CN213708196U - Low boiling point solvent recycling device in glyceryl triacetate refining process - Google Patents
Low boiling point solvent recycling device in glyceryl triacetate refining process Download PDFInfo
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- CN213708196U CN213708196U CN202022420847.9U CN202022420847U CN213708196U CN 213708196 U CN213708196 U CN 213708196U CN 202022420847 U CN202022420847 U CN 202022420847U CN 213708196 U CN213708196 U CN 213708196U
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Abstract
The utility model provides a low boiling point solvent retrieval and utilization device in triacetin refining process relates to the fine chemical industry field, mainly in order to realize taking off the continuous operation of low boiling point solvent to the product when preparing triacetin, and with low boiling point solvent circulation retrieval and utilization, concrete structure is including batching preheating bath (1), batching atomizer (2), one-level esterification tower (3), moisture evaporator (4), evacuating device (5), low temperature evaporator (6) and refined esterification kettle (7), the utility model discloses an aspect reduces the dwell time of product in one-level esterification tower (3) and refined esterification kettle (7), and the product is difficult for discolouring, and owing to realized effectively breaking away from of low boiling point solvent, makes product smell, color and luster, and the quality is stable; on the other hand, the removed low-boiling point solvent can be returned to the first-stage esterification tower (3) again to participate in the reaction, so that the raw materials are fully utilized, the waste and the environmental pollution are avoided, and the production efficiency is improved.
Description
Technical Field
The utility model relates to a fine chemistry industry field, concretely relates to low boiling point solvent retrieval and utilization device in triacetin refining process.
Background
With the rapid development of the industrial technologies such as biochemical pharmacy and food additives, the traditional production mode for extracting substance components from natural biological materials cannot meet the development requirements of modern industry, and meanwhile, due to the rise of new fields such as development, improvement and synthesis of natural active substance resources, the mixture of organic solvents is increasingly used as an extraction and addition solvent, so that a large amount of residual mixed solvent which needs to be separated and recovered is generated, the secondary separation and recovery of the solvent is an effective means for reducing cost, energy and consumption of enterprises, and the development of scientific research and upgrading of a solvent recovery device is accelerated.
The glyceryl triacetate is nontoxic and nonirritating, is widely applied to fragrance fixatives, solvents, flexibilizers, cosmetics, medicines and dye industries, and is also an important raw material for organic synthesis. The industrial production method takes glycerol and acetic acid as raw materials and takes concentrated sulfuric acid as a catalyst for direct esterification; the esterification reaction is carried out in the rectifying tower kettle. And (3) sequentially adding quantitative glycerol, acetic acid, a catalyst and toluene as a water-carrying agent into the tower kettle, and heating after the addition is finished. The distillation operation is carried out while the reaction is carried out under the condition of micro-boiling or sub-boiling of the tower bottom liquid, ester phase is totally refluxed, and water phase is separated. When no water is separated out, adding a certain amount of acetic anhydride into the tower kettle, continuously reacting for a period of time, cooling, and weighing the crude ester and water respectively for analysis. The reaction solution was cooled and the catalyst was filtered off. Rectifying the filtrate at normal pressure, and recovering excessive acetic acid and toluene; then the residual acetic acid is further removed by decompression and rectification. And controlling the temperature of the distillation kettle at 100-120 ℃ in the distillation process, adding a certain amount of activated carbon for decolorization when the temperature of the kettle liquid is reduced to be below 100 ℃, stirring, and filtering out the activated carbon to obtain the product of glyceryl triacetate.
When glycerol and acetic acid are used for synthesizing a glycerol triacetate plasticizer, excessive acetic acid and a water-carrying agent are required to be added, if the low fractions are not removed, the opening flash point of a finished product of the glycerol triacetate is lower, the final application range of the product is directly influenced, the conventional glycerol triacetate production generally adopts the processes of esterification, deacidification, refining and neutralization, a common distillation kettle is adopted for removing a low-boiling point solvent, the low-boiling point solvent is separated and then pumped away, firstly, only the purpose of removing water is achieved, and low-boiling point substances cannot be completely removed; secondly, the removed low boiling point solvent is the raw material which is necessary for the esterification reaction, and the remorse of the low boiling point solvent causes the waste of the raw material, and the direct recycling of the low boiling point solvent should be considered.
Disclosure of Invention
In order to solve the problem, the utility model provides a low boiling point solvent retrieval and utilization device in the refined process of glyceryl triacetate realizes taking off the continuous operation of low boiling point solvent to the product when preparing glyceryl triacetate to with low boiling point solvent recycling, improve production efficiency, stabilize product quality.
In order to achieve the above purpose, the utility model adopts the following technical scheme: a low boiling point solvent recycling device in the refining process of glyceryl triacetate comprises a batching preheating tank 1, a batching atomizer 2, a first-stage esterification tower 3, a moisture evaporator 4, a vacuumizing device 5, a low-temperature evaporator 6 and a refining esterification kettle 7;
the batching preheating tank 1 is connected with the batching atomizer 2, a liquid material pump 8 is arranged between the batching preheating tank 1 and the batching atomizer 2, the batching atomizer 2 is connected to the top of the first-stage esterification tower 3, and an atomizing nozzle of the batching atomizer 2 extends into the first-stage esterification tower 3; a discharge port at the bottom of the first-stage esterification tower 3 is connected with the low-temperature evaporator 6, a valve A9 and a pump A10 are arranged, the top of the first-stage esterification tower 3 is connected with the moisture evaporator 4 through a pipeline, and a valve B12 and a pump B11 are arranged between the valve A9 and the pump A10; the moisture evaporator 4 and the low-temperature evaporator 6 are connected to the vacuum extractor 5 through pipelines at the same time, and a valve C13 and a valve D14 are respectively arranged on respective branches; the moisture evaporator 4 and the low-temperature evaporator 6 are connected with each other, and a valve E15 and a pump E16 are arranged; the discharge hole of the low-temperature evaporator 6 is connected with the feed inlet of the refining esterification kettle 7, and a valve F17 and a pump F18 are arranged;
the moisture evaporator 4 is provided with a mixture feeding hole, a moisture outlet, a mixture discharging hole, a steam inlet 19 and a steam outlet 20, and a steam coil 21 is arranged in the moisture evaporator 4 and is respectively connected with the steam inlet 19 and the steam outlet 20;
the low-temperature evaporator 6 is provided with a material inlet, a low-boiling point solvent material outlet and a water vapor material outlet; the feeding port is connected with the first-stage esterification tower 3 and the moisture evaporator 4 in a gathering way through pipelines; the moisture outlet is connected to the vacuum extractor 5, and the mixture discharge port is connected with the refining esterification kettle 7; a heater 22 is arranged at the middle lower position in the low-temperature evaporator 6, flowing steam is introduced into the heater 22 through a steam inlet pipe 23 and a steam outlet pipe 24 which are arranged on the outer wall of the low-temperature evaporator 6, and materials falling on the heater are heated.
Preferably, a condenser 25 is arranged between the vacuumizing device 5 and the connecting pipeline of the moisture evaporator 4 and the low-temperature evaporator 6, moisture is discharged after water vapor and a low-boiling-point solvent are condensed and layered, and the low-boiling-point solvent returns to the ingredient atomizer 2 and finally enters the first-stage esterification tower 3 to participate in the esterification reaction.
Preferably, a pressure regulator 26 is connected to the first esterification tower 3, and a condensing reflux device is arranged in the connecting pipeline, so that the pressure in the tower can be regulated and the material in the tower can be prevented from being discharged.
When the device works, firstly, the valve A9-the valve F17 are closed, materials such as glycerol, acetic acid and the like are added into the batching preheating tank 1, the materials are heated to a preset temperature by the batching preheating tank, then the heated materials are pumped into the batching atomizer 2 through a feed liquid pump, the materials enter the first-stage esterification tower 3 through a nozzle to carry out esterification reaction after being atomized, and the pressure in the first-stage esterification tower 3 can be adjusted through the pressure adjuster 26; after the reaction is finished, opening a valve B12 and a valve C13, and a steam inlet 19 and a steam outlet 20 of a moisture evaporator 4, sending the mixture of the moisture at the upper middle part and the low boiling point solvent of the first-stage esterification tower 3 into the moisture evaporator 4, introducing steam, heating to remove most of the moisture, and pumping the moisture to a condenser 25 by a vacuum extractor; then closing a valve B12 and a valve C13, opening a valve A9, a valve D14 and a valve E15, converging the materials remained in the moisture evaporator 4 and the first-stage esterification tower 3 through a pump A10 and a pump E16, sending the materials into a low-temperature evaporator 6, simultaneously opening a steam inlet pipe 23 and a steam outlet pipe 24 to introduce flowing steam, heating the materials through a heating plate, pumping the residual moisture and the low-boiling-point solvent out to a condenser 25 through a vacuum pumping device 5, allowing the materials after water and the low-boiling-point solvent are removed to enter a refining esterification kettle 7 through a valve F17 and a pump F18 for refining, and finally conveying the materials from the bottom of the refining esterification kettle 7 to a finished product tank; after the water vapor and the low-boiling-point solvent which are pumped into the condenser 25 by the vacuum pumping device 5 are condensed and layered, the water is discharged, and the low-boiling-point solvent returns to the ingredient atomizer 2 and enters the first-stage esterification tower 3 to participate in the next esterification reaction.
Has the advantages that: the utility model adopts the structure to remove and recycle the excessive low boiling point solvent existing in the preparation process of the glyceryl triacetate, on one hand, the retention time of the product in the first-stage esterification tower 3 and the refined esterification kettle 7 is reduced, the product is not easy to change color, and the product has stable smell, color and luster and stable quality due to the effective separation of the low boiling point solvent; on the other hand, the removed low-boiling-point solvent can be returned to the first-stage esterification tower 3 again to participate in the reaction, so that the raw materials are fully utilized, the waste and the environmental pollution are avoided, and the production efficiency is improved; in addition, the device also has the advantages of simple structure, convenient use and simple and easy operation.
Drawings
FIG. 1 is a schematic structural diagram of a low boiling point solvent recycling apparatus in example 1.
FIG. 2 is a schematic structural diagram of a low boiling point solvent recycling apparatus in example 2.
In the figure, a material preheating tank 1, a material atomizer 2, a first-stage esterification tower 3, a moisture evaporator 4, a vacuumizing device 5, a low-temperature evaporator 6, a refining esterification kettle 7, a liquid material pump 8, a valve A9, a pump A10, a pump B11, a valve B12, a valve C13, a valve D14, a valve E15, a pump E16, a valve F17, a pump F18, a steam inlet 19, a steam outlet 20, a steam coil 21, a heater 22, a steam inlet pipe 23, a steam outlet pipe 24, a condenser 25 and a pressure regulator 26.
Detailed Description
The technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the accompanying drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only some embodiments of the present invention, not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative efforts belong to the protection scope of the present invention; in the description of the present invention, the directions or positional relationships indicated are the directions or positional relationships shown on the drawings, and are only for convenience of description and simplification of description, and it is not intended to indicate or imply that the device or element referred to must have a specific direction, be constructed and operated in a specific direction, and thus should not be construed as limiting the present invention.
Example 1
As shown in fig. 1, a low boiling point solvent recycling device in the refining process of triacetin comprises a batching preheating tank 1, a batching atomizer 2, a first-stage esterification tower 3, a moisture evaporator 4, a vacuumizing device 5, a low-temperature evaporator 6 and a refining esterification kettle 7;
the batching preheating tank 1 is connected with the batching atomizer 2, a liquid material pump 8 is arranged between the batching preheating tank 1 and the batching atomizer 2, the batching atomizer 2 is connected to the top of the first-stage esterification tower 3, and an atomizing nozzle of the batching atomizer 2 extends into the first-stage esterification tower 3; a discharge port at the bottom of the first-stage esterification tower 3 is connected with the low-temperature evaporator 6, a valve A9 and a pump A10 are arranged, the top of the first-stage esterification tower 3 is connected with the moisture evaporator 4 through a pipeline, and a valve B12 and a pump B11 are arranged between the valve A9 and the pump A10; the moisture evaporator 4 and the low-temperature evaporator 6 are connected to the vacuum extractor 5 through pipelines at the same time, and a valve C13 and a valve D14 are respectively arranged on respective branches; the moisture evaporator 4 and the low-temperature evaporator 6 are connected with each other, and a valve E15 and a pump E16 are arranged; the discharge hole of the low-temperature evaporator 6 is connected with the feed inlet of the refining esterification kettle 7, and a valve F17 and a pump F18 are arranged;
the moisture evaporator 4 is provided with a mixture feeding hole, a moisture outlet, a mixture discharging hole, a steam inlet 19 and a steam outlet 20, and a steam coil 21 is arranged in the moisture evaporator 4 and is respectively connected with the steam inlet 19 and the steam outlet 20;
the low-temperature evaporator 6 is provided with a material inlet, a low-boiling point solvent material outlet and a water vapor material outlet; the feeding port is connected with the first-stage esterification tower 3 and the moisture evaporator 4 in a gathering way through pipelines; the moisture outlet is connected to the vacuum extractor 5, and the mixture discharge port is connected with the refining esterification kettle 7; a heater 22 is arranged at the middle lower position in the low-temperature evaporator 6, flowing steam is introduced into the heater 22 through a steam inlet pipe 23 and a steam outlet pipe 24 which are arranged on the outer wall of the low-temperature evaporator 6, and materials falling on the heater are heated.
Example 2
As shown in fig. 2, a low boiling point solvent recycling apparatus in the refining process of triacetin has a structure substantially the same as that described in example 1, except that: a condenser 25 is arranged between the vacuumizing device 5 and the connecting pipeline of the moisture evaporator 4 and the low-temperature evaporator 6, moisture is discharged after water vapor and a low-boiling-point solvent are condensed and layered, and the low-boiling-point solvent returns to the ingredient atomizer 2 and finally enters the primary esterification tower 3 to participate in esterification reaction; the first-stage esterification tower 3 is connected with a pressure regulator 26, and a condensation reflux device is arranged in the connecting pipeline, so that the pressure in the tower can be regulated and the material in the tower can be prevented from being discharged.
Claims (3)
1. A low boiling point solvent recycling device in the refining process of glyceryl triacetate is characterized by comprising a batching preheating tank (1), a batching atomizer (2), a primary esterification tower (3), a moisture evaporator (4), a vacuumizing device (5), a low-temperature evaporator (6) and a refining esterification kettle (7);
the batching preheating tank (1) is connected with the batching atomizer (2), a liquid material pump (8) is arranged between the batching preheating tank and the batching atomizer (2), the batching atomizer (2) is connected to the top of the first-stage esterification tower (3), and an atomizing nozzle of the batching atomizer (2) extends into the first-stage esterification tower (3); a discharge port at the bottom of the first-stage esterification tower (3) is connected with the low-temperature evaporator (6), a valve A (9) and a pump A (10) are arranged, the top of the first-stage esterification tower (3) is connected with the moisture evaporator (4) through a pipeline, and a valve B (12) and a pump B (11) are arranged between the valve A and the moisture evaporator; the moisture evaporator (4) and the low-temperature evaporator (6) are connected to the vacuumizing device (5) through pipelines at the same time, and a valve C (13) and a valve D (14) are respectively arranged on respective branches; the moisture evaporator (4) and the low-temperature evaporator (6) are connected with each other, and a valve E (15) and a pump E (16) are arranged; a discharge hole of the low-temperature evaporator (6) is connected with a feed hole of the refining esterification kettle (7), and a valve F (17) and a pump F (18) are arranged;
the moisture evaporator (4) is provided with a mixture feeding hole, a moisture outlet, a mixture discharging hole, a steam inlet (19) and a steam outlet (20), and a steam coil (21) is arranged inside the moisture evaporator (4) and is respectively connected with the steam inlet (19) and the steam outlet (20);
a feeding port, a low-boiling point solvent discharging port and a water vapor discharging port are arranged on the low-temperature evaporator (6); the feeding port is connected with the first-stage esterification tower (3) and the moisture evaporator (4) in a gathering way through pipelines; the moisture outlet is connected to the vacuum extractor (5), and the mixture discharge port is connected with the refining esterification kettle (7); and a heater (22) is arranged at the middle lower position in the low-temperature evaporator (6), and flowing steam is introduced into the heater (22) through a steam inlet pipe (23) and a steam outlet pipe (24) which are arranged on the outer wall of the low-temperature evaporator (6) to heat materials falling on the heater.
2. The recycling device of low-boiling-point solvent in the refining process of triacetin according to claim 1, characterized in that a condenser (25) is arranged between the vacuum extractor (5) and the connecting pipeline of the moisture evaporator (4) and the low-temperature evaporator (6) to condense and stratify the water vapor and the low-boiling-point solvent.
3. The recycling device of low boiling point solvent in triacetin refining process according to claim 1, characterized in that the pressure regulator (26) is connected to the first esterification tower (3), and the condensing reflux device is installed in the connecting pipeline to regulate the pressure in the tower and prevent the material in the tower from leaking out.
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| CN202022420847.9U CN213708196U (en) | 2020-10-27 | 2020-10-27 | Low boiling point solvent recycling device in glyceryl triacetate refining process |
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| CN202022420847.9U CN213708196U (en) | 2020-10-27 | 2020-10-27 | Low boiling point solvent recycling device in glyceryl triacetate refining process |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114534639A (en) * | 2022-02-19 | 2022-05-27 | 济宁福顺化工有限公司 | Multistage esterification reaction processing system |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114534639A (en) * | 2022-02-19 | 2022-05-27 | 济宁福顺化工有限公司 | Multistage esterification reaction processing system |
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