CN219272164U - System for recycling and purifying dibasic acid in adipic acid production waste liquid - Google Patents
System for recycling and purifying dibasic acid in adipic acid production waste liquid Download PDFInfo
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- CN219272164U CN219272164U CN202223057438.2U CN202223057438U CN219272164U CN 219272164 U CN219272164 U CN 219272164U CN 202223057438 U CN202223057438 U CN 202223057438U CN 219272164 U CN219272164 U CN 219272164U
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Abstract
The application belongs to the technical field of chemical mechanical equipment, and particularly relates to a system for recycling and purifying dibasic acid in adipic acid production waste liquid. The system comprises: the device comprises a climbing film evaporator, a separator, a dibasic acid recovery crystallization unit, a centrifugal separation device, a decoloring tank and a dibasic acid evaporation flaking unit which are sequentially connected through pipelines. The DBA product quality can be further improved and promoted through the impurity removal and decoloration operations such as proper concentration and enrichment (the concentration of materials entering the binary acid evaporation flaking system is increased to 50% from the existing concentration of 20%), cooling centrifugation, dissolution decoloration and the like. By combining with the adjustment of related process parameters, the preliminary application effect shows that the purity of the existing finished product is further improved to 99.7 percent by about 99.3 percent, and the nitric acid content of 0.5 percent and the water content of 0.5 percent of the existing finished product are further reduced to less than or equal to 0.1 percent of nitric acid and less than or equal to 0.3 percent of water, so that the method has better technical significance for improving the quality of DBA products and the value of the DBA products.
Description
Technical Field
The application belongs to the technical field of chemical mechanical equipment, and particularly relates to a system for recycling and purifying dibasic acid in adipic acid production waste liquid.
Background
Adipic acid is an important chemical production raw material and has wide application in the fields of organic synthesis industry, medicine, lubricant manufacture, industrial production and preparation of nylon 66, engineering plastics and the like.
The industrial production of adipic acid is achieved by, at the earliest, taking cyclohexanol as a raw material and then preparing it by nitric acid oxidation (phenol hydrogenation). After 60 s, along with the development of other chemical industries, the production process using cyclohexane as a raw material is gradually changed in industrial production. Namely, the intermediate product cyclohexanone and cyclohexanol mixture (namely ketol oil, also called KA oil) is prepared from cyclohexane, and then oxidation is carried out to prepare adipic acid. In the oxidation process of KA oil, a process route is to take excessive nitric acid as an oxidant, and then the oxidation reaction is realized under the condition of a catalyst and proper reaction conditions, and the adipic acid prepared by the process route has higher yield and higher purity, so that the adipic acid is widely applied to industrial production.
In actual production, main components in adipic acid production waste liquid comprise: about 4% SA (succinic acid), about 13% GA (glutaric acid) and about 4% ADA (adipic acid), wherein the SA/GA/ADA mixture is also commonly referred to as DBA, and the DBA accounts for about 20% in the adipic acid production waste liquid, and the adipic acid production waste liquid contains less than 3% of nitric acid. DBA has wide application as a chemical production raw material, so in actual production, DBA in adipic acid production waste liquid needs to be recovered to improve industrial yield, and meanwhile, the environmental protection treatment cost can be reduced. In the prior art, during DBA extraction, adipic acid production waste liquid is directly sent to a binary acid evaporation flaking system for evaporation flaking, but DBA flaking prepared by the direct production mode is poor in purity (about 99.3%), is mostly yellow-green in color and is high in nitric acid content (about 0.5%), so that the production application range of the obtained DBA product is severely restricted, and the added value of the product of the extracted DBA product is also restricted.
Disclosure of Invention
The application aims to provide a system for recovering and purifying binary acid in adipic acid production waste liquid, so that a certain technical foundation is laid for effectively extracting and obtaining high-purity DBA products.
The technical scheme adopted by the application is described in detail below.
A system for recovering and purifying dibasic acid in adipic acid production waste liquid comprises: the device comprises a climbing film evaporator, a separator, a dibasic acid recovery crystallization unit, a centrifugal separation device, a dissolution and decoloration tank and a dibasic acid evaporation flaking unit which are sequentially connected through pipelines;
wherein:
the climbing film evaporator is connected with a raw material tank for storing adipic acid production waste liquid to be purified through a pipeline; in actual design, a material tank discharge pump is designed on a connecting pipeline between the evaporator and the material tank so as to pump adipic acid production waste liquid in the material tank into the evaporator;
the climbing film evaporator takes low-pressure steam as a heat source and is used for performing preliminary evaporation treatment on adipic acid production waste liquid, and the discharging temperature is controlled to be about 85 ℃;
the separator is specifically, for example, a cyclone separator is used for separating the gas-liquid mixture after evaporation treatment of the climbing film evaporator, wherein the gas phase is discharged into the atmosphere after further recovery treatment, and the liquid phase part enters a subsequent binary acid recovery crystallization unit;
in practical design, the top of the cyclone separator is connected with a vacuum system to maintain the negative pressure state (absolute pressure is 70-80 KPa) in the cyclone separator, thereby being beneficial to the rapid evaporation of the climbing film evaporator;
the dibasic acid recovery crystallization unit comprises a plurality of dibasic acid recovery crystallizers which are connected in series; the dibasic acid recovery crystallizer is used for cooling and crystallizing the liquid phase separated by the separator (separating out dibasic acid); each diacid recovery crystallizer is correspondingly connected with a cooling device (a cooling coil pipe provided with a chilled water inlet pipeline and a chilled water outlet pipeline is generally adopted, so that the cooling crystallization temperature of each diacid recovery crystallizer can be regulated and controlled according to the need);
in the preferred design, the top of the dibasic acid recovery crystallizer is provided with a recovery crystallization stirring device which is used for ensuring that the recovery liquid is uniformly cooled;
in the concrete design, the number of the dibasic acid recovery crystallizers can be 3, and the recovery liquid can sequentially overflow from high to low to enter the next dibasic acid recovery crystallizer by depending on the level difference among different dibasic acid recovery crystallizers after cooling in order to save power; in practical design, each dibasic acid recovery crystallizer can be respectively connected with the existing negative pressure system, so that the inside of the dibasic acid recovery crystallizer is kept in a micro negative pressure state (the vacuum degree is about 140mm water column), and the stable and orderly flow of the recovery liquid is ensured;
after running for a certain time, in order to clean the dibasic acid recovery crystallizer, the dibasic acid recovery crystallizer is connected with a low-pressure steam pipeline and a condensed water discharge pipeline, and low-pressure cleaning steam enters the dibasic acid recovery crystallizer through a coil pipe to heat and clean the dibasic acid recovery crystallizer;
the centrifugal separation device specifically comprises: a centrifugal machine connected with a filter cake washing water (cold high-purity water, 0.6MPa,10 ℃) pipeline and used for centrifugally dehydrating and washing the recovered liquid after the crystallization of the dibasic acid, wherein after the centrifugal washing, the impurity content of the filter cake with the main body of the dibasic acid is further reduced, and the obtained filter cake enters a dissolving and decoloring tank for further treatment;
the dissolution and decoloration tank is used for further performing decoloration and impurity removal treatment after dissolving the filter cake separated by the centrifugal separation device; an active carbon inlet for decoloring and impurity removing and a dissolution water inlet for dissolution are arranged at the upper part of the tank body;
in order to further ensure sufficient dissolution and decoloration, a dissolution and decoloration tank stirrer is designed at the top of the tank body, and/or a dissolution and decoloration tank low-pressure steam inlet and a corresponding dissolution and decoloration tank condensate outlet (the temperature of the dissolution liquid is properly raised, thereby accelerating dissolution) are designed on the tank body;
the carbon filter is used for filtering and removing active carbon in the dissolved and decolored solution; in actual production, a discharging pump of the dissolution and decoloration tank is designed on a connecting pipeline of the carbon filter and the dissolution and decoloration tank and is used for pumping the dissolution and decoloration solution into the carbon filter;
further, the carbon filter is also matched with a sight glass and a carbon protection filter, so that the filtering condition of the carbon filter can be intuitively judged and the stable operation of the carbon filter can be ensured;
the dibasic acid evaporation and flaking unit comprises: the dibasic acid evaporation flaking feeding tank, the dibasic acid evaporation flaking feeding pump and the flaking machine are connected in sequence; filtering to remove active carbon, uniformly storing the solution in a feeding tank, and then pumping the solution into a flaker by a feeding pump to prepare a DBA tablet finished product.
The application provides a binary acid recovery purification system in adipic acid production waste liquid, through suitable concentration and enrichment (will get into binary acid evaporation flaking system's material concentration by current 20% to carry 50%, so on the one hand can reduce the flaking in-process energy consumption, on the other hand can reduce the moisture content of final product), impurity removal decoloration operations such as cooling centrifugation and dissolution decoloration can further improve and promote DBA finished product quality.
By combining with the adjustment of related process parameters, the preliminary application effect shows that after the recovery and purification system provided by the application is adopted, the purity of the existing finished product is further improved to 99.7 percent by about 99.3 percent, and nitric acid with the content of 0.5 percent and water with the content of 0.5 percent of the existing finished product are further reduced to less than or equal to 0.1 percent of nitric acid and less than or equal to 0.3 percent of water, so that the recovery and purification system has better technical significance for improving the quality of DBA products and the value of the DBA products.
Drawings
Fig. 1 is a schematic structural diagram of an adipic acid production liquid recycling system provided by the application.
Examples
As shown in fig. 1, the system for recovering and purifying dibasic acid in adipic acid production waste liquid provided by the present application comprises: the device comprises a climbing film evaporator 3, a separator 4, a dibasic acid recovery crystallization unit, a centrifugal separation device 7, a dissolution and decoloration tank 8, a carbon filter 11 and a dibasic acid evaporation sheeting unit which are connected in sequence through pipelines;
wherein:
the climbing film evaporator 3 is connected with a raw material tank 1 for adipic acid production waste liquid which stores dibasic acid to be purified through a pipeline; in practical design, a material tank discharging pump 2 is designed on a connecting pipeline between the evaporator 3 and the material tank 1 so as to pump adipic acid production waste liquid of dibasic acid to be purified in the material tank 1 into the evaporator 3.
The climbing film evaporator 3 uses low-pressure steam as a heat source and is used for performing preliminary evaporation treatment on adipic acid production waste liquid, and the discharging temperature is controlled to be about 85 ℃.
The separator 4 is specifically, for example, a cyclone separator, and is used for separating the gas-liquid mixture after evaporation treatment of the climbing film evaporator 3, wherein the gas phase is discharged into the atmosphere after further recovery treatment, and the liquid phase part enters a subsequent diacid recovery crystallization unit;
in practical design, the top of the cyclone separator is connected with a vacuum system (not shown in the figure, and the construction is carried out according to the common general knowledge of the prior art), so that the negative pressure state (absolute pressure is 70-80 KPa) in the cyclone separator is maintained, and the rapid evaporation of the climbing film evaporator 3 is facilitated.
The dibasic acid recovery crystallization unit comprises a plurality of dibasic acid recovery crystallizers 5 which are connected in series; the diacid recovery crystallizers 5 are used for cooling and crystallizing the liquid phase separated by the separator (so as to separate out the diacid), so that each diacid recovery crystallizer 5 is correspondingly connected with a cooling device (generally, a cooling coil provided with a chilled water inlet pipeline 5-1 and a chilled water outlet pipeline 5-3 is adopted, and the cooling and crystallizing temperature of each diacid recovery crystallizer can be regulated and controlled according to the requirement);
in the preferred design, the top of the dibasic acid recovery crystallizer 5 is provided with a recovery crystallization stirring device 6 for ensuring uniform cooling of the recovery liquid.
In the embodiment, the number of the dibasic acid recovery crystallizers is 3, so that power is saved, and the recovery liquid after cooling depends on the level difference among different dibasic acid recovery crystallizers and overflows from high to low in sequence to enter the next dibasic acid recovery crystallizer;
in practical design, each diacid recovery crystallizer can be respectively connected with the existing negative pressure system (shown in the figure, and only by referring to the conventional design in the prior art), so that the inside of the diacid recovery crystallizer is kept in a micro negative pressure state (the vacuum degree is about 140mm water column), and the stable and orderly flow of the recovery liquid is ensured;
after running for a certain time, in order to clean the dibasic acid recovery crystallizer, the dibasic acid recovery crystallizer is connected with a low-pressure steam pipeline 5-2 and a condensed water discharge pipeline 5-4, and low-pressure cleaning steam enters the dibasic acid recovery crystallizer through a coil pipe to heat and clean the dibasic acid recovery crystallizer;
in actual production, the temperature of the 3 diacid recovery crystallizers is controlled as follows from high to low in sequence: 50 ℃, 25 ℃ and 12 ℃.
The centrifugal separation device 7 specifically comprises: the centrifugal machine connected with a filter cake washing water (cold high-purity water, 0.6MPa,10 ℃) pipeline is used for centrifugally dewatering and washing the recovered liquid after the dibasic acid is crystallized, after centrifugal washing, the impurity content of the filter cake with the main body of the dibasic acid is further reduced (the washing liquid enters other working procedures for subsequent treatment), and the obtained filter cake enters a dissolution and decoloration tank 8 for further treatment.
The dissolving and decoloring tank 8 is used for further decoloring and impurity removing treatment after dissolving the filter cake separated by the centrifugal separation device 7, so that an active carbon inlet 8-1 for decoloring and impurity removing and a dissolving water inlet 8-2 for dissolving are arranged at the upper part of the tank body; to further ensure sufficient dissolution and decoloration, a dissolution and decoloration tank stirrer 9 can be designed at the top of the tank body, and/or a dissolution and decoloration tank low-pressure steam inlet 8-3 and a corresponding dissolution and decoloration tank condensate outlet 8-4 (the temperature of the dissolution liquid is properly raised, thereby accelerating dissolution) are designed on the tank body;
in the concrete production, the activated carbon can be added according to the mass ratio of 0.5% of the filter cake, and the concentration of the DBA solution after dissolution is controlled at 50%, so that the decolorization and impurity removal are facilitated.
The carbon filter 11 is used for filtering and removing active carbon in the dissolved and decolored solution; in actual production, a discharging pump 10 of the dissolution and decoloration tank is designed on a connecting pipeline between the carbon filter 11 and the dissolution and decoloration tank 8 and is used for pumping the dissolution and decoloration solution into the carbon filter;
further, the carbon filter 11 is also matched with a sight glass 12 and a carbon protection filter 13, so that the filtering condition of the carbon filter can be intuitively judged and the stable operation of the carbon filter can be ensured.
The dibasic acid evaporation and flaking unit comprises: the dibasic acid evaporation flaker feeding tank 14, the dibasic acid evaporation flaker feeding pump 15 and the flaker 16 are connected in sequence;
after the active carbon is removed by filtration, the solution is uniformly stored in a feed tank 14, and then pumped into a flaker 16 by a feed pump 15 to prepare a DBA tablet finished product.
By using the system, taking the specification of adipic acid waste liquid amount of 4t/h as an example, and combining with the adjustment of part of process parameters, actual production is carried out on the DBA yield and quality conditions obtained by preparation of different process parameters, and the results are shown in the following table 1.
TABLE 1 DBA prepared under different process parameters
As can be seen from the results of the table, the DBA products prepared under different process parameter adjustment have slightly different quality, but the purity is higher overall, the nitric acid content is obviously reduced, and the better technical effect is shown.
Generally, the diacid recovery and purification system in the adipic acid production waste liquid provided by the application can further improve and promote DBA finished product quality by properly concentrating (the concentration of materials entering a diacid evaporation flaking system is increased from the existing 20% to 50%, so that on one hand, the energy consumption in the flaking process can be reduced, and on the other hand, the moisture content of a final product can be reduced), cooling centrifugation, dissolving decoloration and other impurity removal decoloration operations, can further promote the existing purity to 99.7%, and can further reduce the nitric acid content of 0.5% and the moisture content of 0.5% of the existing finished product to be less than or equal to 0.1% of nitric acid and less than or equal to 0.3% of water, thereby having better technical significance for improving the DBA product quality and the product value.
Claims (9)
1. A system for recycling and purifying dibasic acid in adipic acid production waste liquid is characterized in that the system comprises: the device comprises a climbing film evaporator, a separator, a dibasic acid recovery crystallization unit, a centrifugal separation device, a dissolution and decoloration tank and a dibasic acid evaporation flaking unit which are sequentially connected through pipelines; wherein:
the climbing film evaporator is connected with a raw material tank for storing adipic acid production waste liquid to be purified through a pipeline;
the climbing film evaporator takes low-pressure steam as a heat source and is used for performing primary evaporation treatment on adipic acid production waste liquid;
the dibasic acid recovery crystallization unit comprises a plurality of dibasic acid recovery crystallizers which are connected in series; the dibasic acid recovery crystallizer is used for cooling and crystallizing the liquid phase separated by the separator to separate out dibasic acid; each dibasic acid recovery crystallizer is correspondingly connected with a cooling device;
the centrifugal separation device specifically comprises: the centrifugal machine is connected with a filter cake washing water pipeline and is used for carrying out centrifugal dehydration washing on the recovered liquid after the dibasic acid is crystallized;
the dissolution and decoloration tank is used for further performing decoloration and impurity removal treatment after dissolving the filter cake separated by the centrifugal separation device; an active carbon inlet for decoloring and impurity removing and a dissolution water inlet for dissolution are arranged at the upper part of the tank body;
the dibasic acid evaporation and flaking unit comprises: the device comprises a dibasic acid evaporation flaking feeding tank, a dibasic acid evaporation flaking feeding pump and a flaking machine which are connected in sequence.
2. The system for recovering and purifying dibasic acid in adipic acid production waste liquid as claimed in claim 1, wherein a discharge pump of the raw material tank is arranged on a connecting pipeline between the evaporator and the raw material tank so as to pump adipic acid production waste liquid in the raw material tank into the evaporator.
3. The system for recovering and purifying dibasic acid in waste liquid from adipic acid production of claim 1, wherein the separator is a cyclone separator; the top of the cyclone separator is connected with a vacuum system to maintain the negative pressure state in the cyclone separator.
4. The system for recovering and purifying dibasic acid in waste liquid from adipic acid production as claimed in claim 1, wherein the cooling device arranged in the dibasic acid recovering crystallizer is a cooling coil provided with a chilled water inlet pipeline and a chilled water outlet pipeline.
5. The system for recovering and purifying dibasic acid in adipic acid production waste liquid as claimed in claim 1, wherein a recovery crystallization stirring device is arranged at the top of the dibasic acid recovery crystallizer.
6. The system for recovering and purifying dibasic acid in adipic acid production waste liquid as claimed in claim 1, wherein each dibasic acid recovering crystallizer is respectively connected with a negative pressure system so as to keep the inside of the dibasic acid recovering crystallizer in a micro negative pressure state, thereby ensuring the stable and orderly flow of the recovered liquid; meanwhile, the dibasic acid recovery crystallizer is connected with a low-pressure steam pipeline and a condensed water discharge pipeline so as to heat and clean the dibasic acid recovery crystallizer.
7. The system for recovering and purifying dibasic acid in adipic acid production waste liquid according to claim 1, wherein the dissolution and decoloration tank is provided with a dissolution and decoloration tank stirrer at the top of the tank body, and/or the tank body is provided with a dissolution and decoloration tank low-pressure steam inlet and a corresponding dissolution and decoloration tank condensate outlet.
8. The system for recovering and purifying dibasic acid in adipic acid production waste liquid as claimed in claim 1, wherein a discharge pump of the dissolution and decoloration tank is arranged on a connecting pipeline of the carbon filter and the dissolution and decoloration tank and is used for pumping the dissolution and decoloration solution into the carbon filter.
9. The system for recovering and purifying dibasic acid in adipic acid production waste liquid as claimed in claim 1, wherein the carbon filter is provided with a sight glass and a carbon protection filter, so as to visually judge the filtering condition of the carbon filter and ensure the stable operation of the carbon filter.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202223057438.2U CN219272164U (en) | 2022-11-17 | 2022-11-17 | System for recycling and purifying dibasic acid in adipic acid production waste liquid |
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| CN202223057438.2U CN219272164U (en) | 2022-11-17 | 2022-11-17 | System for recycling and purifying dibasic acid in adipic acid production waste liquid |
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| CN202223057438.2U Active CN219272164U (en) | 2022-11-17 | 2022-11-17 | System for recycling and purifying dibasic acid in adipic acid production waste liquid |
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