high boiling rectifying column, and 170 DEG C of operating condition tower bottom, -0.1MPa, tower top 110
DEG C, -0.1MPa, reflux ratio 5.High boiling rectifying column materials at bottom of tower enters in scraper evaporator 6, and the gas phase of scraper evaporator 6 enters
High boiling rectifying column.Scraper evaporator 6 discharges high boiling isooctyl thioglycolate content 5wt%max, in high boiling rectifying column rectifying finished product
Isooctyl thioglycolate content is 99.5wt% or more.
Isooctyl thioglycolate crude product product rectification yield after rectifying reaches 90% or more, finished product content 99.5wt% with
On, discharge high boiling 5wt%max.2 water rem oval of falling film evaporator is high, and the water removal time is short, high boiling rectifying column and scraper evaporator 6
Combined purifying recycles high boiling middle isooctyl thioglycolate, and the rate of recovery is higher.
The present invention is not limited to above-mentioned specific embodiment, those skilled in the art from the above idea,
Without creative labor, the various transformation made are within the scope of the present invention.
Claims (9)
1. a kind of isooctyl thioglycolate continuous rectification apparatus, which is characterized in that including falling film evaporator, purification rectifying column, at
Product rectifying column and high boiling rectifying column, the entrance of the falling film evaporator are connected with thick ester tank, the liquid phase of the falling film evaporator
It exports and is connect with the entrance of the purification rectifying column, the liquid-phase outlet of the purification rectifying column and the entrance of the finished product rectifying column
Connection, the liquid-phase outlet of the finished product rectifying column is connect with the entrance of the high boiling rectifying column, on the high boiling rectifying tower side
Set finished product material outlet is connected to finished product receiving tank, the falling film evaporator, the purification rectifying column, the finished product rectifying column
And the gaseous phase outlet of the high boiling rectifying column is all connected to condenser system.
2. a kind of isooctyl thioglycolate continuous rectification apparatus as described in claim 1, which is characterized in that the high boiling distillation
The outlet at bottom of tower is connected to the entrance of scraper evaporator, and the outlet of the scraper evaporator is connected to high boiling product receiving tank.
3. a kind of isooctyl thioglycolate continuous rectification apparatus as claimed in claim 2, which is characterized in that the condenser system
Including condenser and condensation receiving tank, it is connected to the condenser system of the falling film evaporator and is connected to the purification rectifying column
Condenser system shares the same condensation receiving tank.
4. a kind of isooctyl thioglycolate continuous rectification apparatus as claimed in claim 3, which is characterized in that the condenser system
Further include the vacuum system for being connected to the condenser, be connected to it is described purification destilling tower condenser system and be connected to it is described at
The condenser system of product destilling tower shares the same vacuum system.
5. a kind of isooctyl thioglycolate continuous rectification apparatus as described in Claims 1-4 is any, which is characterized in that described
Return-flow structure is equipped on purification rectifying column, the finished product rectifying column and the high boiling rectifying column and boils structure again.
6. a kind of isooctyl thioglycolate continuous rectification apparatus as described in claim 1, which is characterized in that the purification rectifying
It is equipped with filled layer in tower, the finished product rectifying column and the high boiling rectifying column, the filler in the filled layer is silk screen, plate
One of ripple, Raschig ring and Pall ring or any several combination.
7. a kind of isooctyl thioglycolate continuous rectification apparatus as claimed in claim 6, which is characterized in that the material of the filler
Matter is ceramics or 316L stainless steel or titanium.
8. a kind of isooctyl thioglycolate continuous rectificating technique, which comprises the following steps:
S1, isooctyl thioglycolate crude product are transported in the falling film evaporator via thick ester tank, are existed by the falling film evaporator
The moisture having in crude product is removed under certain temperature and pressure；
Isooctyl thioglycolate crude product after S2, water removal enters in the purification rectifying column, removes low boiling component；
Isooctyl thioglycolate crude product after S3, removing low boiling component enters in the finished product rectifying column, carries out rectification and purification,
And distill out isooctyl thioglycolate first product；
S4, isooctyl thioglycolate first product enter the high boiling rectifying column in, further purification be isooctyl thioglycolate at
Product；
S5, the high boiling rectifying tower bottom high-boiling components enter the scraper evaporator further purify recycle thioacetic acid at
Product, and the high-boiling components after purification are transported to out-of-bounds.
9. a kind of isooctyl thioglycolate continuous rectificating technique as claimed in claim 8, which is characterized in that falling liquid film described in S1
The temperature and pressure of evaporator is respectively 70~100 DEG C, -0.07~-0.1MPa；The tower top temperature of rectifying column is purified described in S2
It is 70~110 DEG C, column bottom temperature is 120~160 DEG C, and the pressure of tower top and tower bottom is -0.1MPa；Finished product rectifying column described in S3
Tower top temperature be 90~120 DEG C, column bottom temperature is 130~170 DEG C, and the pressure of tower top and tower bottom is -0.1MPa；Described in S4
The tower top temperature of high boiling rectifying column is 100~120 DEG C, and column bottom temperature is 150~180 DEG C, tower top and tower bottom pressure be-
0.1MPa。
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| CN105646435A (en) * | 2014-11-11 | 2016-06-08 | 中国石油化工股份有限公司 | Process for continuous preparation of high purity epsilon-caprolactone on the basis of anhydrous peroxy isobutyric acid |
| CN105753649A (en) * | 2016-04-18 | 2016-07-13 | 南京师范大学 | Method of recycling isooctanol from waste solvent in production process of isooctyl thioglycolate |
| US20190161365A1 (en) * | 2016-07-29 | 2019-05-30 | Siemens Aktiengesellschaft | Device for Separating Product Water From Impure Raw Water |
| CN107721890A (en) * | 2017-11-08 | 2018-02-23 | 福州大学 | Reactive distillation produces the method and its process units of isooctyl thioglycolate |
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