CN108250065B - Device and method for recovering perfluorooctanoic acid from fluoropolymer drying tail gas - Google Patents
Device and method for recovering perfluorooctanoic acid from fluoropolymer drying tail gas Download PDFInfo
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- CN108250065B CN108250065B CN201611236219.7A CN201611236219A CN108250065B CN 108250065 B CN108250065 B CN 108250065B CN 201611236219 A CN201611236219 A CN 201611236219A CN 108250065 B CN108250065 B CN 108250065B
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Abstract
The invention relates to a device and a method for recovering perfluorooctanoic acid from tail gas generated in the process of drying fluorine-containing polymer by a vacuum oven. The recovery device comprises a vacuum oven, a buffer tank, a water ring vacuum pump, a water tank, a distillation tower and a rectifying tower which are connected in sequence; wherein the water ring vacuum pump forms a water circulation unit with the water tank through the heat exchanger. The invention utilizes the recovery device to recover the perfluorooctanoic acid, and has good recovery effect and short process flow. The concentrated solution of the high-concentration perfluorooctanoic acid enriched in the buffer tank can be directly used or continuously rectified to obtain the perfluorooctanoic acid; in addition, a small amount of perfluorooctanoic acid in the circulating water can be effectively recovered after distillation and rectification. The perfluoro caprylic acid recovered by the recovery device and the method has the advantages of about 72 percent of recovery rate, more than 99.8 percent of purity and high practical value.
Description
Technical Field
The invention belongs to the field of chemical waste gas treatment, and particularly relates to a method and equipment for enriching and recovering perfluorooctanoic acid from tail gas generated by drying fluorine-containing polymers.
Background
Common fluoropolymer drying methods mainly include vacuum drying and hot air circulation drying. Wherein, in the vacuum drying method, the fluorine-containing polymer is heated to 120-200 ℃, and water is evaporated with the ammonium perfluorooctanoate and the perfluorooctanoic acid and is gradually pumped away along with vacuum pumping. In order to prevent the contamination of perfluorooctanoic acid, it is necessary to recover perfluorooctanoic acid in the dry fluoropolymer tail gas.
In the prior art, an absorption tower is mainly used for absorbing perfluorooctanoic acid. In CN201310332105.2, the absorption liquid is used for absorbing the tail gas containing the perfluorooctanoic acid steam, and the absorption liquid after absorbing the perfluorooctanoic acid adopts a nanofiltration membrane or a reverse osmosis membrane to concentrate perfluorooctanoic acid salt in the absorption liquid. The method needs to be put into a tail gas absorption tower, the investment and operation cost is high, and the perfluorooctanoic acid is easy to accumulate in a hot air pipe before entering the absorption tower.
Disclosure of Invention
Aiming at the defects in the prior art, the invention provides a method for recovering perfluorooctanoic acid from tail gas generated by drying a fluorine-containing polymer in a vacuum oven and a matched device thereof. The method directly uses the evacuation system of the vacuum oven, does not need to build a new tail gas absorption device, and has good recovery effect and short process flow.
The scheme of the invention is as follows:
a device for recovering perfluorooctanoic acid from tail gas generated in the drying of fluorine-containing polymers comprises a vacuum oven, a buffer tank, a water ring vacuum pump, a water tank, a distillation tower and a rectifying tower which are sequentially connected; wherein the water ring vacuum pump forms a water circulation unit with the water tank through the heat exchanger.
The invention directly utilizes the evacuation system of the existing vacuum oven to treat the tail gas containing the perfluorooctanoic acid, does not need to newly build a tail gas absorption device, effectively reduces the recovery cost, has good recovery effect and short process flow, and is very suitable for industrial popularization.
The recovery apparatus is described in detail below:
the difference is that the connecting pipeline of the vacuum oven and the buffer tank in the existing evacuation system is only connected with the air inlet at the top of the buffer tank, and the connecting pipeline of the vacuum oven and the buffer tank in the recovery device provided by the invention needs to extend into the middle of the buffer tank from the top of the buffer tank, so that full condensation of the perfluorooctanoic acid in the buffer tank can be ensured, and the recovery rate of the perfluorooctanoic acid is improved.
The buffer tank does not need heat preservation treatment, but needs heat preservation treatment on a connecting pipeline of an air inlet of the buffer tank so as to adjust the temperature of the buffer tank. The heat preservation treatment is a conventional pipeline heat preservation method which is known to those skilled in the art, and the present invention is not particularly limited thereto.
The heat exchanger is selected from a plate heat exchanger or a shell and tube heat exchanger.
And a liquid outlet at the bottom of the buffer tank is connected with a next device which can directly utilize the concentrated solution of the perfluorooctanoic acid, or is connected with another liquid inlet pipeline of the rectifying tower, so that the further rectification and recovery are facilitated.
The working principle of the recovery device is as follows:
after the fluoropolymer is dried by a vacuum oven, tail gas enters a buffer tank, most of the perfluorooctanoic acid in the tail gas is concentrated in vacuum and then is discharged from the bottom of the buffer tank and enters a rectifying tower; meanwhile, the water ring vacuum pump provides negative pressure for the vacuum oven and the buffer tank, the residual perfluoro caprylic acid in the buffer tank enters the water ring vacuum pump along with the tail gas, and most of the residual perfluoro caprylic acid in the tail gas is absorbed by circulating water in the cavity of the water ring vacuum pump and enters the water tank along with the circulating water to be enriched; meanwhile, in order to further reduce the content of the perfluorooctanoic acid in the tail gas, the tail gas discharged by the water ring vacuum pump is introduced into a water tank for continuous enrichment so as to further remove the residual trace perfluorooctanoic acid in the tail gas; and (3) continuously circulating water among the water tank, the heat exchanger and the water ring vacuum pump, continuously accumulating the perfluorooctanoic acid in the water tank, and when the mass concentration of the perfluorooctanoic acid in the water tank reaches about 10%, conveying the aqueous solution containing the perfluorooctanoic acid to a distillation tower for concentration and a rectification tower for treatment, and recovering the perfluorooctanoic acid.
The invention also provides a method for recovering perfluorooctanoic acid from tail gas generated in drying fluoropolymer, which comprises the following steps:
1) after the fluoropolymer is dried by a vacuum oven, tail gas of the fluoropolymer enters a buffer tank for vacuum concentration, and most of the perfluoro caprylic acid in the tail gas is enriched at the bottom of the buffer tank to form a concentrated solution;
2) residual perfluorooctanoic acid which is not enriched in the buffer tank enters a water ring vacuum pump along with tail gas, and is mixed with circulating water for heat and mass transfer; at the moment, most of the perfluoro caprylic acid and the perfluoro ammonium caprylate in the tail gas are absorbed by the circulating water in the cavity of the water ring vacuum pump and enter the water tank along with the circulating water for enrichment; the residual unabsorbed trace perfluorooctanoic acid is discharged from the water ring vacuum pump along with the tail gas and then enters a water tank for further enrichment; the water in the water tank is circulated to the water ring vacuum pump through the heat exchanger;
3) the method comprises the following steps that with the continuous circulation of circulating water among a water tank, a heat exchanger and a water ring vacuum pump and the introduction of tail gas, the perfluoro caprylic acid in the water tank is accumulated continuously, and when the mass concentration of the perfluoro caprylic acid in the water tank reaches a specified concentration, a water solution containing the perfluoro caprylic acid is conveyed to a distillation tower for concentration and a rectification tower for treatment, and the perfluoro caprylic acid is recovered.
In the above recovery method step 1), the temperature of the vacuum oven is raised from normal temperature to 120 ℃ for about 3 hours, most of the water entrained in the resin is evaporated in the period, meanwhile, the surfactant ammonium perfluorooctanoate is decomposed into perfluorooctanoic acid and ammonia, the ammonia is evaporated firstly due to low boiling point, the perfluorooctanoic acid still remains in the resin due to high boiling point, and the water vapor and the ammonia are partially condensed in the buffer tank; cutting off an inlet valve and an outlet valve of the buffer tank at 120-140 ℃, and discharging accumulated water in the buffer tank into a circulating water tank from a bottom valve; and continuously heating, and finally, keeping the stable operation temperature of the vacuum oven at 140-180 ℃.
In the step 1) of the recovery method, the vacuum concentration conditions in the buffer tank are as follows: the operating vacuum degree is 60-80kPa, and preferably 70 kPa; the temperature is 70-120 ℃, preferably 80-110 ℃. The invention adjusts the temperature of the buffer tank by partially insulating the pipeline before entering the buffer tank, thereby effectively saving energy.
When the temperature of the vacuum oven exceeds 130 ℃, the perfluorooctanoic acid gradually evaporates. At this time, the perfluorooctanoic acid in the tail gas is mostly enriched in the buffer tank. Because a large amount of water is discharged in the early stage, and the temperature of the buffer tank is kept between 70 and 120 ℃, the whole buffer tank is equivalent to a set of vacuum concentration device, and the concentration of the concentrated solution of the perfluorooctanoic acid enriched in the buffer tank is very high and can reach more than 50 percent.
In the above recovery method, step 1), the concentrated solution may be used directly as a solution, or may be further fed to a rectifying column.
In the step 2) of the recovery method, in the water ring vacuum pump, the high-temperature tail gas and the circulating water exchange mass transfer to gradually increase the water temperature. In order to prevent the normal operation of equipment from being influenced by overhigh water temperature, the temperature of circulating water after heat exchange needs to be controlled to be not higher than 60 ℃.
In the step 3) of the recovery method, when the mass concentration of the perfluorooctanoic acid in the water tank reaches 8 to 12%, the aqueous solution containing the perfluorooctanoic acid is conveyed to a distillation column for concentration, and simultaneously, deionized water is supplemented into the water tank.
As a preferred embodiment of the invention, the method for recovering the perfluorooctanoic acid from the fluoropolymer drying tail gas comprises the following steps:
1) after the fluoropolymer is dried by a vacuum oven, tail gas of the fluoropolymer enters a buffer tank for vacuum concentration, and most of the perfluoro caprylic acid in the tail gas is enriched at the bottom of the buffer tank to form a concentrated solution;
the stable working temperature of the vacuum oven is 140-180 ℃;
the vacuum concentration conditions in the buffer tank are as follows: the operating vacuum degree is 60-80kPa, and preferably 70 kPa; the temperature is 70-120 ℃, preferably 80-110 ℃;
2) residual perfluorooctanoic acid which is not enriched in the buffer tank enters a water ring vacuum pump along with tail gas, and is mixed with circulating water for heat and mass transfer; at the moment, most of the perfluoro caprylic acid and the perfluoro ammonium caprylate in the tail gas are absorbed by the circulating water in the cavity of the water ring vacuum pump and enter the water tank along with the circulating water for enrichment; the residual unabsorbed trace perfluorooctanoic acid is discharged from the water ring vacuum pump along with the tail gas and then enters a water tank for further enrichment; the water in the water tank is circulated to the water ring vacuum pump through the heat exchanger;
the water temperature of the circulating water is controlled to be not more than 60 ℃;
3) with the continuous circulation of circulating water among the water tank, the heat exchanger and the water ring vacuum pump and the introduction of tail gas, the perfluoro caprylic acid in the water tank is continuously accumulated, and when the mass concentration of the perfluoro caprylic acid in the water tank reaches a specified concentration, the aqueous solution containing the perfluoro caprylic acid is conveyed to a distillation tower for concentration and a rectification tower for treatment, and the perfluoro caprylic acid is recovered;
when the mass concentration of the perfluorooctanoic acid in the water tank reaches 8-12%, the aqueous solution containing the perfluorooctanoic acid is conveyed to a distillation tower for concentration, and simultaneously deionized water is supplemented into the water tank.
The invention has the beneficial effects that:
the method directly utilizes the evacuation system of the vacuum oven to recover the perfluorooctanoic acid in the tail gas, does not need to newly build a tail gas absorption device (such as an absorption tower), and has good recovery effect and short process flow. The concentrated solution of the high-concentration perfluorooctanoic acid enriched in the buffer tank can be directly used or continuously rectified to obtain the perfluorooctanoic acid; in addition, a small amount of perfluorooctanoic acid in the circulating water can be effectively recovered after distillation and rectification. The perfluoro caprylic acid recovered by the recovery device and the method has the advantages of about 72 percent of recovery rate, more than 99.8 percent of purity and high practical value.
Drawings
Fig. 1 shows a perfluorooctanoic acid recovery apparatus according to the present invention.
Detailed Description
The following examples are intended to illustrate the invention but are not intended to limit the scope of the invention.
Example 1
As in fig. 1. The embodiment provides a device for recovering perfluorooctanoic acid from tail gas generated in drying fluorine-containing polymers, which comprises a vacuum oven, a buffer tank, a water ring vacuum pump, a water tank, a distillation tower and a rectifying tower which are sequentially connected; wherein the water ring vacuum pump and the water tank form a water circulation unit through the heat exchanger;
in the recovery device, the connecting pipeline between the vacuum oven and the buffer tank needs to extend into the middle of the buffer tank from the top of the buffer tank, so that full condensation of the perfluorooctanoic acid in the buffer tank can be ensured, and the recovery rate of the perfluorooctanoic acid is improved.
The buffer tank does not need heat preservation treatment, but partial heat preservation is carried out at the position of the air inlet connecting pipeline of the buffer tank so as to adjust the temperature of the buffer tank.
The heat exchanger is selected from a plate condenser.
And a liquid outlet at the bottom of the buffer tank is connected with another liquid inlet pipeline of the rectifying tower so as to be convenient for further rectification and recovery.
Example 2
The embodiment provides a method for recovering perfluorooctanoic acid from polytetrafluoroethylene vacuum drying tail gas by using the recovery device in embodiment 1, which comprises the following steps:
1) after the fluoropolymer is dried by a vacuum oven, tail gas of the fluoropolymer enters a buffer tank for vacuum concentration, and most of the perfluoro caprylic acid in the tail gas is enriched at the bottom of the buffer tank to form a concentrated solution;
wherein, the temperature of the vacuum oven is increased from normal temperature to 120 ℃ for about 3 hours, most of water carried in the resin is evaporated in the time, meanwhile, the surfactant ammonium perfluorooctanoate is decomposed into perfluorooctanoic acid and ammonia, the ammonia is evaporated firstly due to low boiling point, and the perfluorooctanoic acid is still remained in the resin due to high boiling point. This water vapor, ammonia, will partially condense in the buffer tank. And (4) cutting off an inlet valve and an outlet valve of the buffer tank at 120-140 ℃, and discharging accumulated water in the buffer tank into the circulating water tank from the bottom valve. And continuously heating, wherein the final stable operation temperature of the oven is 140-180 ℃.
When the temperature of the oven exceeds 130 ℃, the perfluorooctanoic acid gradually evaporates. At this time, the perfluorooctanoic acid in the tail gas is mostly enriched in the buffer tank. Because a large amount of water pumped out in the earlier stage is discharged, and the temperature of the buffer tank is kept between 70 and 120 ℃ all the time in the drying process, the whole buffer tank is equivalent to a set of vacuum concentration device, and the concentration of the recovered perfluoro caprylic acid in the buffer tank is very high and can reach more than 50 percent. After the purification is finished, the perfluoro caprylic acid enriched in the buffer tank can be directly used in a solution mode, and can also be sent to a rectifying device for continuous purification.
2) The tail gas passing through the buffer tank also contains a small part of perfluoro caprylic acid which enters the impeller of the circulating vacuum pump along with the tail gas, and is mixed with circulating water to transfer heat and mass, and the perfluoro caprylic acid enters the circulating water.
The high-temperature tail gas exchanges heat with circulating water, so that the temperature of the circulating water is gradually increased. In order to prevent the normal operation of equipment from being influenced by overhigh circulating water temperature, the circulating water is cooled in the drying process, and the circulating water temperature is controlled to be not higher than 60 ℃.
3) When the mass concentration of the perfluorooctanoic acid in the circulating water solution reaches about 10%, the water solution in the water tank is pumped to a distillation tower for concentration and a rectification system for continuous treatment. Taking a product with the boiling point of 190 ℃, and finally obtaining the perfluorooctanoic acid with the mass content of 99.8%.
In this embodiment, most of the perfluoro caprylic acid in the tail gas pumped out by the vacuum oven is enriched in the buffer tank, the residual perfluoro caprylic acid is contacted and mixed with the circulating water in the water ring vacuum pump along with the tail gas, and the ammonium perfluoro caprylate and the perfluoro caprylic acid contained in the gas are dissolved in the circulating water and enter the water tank for enrichment. And introducing the tail gas passing through the water ring vacuum pump below the liquid level of the circulating water tank to further absorb the residual perfluorooctanoic acid in the tail gas.
According to the charging amount of the reaction kettle, the recovery rate of the sum of the perfluorooctanoic acid in the buffer tank and the circulating water tank is about 72 percent (the rest of the perfluorooctanoic acid enters the condensation water during condensation), which is shown in table 1.
TABLE 1 recovery of perfluorooctanoic acid at different operating temperatures of the buffer tank (vacuum 70kPa)
| Operating temperature/. degree.C | 80 | 90 | 100 | 110 |
| Percent recovery in surge tank% | 64.7 | 62.8 | 60.1 | 57.3 |
| Concentration/% of perfluorooctanoic acid in buffer tank | 50.7 | 52.6 | 53.2 | 55.4 |
| Percent recovery in the circulating water tank/%) | 9.9 | 13.4 | 14.9 | 16.0 |
| Total recovery% | 72.6 | 71.8 | 73.8 | 71.3 |
Although the invention has been described in detail hereinabove with respect to a general description and specific embodiments thereof, it will be apparent to those skilled in the art that modifications or improvements may be made thereto based on the invention. Accordingly, such modifications and improvements are intended to be within the scope of the invention as claimed.
Claims (7)
1. A method for recovering perfluorooctanoic acid from fluoropolymer drying tail gas is characterized by comprising the following steps:
1) after the fluoropolymer is dried by a vacuum oven, tail gas of the fluoropolymer enters a buffer tank for vacuum concentration, and most of the perfluoro caprylic acid in the tail gas is enriched at the bottom of the buffer tank to form a concentrated solution;
2) residual perfluorooctanoic acid which is not enriched in the buffer tank enters a water ring vacuum pump along with tail gas, and is mixed with circulating water for heat and mass transfer; at the moment, most of the perfluoro caprylic acid and the perfluoro ammonium caprylate in the tail gas are absorbed by the circulating water in the cavity of the water ring vacuum pump and enter the water tank along with the circulating water for enrichment; the residual unabsorbed trace perfluorooctanoic acid is discharged from the water ring vacuum pump along with the tail gas and then enters a water tank for further enrichment; the water in the water tank is circulated to the water ring vacuum pump through the heat exchanger;
3) with the continuous circulation of circulating water among the water tank, the heat exchanger and the water ring vacuum pump and the introduction of tail gas, the perfluoro caprylic acid in the water tank is continuously accumulated, and when the mass concentration of the perfluoro caprylic acid in the water tank reaches 8-12%, the aqueous solution containing the perfluoro caprylic acid is conveyed to a distillation tower for concentration and a rectification tower for treatment, and the perfluoro caprylic acid is recovered.
2. The method for recovering perfluorooctanoic acid from fluoropolymer drying off-gas according to claim 1, wherein in step 1), the temperature of the vacuum oven is 140 to 180 ℃.
3. The method for recovering perfluorooctanoic acid from fluoropolymer drying off-gas according to claim 1, wherein in step 1), the vacuum concentration conditions in the buffer tank are as follows: the operation vacuum degree is 60-80 kPa; the temperature is 70-120 ℃.
4. The method for recovering perfluorooctanoic acid from fluoropolymer drying off-gas according to claim 3, wherein in step 1), the vacuum concentration conditions in the buffer tank are as follows: the vacuum degree is 70kPa, and the temperature is 80-110 ℃.
5. The method for recovering perfluorooctanoic acid from fluoropolymer drying off-gas according to claim 1, wherein in step 3), when the concentration of perfluorooctanoic acid in the water tank reaches 8 to 12% by mass, the aqueous solution containing perfluorooctanoic acid is sent to a distillation column for concentration, and deionized water is added to the water tank.
6. The method of claim 1, comprising the steps of:
1) after the fluoropolymer is dried by a vacuum oven, tail gas of the fluoropolymer enters a buffer tank for vacuum concentration, and most of the perfluoro caprylic acid in the tail gas is enriched at the bottom of the buffer tank to form a concentrated solution;
the stable working temperature of the vacuum oven is 140-180 ℃;
the vacuum concentration conditions in the buffer tank are as follows: the operation vacuum degree is 60-80 kPa; the temperature is 70-120 ℃;
2) residual perfluorooctanoic acid which is not enriched in the buffer tank enters a water ring vacuum pump along with tail gas, and is mixed with circulating water for heat and mass transfer; at the moment, most of the perfluoro caprylic acid and the perfluoro ammonium caprylate in the tail gas are absorbed by the circulating water in the cavity of the water ring vacuum pump and enter the water tank along with the circulating water for enrichment; the residual unabsorbed trace perfluorooctanoic acid is discharged from the water ring vacuum pump along with the tail gas and then enters a water tank for further enrichment; the water in the water tank is circulated to the water ring vacuum pump through the heat exchanger;
the water temperature of the circulating water is controlled to be not more than 60 ℃;
3) with the continuous circulation of circulating water among the water tank, the heat exchanger and the water ring vacuum pump and the introduction of tail gas, the perfluoro caprylic acid in the water tank is continuously accumulated, when the mass concentration of the perfluoro caprylic acid in the water tank reaches 8-12%, the aqueous solution containing the perfluoro caprylic acid is conveyed to a distillation tower for concentration and a rectification tower for treatment, and the perfluoro caprylic acid is recovered; and simultaneously supplying deionized water to the water tank.
7. The method for recovering perfluorooctanoic acid from fluoropolymer dry tail gas according to claim 6, wherein in step 1), the vacuum concentration conditions in the buffer tank are as follows: the operation vacuum degree is 70 kPa; the temperature is 80-110 ℃.
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| CN107501081B (en) * | 2017-09-15 | 2023-05-26 | 四川宏图普新微波科技有限公司 | System and method for recycling perfluoro caprylic acid from polytetrafluoroethylene dispersion resin particle wet material |
Citations (4)
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| JPH07102357B2 (en) * | 1991-08-12 | 1995-11-08 | 新日本製鐵株式会社 | Apparatus and method for treating water containing organochlorine compound |
| CN101496981A (en) * | 2009-01-20 | 2009-08-05 | 郝璐 | Method for purifying methyl isobutyl ketone exhaust gas in vacuum system using waste compressor oil |
| CN102643189A (en) * | 2012-03-31 | 2012-08-22 | 中昊晨光化工研究院 | System and method for recovering perfluoro caprylic acid from tail gas |
| CN202440456U (en) * | 2011-12-30 | 2012-09-19 | 金发科技股份有限公司 | Device for treating tail gas during production process of polyester or copolyester |
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2016
- 2016-12-28 CN CN201611236219.7A patent/CN108250065B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH07102357B2 (en) * | 1991-08-12 | 1995-11-08 | 新日本製鐵株式会社 | Apparatus and method for treating water containing organochlorine compound |
| CN101496981A (en) * | 2009-01-20 | 2009-08-05 | 郝璐 | Method for purifying methyl isobutyl ketone exhaust gas in vacuum system using waste compressor oil |
| CN202440456U (en) * | 2011-12-30 | 2012-09-19 | 金发科技股份有限公司 | Device for treating tail gas during production process of polyester or copolyester |
| CN102643189A (en) * | 2012-03-31 | 2012-08-22 | 中昊晨光化工研究院 | System and method for recovering perfluoro caprylic acid from tail gas |
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