CN210261601U - Continuous production device of dioctyl adipate - Google Patents
Continuous production device of dioctyl adipate Download PDFInfo
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- CN210261601U CN210261601U CN201921177509.8U CN201921177509U CN210261601U CN 210261601 U CN210261601 U CN 210261601U CN 201921177509 U CN201921177509 U CN 201921177509U CN 210261601 U CN210261601 U CN 210261601U
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Abstract
The utility model relates to a serialization apparatus for producing of dioctyl adipate belongs to plasticizer production technical field. In the utility model, a reaction kettle is connected with a crude ester buffer tank, a neutralization reactor, a neutralization and sedimentation separation tank, a primary washing stirring tank, a primary washing settling tank, a secondary washing stirring tank, a secondary washing settling tank, a neutralization crude ester tank, an ester heat exchanger, a stripping product tank, an adsorption separator, a filter and a finished product tank in sequence; the reaction kettle is connected with the esterification tower, the esterification condenser and the alcohol-water separation tank in sequence; the ester heat exchanger is connected with a stripping preheater, a stripping tower, a stripping condenser and a stripping separating tank in sequence; the stripping tower is also connected with a drying tower and an ester heat exchanger in sequence. The utility model has the advantages of being scientific and reasonable in design, the simple operation elasticity is big, and the deformability is strong, and safety ring protects, and the product quality who produces is high, can adapt to market needs.
Description
Technical Field
The utility model relates to a serialization apparatus for producing of dioctyl adipate belongs to plasticizer production technical field.
Background
Dioctyl adipate (DOA) is an environment-friendly plasticizer industrially produced in recent years, and in the early stage, because the yield is small and the technical level is low, a full-batch production process and a full-batch production device are adopted, so that the prepared product has poor quality (low purity, high acid value and high moisture), frequent manual operation, high labor intensity and severe environment, the production efficiency and quality of dioctyl adipate are severely restricted, and the technical improvement is urgently needed.
SUMMERY OF THE UTILITY MODEL
The utility model aims at providing a serialization apparatus for producing of dioctyl adipate, its design scientific and reasonable, the simple operation elasticity is big, and the strainability is strong, and safety ring protects, and the product quality who produces is high, can adapt to the market needs.
The utility model discloses a dioctyl adipate's serialization apparatus for producing, reation kettle and crude ester buffer tank, neutralization reactor, neutralization and sedimentation separation jar, primary washing agitator tank, primary washing settling tank, secondary washing agitator tank, secondary washing settling tank, neutralization crude ester jar, ester heat exchanger, strip product jar, adsorption separator, filter and finished product jar link to each other in proper order; the reaction kettle is connected with the esterification tower, the esterification condenser and the alcohol-water separation tank in sequence; the ester heat exchanger is connected with a stripping preheater, a stripping tower, a stripping condenser and a stripping separating tank in sequence; the stripping tower is also connected with a drying tower and an ester heat exchanger in sequence.
The reaction kettle is sequentially connected with the octanol metering tank and the octanol raw material storage tank.
Preferably, the stripping separation tank is connected with an octanol raw material storage tank, so that the recovered octanol can be reused.
Preferably, the alcohol-water separation tank is connected with the esterification tower; the bottom of the esterification tower is connected with the reaction kettle.
Preferably, the primary water washing settling tank is connected with the neutralization reactor, so that water after settling separation flows back to the neutralization reactor for recycling.
Preferably, the second-stage washing settling tank is connected with the first-stage washing stirring tank, and water after the second-stage settling separation has good water quality and flows back to the first-stage washing stirring tank for recycling.
Preferably, the adsorption separator and the filter are respectively connected with the slag pool.
When the dioctyl adipate is produced, starting the continuous dioctyl adipate production device, adding excessive octanol into a reaction kettle, adding adipic acid and a modified titanate catalyst, controlling the system pressure to be less than or equal to 10KPa, controlling the temperature rise speed when the temperature rises to about 220 ℃, sampling and analyzing the acid value of a reactant when constant-temperature esterification is carried out for about 2 hours, closing heating steam of the reaction kettle when the acid value is less than 0.2mgKOH/g, and putting crude ester in the reaction kettle into a crude ester buffer tank through a heat exchanger. And (3) feeding the gas phase evaporated from the reaction kettle into an esterification tower, performing reverse contact heat exchange with reflux alcohol on the top of the tower, then feeding the gas phase into an esterification condenser for condensation, emptying non-condensable gas through an emptying line, feeding the condensed liquid into an alcohol-water separation tank through a heat exchanger for alcohol-water separation, and overflowing the alcohol from the upper part of the condensed liquid back to the esterification tower so as to maintain the excessive alcohol. The water enters a reuse water storage tank through a U-shaped pipe.
And directly conveying the crude ester into a neutralization reactor from a crude ester buffer tank by using a pump, mixing the crude ester with waste alkaline water, carrying out neutralization reaction under the stirring action, and controlling the temperature of the crude ester entering the neutralization at 80-90 ℃. Overflowing the reacted materials into a neutralization and sedimentation separation tank for carrying out ester and water phase separation, overflowing the ester from the upper part into a primary washing and stirring tank, adding fresh alkaline water, carrying out primary neutralization and washing and stirring, washing off salts and impurities, overflowing the reacted materials into the primary washing and sedimentation tank, allowing the separated water to enter a reuse water storage tank through a U-shaped pipe, and carrying out next water treatment; overflowing the separated ester to a secondary washing stirring tank, adding fresh alkaline water, carrying out secondary neutralization washing stirring, further washing to remove salts and impurities, overflowing the reacted materials to a primary washing settling tank, allowing the separated water to enter a reuse water storage tank through a U-shaped pipe, and carrying out next water treatment; the separated ester overflows to a neutralized crude ester tank.
The neutralized crude ester contains water, a small amount of low-boiling-point substances and a certain amount of alcohol, the neutralized crude ester is pumped into an ester heat exchanger by a pump for heat exchange, then the neutralized crude ester enters a stripping preheater for preheating, and then enters a stripping tower for vacuum dealcoholization, the absolute pressure at the top of the stripping tower is less than 10KPa, the crude ester is extracted from the bottom of the tower, the crude ester is further subjected to vacuum stripping by a drying tower (the absolute pressure is 1KPa), so that the content of low-boiling-point substances such as water, alcohol and the like is further reduced, and the dealcoholized crude ester is cooled by a common heat exchanger and then. And the gas at the top of the tower is condensed by a stripping condenser and then enters a stripping separation tank, the alcohol separated by the stripping separation tank enters a circulating alcohol tank, and the condensed tail gas is pumped out by a liquid ring vacuum pump and is evacuated.
In order to achieve the specified color values of the products, the dealcoholized crude esters are decolorized with activated carbon. The ester in the stripped product tank is pumped into an adsorption separator. The activated carbon and the crude ester were mixed with stirring. The crude ester containing the activated carbon is pumped to a filter for filtration, and the whole process comprises the steps of filling, pre-filtering, residual filtering, drying, slag throwing and the like. The removed active carbon is discharged into a slag pool for waste slag treatment, the residual active carbon is removed, and finally the active carbon is cooled to 50 ℃ by a common heat exchanger and is taken as a product to be sent into a finished product tank.
All the components described in the present invention are well known devices in the art, and the specific structure thereof does not need to be disclosed.
Compared with the prior art, the utility model discloses following beneficial effect has:
the utility model has the advantages of being scientific and reasonable in design, the simple operation elasticity is big, and the deformability is strong, and safety ring protects, and is with low costs, efficient, and the product quality who produces is high, can adapt to market needs.
Drawings
Fig. 1 is a schematic structural diagram of the present invention;
in the figure: 1. an octanol metering tank; 2. a reaction kettle; 3. an esterification tower; 4. an esterification condenser; 5. an alcohol-water separation tank; 6. a neutralization reactor; 7. a neutralization and sedimentation separation tank; 8. a first-stage water washing stirring tank; 9. a first-stage washing settling tank; 10. a second-stage washing stirring tank; 11. a secondary washing settling tank; 12. a neutralization crude ester tank; 13. an ester heat exchanger; 14. a stripping preheater; 15. a stripping column; 16. a stripping condenser; 17. a stripping knockout drum; 18. a drying tower; 19. a stripped product tank; 20. an adsorption separator; 21. a filter; 22. a finished product tank; 23. a crude ester buffer tank; 24. octanol raw materials storage tank.
Detailed Description
The present invention is further described with reference to the following examples, which are not intended to limit the practice of the invention.
Example 1
As shown in fig. 1, the continuous production apparatus of dioctyl adipate of the present invention, the reaction kettle 2 is connected with a crude ester buffer tank 23, a neutralization reactor 6, a neutralization settling separation tank 7, a primary washing agitator tank 8, a primary washing agitator tank 9, a secondary washing agitator tank 10, a secondary washing agitator tank 11, a neutralization crude ester tank 12, an ester heat exchanger 13, a stripping product tank 19, an adsorption separator 20, a filter 21 and a finished product tank 22 in sequence; the reaction kettle 2 is connected with an esterification tower 3, an esterification condenser 4 and an alcohol-water separation tank 5 in sequence; the ester heat exchanger 13 is connected with a stripping preheater 14, a stripping tower 15, a stripping condenser 16 and a stripping separation tank 17 in sequence; the stripping column 15 is also connected in series with a drying column 18 and an ester heat exchanger 13.
The reaction kettle 2 is sequentially connected with the octanol metering tank 1 and the octanol raw material storage tank 24.
The stripping separation tank 17 is connected with an octanol raw material storage tank 24, so that the recovered octanol can be reused.
The alcohol-water separation tank 5 is connected with the esterification tower 3; the bottom of the esterification tower 3 is connected with the reaction kettle 2.
The first-stage washing settling tank 9 is connected with the neutralization reactor 6, so that water after settling separation flows back to the neutralization reactor 6 for recycling.
The second grade washing settling cask 11 links to each other with first grade washing agitator tank 8, and the quality of water after the second grade sedimentation separation is better, flows back to first grade washing agitator tank 8, carries out cyclic utilization.
The adsorption separator 20 and the filter 21 are respectively connected with the slag pool.
When the dioctyl adipate is produced, starting the continuous dioctyl adipate production device, adding excessive octanol into the reaction kettle 2, adding adipic acid and a modified titanate catalyst, controlling the system pressure to be less than or equal to 10KPa, controlling the temperature rise speed when the temperature rises to about 220 ℃, sampling and analyzing the acid value of a reactant when constant-temperature esterification is carried out for 2 hours, closing heating steam of the reaction kettle 2 when the acid value is 0.18mgKOH/g, and putting the crude ester in the reaction kettle 2 into a crude ester buffer tank 23 through a heat exchanger. The gas phase evaporated from the reaction kettle 2 enters an esterification tower 3, enters an esterification condenser 4 for condensation after being in reverse contact heat exchange with reflux alcohol at the top of the tower, noncondensable gas is discharged from a vent line, condensed liquid enters an alcohol-water separation tank 5 for alcohol-water separation after passing through a heat exchanger, and alcohol overflows from the upper part and returns to the esterification tower 3 so as to maintain the excessive alcohol. The water enters a reuse water storage tank through a U-shaped pipe.
The crude ester is directly sent to the neutralization reactor 6 from the crude ester buffer tank 23 by a pump, is mixed with the waste alkaline water, is subjected to neutralization reaction under the stirring action, and the temperature of the crude ester entering the neutralization is controlled at 85 +/-3 ℃. The reacted materials overflow into a neutralization and sedimentation separation tank 7 for ester and water phase separation, the ester overflows into a primary washing and stirring tank 8 from the upper part, fresh alkaline water is added for primary neutralization and washing and stirring, salts and impurities are washed away, the reacted materials overflow into a primary washing and sedimentation tank 9, the separated water enters a reuse water storage tank through a U-shaped pipe and then is subjected to next water treatment; overflowing the separated ester to a secondary washing stirring tank 10, adding fresh alkaline water, carrying out secondary neutralization washing stirring, further washing to remove salts and impurities, overflowing the reacted materials to a primary washing settling tank 11, allowing the separated water to enter a reuse water storage tank through a U-shaped pipe, and carrying out next water treatment; the separated ester overflows to a neutralized crude ester tank 12.
The neutralized crude ester contains water, a small amount of low boiling point substances and a certain amount of alcohol, the neutralized crude ester is pumped into an ester heat exchanger 13 by a pump for heat exchange, then the neutralized crude ester enters a stripping preheater 14 for preheating, and then enters a stripping tower 15 for vacuum dealcoholization, the absolute pressure at the top of the stripping tower 15 is less than 10KPa, the crude ester is extracted from the bottom of the tower, the crude ester is further subjected to vacuum stripping by a drying tower 18 (the absolute pressure is 1KPa), so that the content of low boiling point substances such as water, alcohol and the like is further reduced, and the dealcoholized crude ester is cooled by a common heat exchanger and then sent to a. The gas at the top of the tower is condensed by a stripping condenser 16 and then enters a stripping separation tank 17, the alcohol separated by the stripping separation tank 17 enters a circulating alcohol tank, and the condensed tail gas is pumped out by a liquid ring vacuum pump and is evacuated.
In order to achieve the specified color values of the products, the dealcoholized crude esters are decolorized with activated carbon. The ester in the stripped product tank 19 is directed to an adsorption separator 20. The bagged active carbon is lifted to a 13M frame by a lifter, added into a hopper bin, sent to an adsorption separator 20 through a screw conveyor, and stirred and mixed with crude ester, wherein the adding amount of the active carbon is as follows: the DOA is produced to be 2 kg/ton product, the crude ester containing the active carbon is pumped to a filter 21 for filtration, and the whole process comprises the steps of filling, pre-filtering, filtering the rest, drying, slag throwing and the like. The removed activated carbon is discharged into a slag pool for waste slag treatment, the residual activated carbon is removed, and finally the activated carbon is cooled to 50 ℃ by a common heat exchanger and is sent to a finished product tank 22 as a product.
Utilize the utility model discloses the dioctyl adipate that production obtained, with utilize the dioctyl adipate that current production intermittent type device production obtained, carry out the performance contrast, see table 1 as a result.
TABLE 1
Claims (7)
1. A serialization apparatus for producing of dioctyl adipate which characterized in that: the reaction kettle (2) is sequentially connected with a crude ester buffer tank (23), a neutralization reactor (6), a neutralization and sedimentation separation tank (7), a primary washing stirring tank (8), a primary washing sedimentation tank (9), a secondary washing stirring tank (10), a secondary washing sedimentation tank (11), a neutralization crude ester tank (12), an ester heat exchanger (13), a stripping product tank (19), an adsorption separator (20), a filter (21) and a finished product tank (22); the reaction kettle (2) is connected with the esterification tower (3), the esterification condenser (4) and the alcohol-water separation tank (5) in sequence; the ester heat exchanger (13) is connected with a stripping preheater (14), a stripping tower (15), a stripping condenser (16) and a stripping separating tank (17) in sequence; the stripping tower (15) is also connected with a drying tower (18) and an ester heat exchanger (13) in sequence.
2. The continuous dioctyl adipate producing apparatus according to claim 1, wherein: the reaction kettle (2) is connected with the octanol metering tank (1) and the octanol raw material storage tank (24) in sequence.
3. The continuous dioctyl adipate producing apparatus according to claim 1, wherein: the stripping separation tank (17) is connected with an octanol raw material storage tank (24).
4. The continuous dioctyl adipate producing apparatus according to claim 1, wherein: the alcohol-water separation tank (5) is connected with the esterification tower (3); the bottom of the esterification tower (3) is connected with the reaction kettle (2).
5. The continuous dioctyl adipate producing apparatus according to claim 1, wherein: the first-stage washing settling tank (9) is connected with the neutralization reactor (6).
6. The continuous dioctyl adipate producing apparatus according to claim 1, wherein: the secondary washing settling tank (11) is connected with the primary washing stirring tank (8).
7. The continuous dioctyl adipate producing apparatus according to claim 1, wherein: the adsorption separator (20) and the filter (21) are respectively connected with the slag pool.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201921177509.8U CN210261601U (en) | 2019-07-24 | 2019-07-24 | Continuous production device of dioctyl adipate |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201921177509.8U CN210261601U (en) | 2019-07-24 | 2019-07-24 | Continuous production device of dioctyl adipate |
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| CN210261601U true CN210261601U (en) | 2020-04-07 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114307926A (en) * | 2021-12-28 | 2022-04-12 | 浙江伟博化工科技有限公司 | Continuous production device and production process for dioctyl adipate |
| CN117486716A (en) * | 2023-12-28 | 2024-02-02 | 天津渤化澳佳永利化工有限责任公司 | DOA production method |
-
2019
- 2019-07-24 CN CN201921177509.8U patent/CN210261601U/en active Active
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114307926A (en) * | 2021-12-28 | 2022-04-12 | 浙江伟博化工科技有限公司 | Continuous production device and production process for dioctyl adipate |
| CN117486716A (en) * | 2023-12-28 | 2024-02-02 | 天津渤化澳佳永利化工有限责任公司 | DOA production method |
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