CN211836378U - Continuous rectification device for isooctyl thioglycolate - Google Patents
Continuous rectification device for isooctyl thioglycolate Download PDFInfo
- Publication number
- CN211836378U CN211836378U CN201921221322.3U CN201921221322U CN211836378U CN 211836378 U CN211836378 U CN 211836378U CN 201921221322 U CN201921221322 U CN 201921221322U CN 211836378 U CN211836378 U CN 211836378U
- Authority
- CN
- China
- Prior art keywords
- rectification
- rectifying column
- finished product
- purification
- isooctyl thioglycolate
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Active
Links
Images
Landscapes
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The utility model discloses an isooctyl thioglycolate continuous rectification device relates to organic chemical industry rectification technical field, including falling film evaporator, purification rectifying column, finished product rectifying column and high boiling rectifying column, falling film evaporator's liquid phase export and the entry linkage of purification rectifying column, the liquid phase export of purification rectifying column and the entry linkage of finished product rectifying column, the liquid phase export of finished product rectifying column and the entry linkage of high boiling rectifying column, falling film evaporator, purification rectifying column, the gaseous phase export of finished product rectifying column and high boiling rectifying column all connect in condensing system. The utility model provides an among the prior art isooctyl thioglycolate dwell time in rectification system long, the secondary reaction is many, discharges high boiling in isooctyl thioglycolate content high, and is difficult to realize the problem of continuous rectification production. The utility model discloses a isooctyl thioglycolate serialization rectification reduces isooctyl thioglycolate dwell time in rectification system, reduces the side reaction and takes place, purifies the recovery to the further rectification of high boiling result.
Description
Technical Field
The invention relates to the technical field of organic chemical rectification, in particular to a continuous rectification device for isooctyl thioglycolate.
Background
Isooctyl thioglycolate is mainly generated by the esterification reaction of thioglycolic acid and isooctyl alcohol under the action of a catalyst. In the reaction process, a large amount of isooctyl alcohol is excessive, and a few side reactions are accompanied, and the catalyst needs to be removed by washing after the esterification reaction, so that the isooctyl thioglycolate contains isooctyl alcohol, water, high-boiling substances and other components. The traditional distillation mainly takes a distillation kettle as a main part, adopts an intermittent process, has complex distillation procedure, long distillation time, high mercaptoacetic acid content in discharged high boiling point and low distillation yield of a finished product. In particular, isooctyl thioglycolate as a heat-sensitive substance stays in a distillation system for a long time, and side reactions are more severe.
Patent CN204246861U discloses a continuous rectification device of isooctyl thioglycolate, which comprises a vacuum system and a rectification system. The vacuum system is communicated with a condenser gas outlet at the top of the rectifying system through a buffer tank, the middle part of the rectifying tower is fed, a reflux distribution section is arranged at the top, a light component outlet is arranged at the reflux distribution section, and heat is provided by the external circulation heating of a reboiler at the bottom of the tower. In the patent technology, the retention time of isooctyl thioglycolate in a rectification system is long, side reactions are more, the content of isooctyl thioglycolate in discharged high boiling is high, and continuous rectification production is difficult to realize.
Disclosure of Invention
Aiming at the defects, the invention aims to provide a continuous rectification device of isooctyl thioglycolate, and aims to solve the problems that in the prior art, isooctyl thioglycolate has long retention time in a rectification system, more side reactions, high content of isooctyl thioglycolate in high boiling discharge and difficulty in realizing continuous rectification production.
In order to solve the technical problems, the technical scheme of the invention is as follows:
a continuous rectification device for isooctyl thioglycolate comprises a falling-film evaporator, a purification rectification tower, a finished product rectification tower and a high-boiling rectification tower, wherein an inlet of the falling-film evaporator is connected with a crude ester tank, a liquid-phase outlet of the falling-film evaporator is connected with an inlet of the purification rectification tower, a liquid-phase outlet of the purification rectification tower is connected with an inlet of the finished product rectification tower, a liquid-phase outlet of the finished product rectification tower is connected with an inlet of the high-boiling rectification tower, a finished product outlet arranged on the tower side of the high-boiling rectification tower is connected with a finished product receiving tank, and gas-phase outlets of the falling-film evaporator, the purification rectification tower, the finished product rectification tower and the high-boiling rectification tower are connected with a condensation system.
Wherein, the outlet at the bottom of the high-boiling rectifying tower is connected with the inlet of the scraper evaporator, and the outlet of the scraper evaporator is connected with the high-boiling product receiving tank.
Wherein, the condensing system comprises a condenser and a condensation receiving tank, and the condensing system connected with the falling film evaporator and the condensing system connected with the purification and rectification tower share the same condensation receiving tank.
Wherein, the condensing system still includes the vacuum system who connects in the condenser, and the condensing system who connects in purification rectifying column shares the same vacuum system with the condensing system who connects in finished product rectifying column.
Wherein, the purification rectifying tower, the finished product rectifying tower and the high-boiling rectifying tower are all provided with a reflux structure and a reboiling structure.
Wherein, the purification and rectification tower, the finished product rectification tower and the high-boiling rectification tower are all internally provided with filling layers, and the filling materials in the filling layers are one or the combination of any more of a silk screen, plate corrugations, Raschig rings and pall rings.
Wherein, the material of the filler is ceramic, 316L stainless steel or titanium.
After the technical scheme is adopted, the invention has the beneficial effects that:
because isooctyl thioglycolate continuous rectification device includes falling film evaporator, purification rectifying column, finished product rectifying column and high boiling rectifying column, the raw materials are first dewatered by falling film evaporator, then pass through purification rectifying column, finished product rectifying column and high boiling rectifying column in proper order and carry out purification many times, thereby realized the multistage continuous rectification of raw materials, with the rectification process carried out with hierarchical accuracy, effectively reduced the rectification time in every level, reduced the incidence of side reaction, improved the efficiency of rectification, reduced the time of whole rectification reaction.
Because the outlet at the bottom of the high-boiling rectifying tower is connected with the scraper evaporator, the isooctyl thioglycolate in the high-boiling product is purified and refluxed by the scraper evaporator, so that the content of the isooctyl thioglycolate in the high-boiling product is reduced.
Because the gas phase outlets of the falling film evaporator, the purification rectifying tower, the finished product rectifying tower and the high-boiling rectifying tower are connected to the condensing system, the byproduct in the purification process can be rapidly discharged, and the influence of the byproduct on the rectifying reaction rate is effectively avoided.
Because the condensing system connected with the falling film evaporator and the condensing system connected with the purification and rectification tower share the same condensation receiving tank, and the condensing system connected with the purification and rectification tower and the condensing system connected with the finished product rectification tower share the same vacuum system, the whole distillation system is effectively simplified, the structure of the whole distillation system is more compact, and the manufacturing cost is reduced.
In conclusion, the invention solves the problems that the retention time of isooctyl thioglycolate in a rectification system is long, side reactions are more, the content of isooctyl thioglycolate in discharged high boiling is high, and continuous rectification production is difficult to realize in the prior art. The invention realizes the continuous rectification of the isooctyl thioglycolate, reduces the retention time of the isooctyl thioglycolate in a rectification system, reduces the occurrence of side reactions, further rectifies, purifies and recycles high-boiling products, and improves the yield of the isooctyl thioglycolate.
Drawings
FIG. 1 is a schematic structural diagram of a continuous rectification device for isooctyl thioglycolate.
In the figure, 1-crude ester tank, 2-falling film evaporator, 20-first condenser, 21-first vacuum system, 3-purification rectifying tower, 4-second condenser, 31-second vacuum system, 32-first receiving tank, 4-finished product rectifying tower, 40-third condenser, 41-second receiving tank, 5-high boiling rectifying tower, 50-fourth condenser, 51-third vacuum system, 52-third receiving tank, 6-scraper evaporator, 60-high boiling product receiving tank, 7-finished product receiving tank, 80-material pump, 81-reflux structure and 82-reboiling structure.
Detailed Description
The invention is further elucidated with reference to the drawing.
All the directions referred to in the specification are based on the directions of the isooctyl thioglycolate continuous rectification device in normal operation, the directions of the isooctyl thioglycolate continuous rectification device in storage and transportation are not limited, and only represent relative position relations, but not absolute position relations.
As shown in figure 1, the continuous rectification device of isooctyl thioglycolate comprises a crude ester tank 1, a falling-film evaporator 2, a purification and rectification tower 3, a finished product rectification tower 4, a high-boiling rectification tower and a scraper evaporator 6, wherein the crude ester tank 1, the falling-film evaporator 2, the purification and rectification tower 3, the finished product rectification tower 4, the high-boiling rectification tower and the scraper evaporator 6 are sequentially connected in series, the discharge gate of crude ester jar 1 passes through the pipe connection promptly and on the pan feeding mouth of falling film evaporator 2, the liquid phase export of falling film evaporator 2 passes through the pipe connection at the pan feeding mouth of purification rectifying column 3, the liquid phase export of purification rectifying column 3 passes through the pan feeding mouth of pipe connection at finished product rectifying column 4, the liquid phase exit linkage of finished product rectifying column 4 is at the pan feeding mouth of high-boiling rectifying column, the bottom exit linkage of high-boiling rectifying column 5 is at the pan feeding mouth of scraper blade evaporator 6, the exit linkage of scraper blade evaporator 6 is in high-boiling receiving tank 60. The material-beating pump 80 is installed on each section of pipeline.
As shown in fig. 1, a crude ester tank 1 is used for storing isooctyl thioglycolate crude products, a falling film evaporator 2 is used for removing water from the isooctyl thioglycolate crude products, and the mechanisms of a purification and rectification tower 3, a finished product rectification tower 4 and a high-boiling rectification tower are the same, and the three towers are different in reaction conditions (reaction temperature and pressure in the towers). The purification and rectification tower 3 is used for primary purification to remove low-boiling point components in the dehydrated isooctyl thioglycolate crude product. The finished product rectifying tower 4 and the high-boiling rectifying tower 5 further purify the purified product, gradually increase the content of the finished product in the product, convey the finished product material to a finished product receiving tank 7 from a finished product material outlet of the high-boiling rectifying tower 5, discharge the high-boiling product in the high-boiling rectifying tower 5 from the bottom and enter a scraper evaporator 6 for purification, the purified product flows back to the high-boiling distilling tank, and the purified high-boiling product enters a high-boiling product receiving tank 60.
As shown in fig. 1, the gas phase outlets of the falling film evaporator 2, the purification and rectification tower 3, the finished product rectification tower 4, the high-boiling rectification tower and the scraper evaporator 6 are all connected to a condensing system. The condensing system comprises a first condenser 20, a second condenser 30, a third condenser 40 and a fourth condenser 50; a first vacuum system 21, a second vacuum system 31, and a third vacuum system 51; a first receiving tank 32, a second receiving tank 41, and a third receiving tank 52. The gas phase outlet of the falling film generator is connected to a first condenser 20, and the first condenser 20 is connected with a first vacuum system 21 and a first receiving tank 32; a gas phase outlet of the purification and rectification tower 3 is connected with a second condenser 30, and the second condenser 30 is connected with a second vacuum system 31 and a first receiving tank 32; the gas phase outlet of the finished product rectifying column 4 is connected to a third condenser 40, the third condenser 40 is connected to the second vacuum system 31 and the second receiving tank 41, the gas phase outlet of the high-boiling rectifying column is connected to a fourth condenser 50, and the fourth condenser 50 is connected to a third vacuum system 51 and a third receiving tank 52.
As shown in fig. 1, the purifying and rectifying tower 3, the finished product rectifying tower 4 and the high-boiling rectifying tower are all provided with a reflux structure 81 and a reboiling structure 82, the reflux structure 81 is that the outlet of each condenser is connected to the upper reflux opening of the tower through a branch, the reboiling structure 82 is that the outlet of the bottom of the tower is connected to the inlet of the reboiler through a branch, and the outlet of the reboiler is connected to the lower reflux opening of the tower. The backflow structure 81 and the reboiling structure 82 enable gas and liquid in the tire body to be in reverse contact, heavy components in ascending gas are condensed, light components in descending liquid are evaporated in a heat absorption mode, and the repeated condensation and evaporation effects further increase the separation precision of products.
As shown in fig. 1, the purifying and rectifying tower 3, the finished product rectifying tower 4 and the high-boiling rectifying tower are respectively provided with a filling layer, the filling layer is preferably provided with two layers, the filling material in the filling layer is one or the combination of any more of a silk screen, a plate corrugation, a raschig ring and a pall ring, and the material of the filling material is ceramic or 316L stainless steel or titanium metal.
A continuous rectification process of isooctyl thioglycolate comprises the following steps:
firstly, conveying isooctyl thioglycolate crude products into a falling-film evaporator 2 through a crude ester tank 1, and removing water in the crude products by the falling-film evaporator 2 at a certain temperature and pressure;
secondly, the dehydrated isooctyl thioglycolate crude product enters a purification and rectification tower 3 to remove low-boiling point components;
thirdly, the isooctyl thioglycolate crude product from which the low-boiling point components are removed enters a finished product rectifying tower 4 for primary rectifying purification, and the finished product of the isooctyl thioglycolate is distilled;
fourthly, the primary finished product of the isooctyl thioglycolate enters a high-boiling rectifying tower, and the finished product of the isooctyl thioglycolate is purified and recovered;
fifthly, the high-boiling residues at the bottom of the high-boiling rectifying tower enter a scraper evaporator 6 for further purification and recovery of finished products of mercaptoacetic acid, and the purified high-boiling residues are conveyed to the outside.
Wherein the temperature and the pressure of the falling-film evaporator 2 in the step 1 are respectively 70-100 ℃ and-0.07-0.1 MPa; in the step 2, the temperature of the top of the purification and rectification tower 3 is 70-110 ℃, the temperature of the bottom of the tower is 120-160 ℃, and the pressure between the top of the tower and the bottom of the tower is-0.1 MPa; the temperature of the top of the rectifying tower 4 in the step 3 is 90-120 ℃, the temperature of the bottom of the rectifying tower is 130-170 ℃, and the pressure between the top of the rectifying tower and the bottom of the rectifying tower is-0.1 MPa; and 4, the temperature of the top of the high-boiling rectifying tower is 100-120 ℃, the temperature of the bottom of the high-boiling rectifying tower is 150-180 ℃, and the pressure between the top of the high-boiling rectifying tower and the bottom of the high-boiling rectifying tower is-0.1 MPa.
Specifically, the isooctyl thioglycolate crude product with the water content of 0.5 wt% enters a falling-film evaporator 2, the operating condition of the falling-film evaporator 2 is 80 ℃ and-0.09 MPa, and the water content of the isooctyl thioglycolate crude product after passing through the falling-film evaporator 2 is 0.
And (3) feeding the dewatered isooctyl thioglycolate crude product into a purification and rectification tower 3, wherein the operation conditions of the purification and rectification tower 3 are that the tower bottom is at 120 ℃ and-0.09 MPa, the tower top is at 90 ℃ and-0.09 MPa, the reflux ratio is 2, and the content of the isooctyl thioglycolate in the isooctyl thioglycolate crude product after passing through the purification and rectification tower 3 reaches 90 wt%.
The material at the bottom of the purification and rectification tower 3 enters a finished product rectification tower 4 under the operating conditions of 135 ℃ at the bottom of the tower, 0.1MPa, 100 ℃ at the top of the tower, 0.1MPa, a reflux ratio of 4 and a finished product content of more than 99.5 percent.
The material at the bottom of the finished product rectifying tower 4 enters a high-boiling rectifying tower under the operating conditions of 170 ℃ below zero and 0.1MPa at the bottom of the tower, 110 ℃ above the tower, 0.1MPa at the top of the tower and a reflux ratio of 5. The material at the bottom of the high-boiling rectifying tower enters a scraper evaporator 6, and the gas phase of the scraper evaporator 6 enters the high-boiling rectifying tower. The scraper evaporator 6 discharges isooctyl thioglycolate with high boiling point with the content of 5 wt% max, and the rectification finished product of the high boiling rectification tower has the content of isooctyl thioglycolate of more than 99.5 wt%.
After the isooctyl thioglycolate crude product is rectified, the rectification yield of the product reaches over 90 percent, the content of the finished product is over 99.5 weight percent, and 5 weight percent max of high boiling is discharged. The falling-film evaporator 2 has high water removal efficiency and short water removal time, and the high-boiling rectifying tower and the scraper evaporator 6 are combined to purify and recover isooctyl thioglycolate in high boiling, so that the recovery rate is high.
The present invention is not limited to the above-described embodiments, and those skilled in the art will be able to make various modifications without creative efforts from the above-described conception, and fall within the scope of the present invention.
Claims (7)
1. The utility model provides an isooctyl thioglycolate continuous rectification device, its characterized in that, includes falling film evaporator, purification rectifying column, finished product rectifying column and high-boiling rectifying column, the entry linkage of falling film evaporator has crude ester jar, the liquid phase export of falling film evaporator with the entry linkage of purification rectifying column, the liquid phase export of purification rectifying column with the entry linkage of finished product rectifying column, the liquid phase export of finished product rectifying column with the entry linkage of high-boiling rectifying column, the finished product material exit linkage that establishes on the high-boiling rectifying column tower side is in finished product receiving tank, falling film evaporator purification rectifying column, finished product rectifying column and the gaseous phase export of high-boiling rectifying column all are connected in condensing system.
2. The continuous rectification apparatus of isooctyl thioglycolate as claimed in claim 1, wherein the bottom outlet of said high boiling rectification column is connected to the inlet of a wiped film evaporator, and the outlet of said wiped film evaporator is connected to a high boiling product receiving tank.
3. The continuous rectification apparatus of isooctyl thioglycolate as claimed in claim 2, wherein the condensation system comprises a condenser and a condensation receiving tank, and the condensation system connected to the falling film evaporator and the condensation system connected to the purification and rectification column share the same condensation receiving tank.
4. The continuous rectification apparatus of isooctyl thioglycolate as claimed in claim 3, wherein said condensation system further comprises a vacuum system connected to said condenser, wherein said condensation system connected to said purification rectification column and said condensation system connected to said final rectification column share the same vacuum system.
5. The continuous rectifying device for isooctyl thioglycolate according to any one of claims 1 to 4, wherein a reflux structure and a reboiling structure are arranged on the purification rectifying tower, the finished product rectifying tower and the high-boiling rectifying tower.
6. The continuous rectification device of isooctyl thioglycolate according to claim 1, wherein the purification and rectification tower, the finished product rectification tower and the high-boiling rectification tower are respectively provided with a packing layer, and the packing in the packing layer is one or a combination of any more of a wire mesh, plate corrugations, Raschig rings and pall rings.
7. The continuous rectification apparatus of isooctyl thioglycolate as claimed in claim 6, wherein the material of the packing is ceramic or 316L stainless steel or titanium.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201921221322.3U CN211836378U (en) | 2019-07-29 | 2019-07-29 | Continuous rectification device for isooctyl thioglycolate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201921221322.3U CN211836378U (en) | 2019-07-29 | 2019-07-29 | Continuous rectification device for isooctyl thioglycolate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN211836378U true CN211836378U (en) | 2020-11-03 |
Family
ID=73130133
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201921221322.3U Active CN211836378U (en) | 2019-07-29 | 2019-07-29 | Continuous rectification device for isooctyl thioglycolate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN211836378U (en) |
-
2019
- 2019-07-29 CN CN201921221322.3U patent/CN211836378U/en active Active
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN111100005B (en) | Process method for separating and refining butyl butyrate by using partition plate tower | |
| CN110845327A (en) | Process for purifying benzoic acid | |
| CN110862330B (en) | Efficient energy-saving rectification process for recycling DMAC waste liquid | |
| CN211170525U (en) | Preparation system of n-amyl acetate | |
| CN100395226C (en) | Method for mass producing butyl acetate by reactive distillation method and using sulfuric acid as catalyst | |
| CN209178263U (en) | The process unit of octyl alconyl is prepared using crude propylene | |
| CN211836378U (en) | Continuous rectification device for isooctyl thioglycolate | |
| CN212655719U (en) | N-propyl acetate production system capable of recycling in grading manner | |
| CN113666893A (en) | Refining method of furfural | |
| CN110280038B (en) | Titanium tetrachloride rectifying device | |
| CN1038672C (en) | Rectifying device for refining crude vanillin | |
| CN105194899A (en) | Variable-diameter rectifying device and method for separating methylbenzene-isobutylbenzene mixture | |
| CN105669445A (en) | Production technology of ethyl acetate | |
| CN215609419U (en) | N-methyl diisopropanolamine continuous rectification device | |
| CN210495287U (en) | Novel distillation tower without extracting industrial alcohol | |
| CN210205939U (en) | Glycerol distillation equipment | |
| CN112409181A (en) | Dimethyl oxalate rectifying device for coal chemical industry | |
| CN106512462A (en) | Turpentine continuous rectification device | |
| CN107141199A (en) | Methanol mother liquor is without refluxed cryogenic rectificating method and equipment | |
| CN112047834A (en) | Device and method for continuously preparing isobutyric anhydride | |
| CN104496787B (en) | Method for recovering waste acid mother liquid during acetic acid synthesis with methanol carbonylation method | |
| CN206955650U (en) | A kind of purification system of fume colloidal silica production silicon tetrachloride | |
| CN211383861U (en) | Two-stage series rectifying tower | |
| CN114853607B (en) | Monomer-containing solvent refining system and process | |
| CN218962167U (en) | Impurity removing device for tower bottom liquid of methanol recovery tower |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| GR01 | Patent grant | ||
| GR01 | Patent grant |