Dioctyl phthalate separation and purification device
The dioctyl phthalate separation and purification device, which uses a dual-phase separator and an anchor-type stirring paddle scraper system, solves the problems of incomplete separation and slow cleaning, achieving efficient phase separation and heat recovery, and improving product quality and energy utilization.
Patent Information
- Application Number
- CN202520165392.0
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2025-01-23
- Publication Date
- 2026-02-27
- Estimated Expiration
- 2035-01-23
AI Technical Summary
In existing dioctyl phthalate production facilities, incomplete separation leads to low product yield and purity, slow cleaning easily causes cross-contamination, and insufficient heat recovery and utilization, increasing production costs.
The dioctyl phthalate separation and purification device, which adopts a dual-phase separator structure, combined with an anchor-type agitator and scraper cleaning system, and heat recovery from the condenser and heat exchanger, achieves more thorough phase separation and rapid cleaning, reducing energy waste.
It improved product yield and purity, reduced cross-contamination, lowered production costs, and increased energy utilization.
Smart Images
Figure CN223945007U_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The utility model relates to the technical field of dioctyl phthalate production, specifically to dioctyl phthalate separation and purification device. BACKGROUND
[0002] As an important plasticizer, dioctyl phthalate (DOP) is widely used in the processing of polyvinyl chloride (PVC) products, such as plastic film, artificial leather, and cable sheath. The separation and purification of dioctyl phthalate is crucial for ensuring product quality and performance.
[0003] In the production of a workshop, the existing devices mostly use a single phase separator for phase separation operation of the material in the separation stage of dioctyl phthalate. However, due to the complex composition of the mixture produced in the production process of dioctyl phthalate, the single phase separator cannot achieve sufficient separation of each phase, resulting in some product residues in other phases, incomplete separation, reduced product yield, and affected product purity. In addition, when producing different batches, the cleaning of the reaction kettle is a prominent problem. Traditional cleaning methods often cannot quickly and cleanly remove the reaction residues and impurities on the inner wall of the reaction kettle. This not only increases the cleaning time and cost, but also may cause cross-contamination between different batches of products, affecting product quality stability. In the existing separation and purification device, the heat recovery and utilization are not sufficient. For example, the heat generated in some links is not effectively recovered and directly discharged into the environment, causing energy waste and increasing production costs. SUMMARY
[0004] In view of the above deficiencies in the prior art, the purpose of the present utility model is to provide a dioctyl phthalate separation and purification device, wherein the reaction kettle is connected to the main phase separator through the condenser, and the main phase separator is connected to the auxiliary phase separator, forming a double phase separator structure that can more fully separate the phases, improve the separation effect, reduce product residues, and improve product yield and purity. The reaction kettle is internally provided with an anchor-type stirring paddle driven by a stirring motor, and a scraper is provided on the upper side, which is connected to a hydraulic cylinder to quickly and effectively scrape and clean the inner wall of the reaction kettle after production, in combination with the spray disc and the spray water inlet pipeline, to quickly and cleanly clean the reaction kettle and reduce cross-contamination between different batches of production. The condenser coil inside the condenser is connected to the heat exchanger through the connecting pipeline, achieving effective recovery and utilization of heat, improving energy utilization rate, and reducing production cost.
[0005] The utility model is implemented by using the following technical solutions:
[0006] The dioctyl phthalate separation and purification device, comprising a reaction kettle, the reaction kettle is connected with a water washing tank through a neutralization tank, the water washing tank is connected with a filter through a decoloring kettle, the filter is connected with a rectifying tower through a heat exchanger, the reaction kettle is connected with a main phase separator through a condenser, and the main phase separator is connected with an auxiliary phase separator.
[0007] The reaction kettle is the core reaction place for dioctyl phthalate production, and raw materials such as phthalic anhydride and 2-ethylhexanol are reacted to generate dioctyl phthalate under the action of a catalyst. The anchor stirring paddle inside is driven by a stirring motor, which can fully mix the raw materials, improve the reaction rate and uniformity, and ensure that the reaction is fully carried out. In view of the problem that cleaning is not fast and clean during different batches of production, the scraper moves closely to the inner wall of the reaction kettle under the drive of the hydraulic cylinder, and the adhered reactants and impurities are scraped off. Combined with the spray disc and the spray water inlet pipeline, the reaction kettle can be quickly and thoroughly cleaned, effectively reducing cross contamination between different batches and ensuring product quality stability.
[0008] The inside of the reaction kettle is provided with an anchor stirring paddle driven by a stirring motor, the upper part of the anchor stirring paddle is provided with a scraper, the scraper is connected with a hydraulic cylinder, and the lower part of the reaction kettle is provided with an obtuse angle discharge device.
[0009] The inside of the reaction kettle is provided with a spray disc, the spray disc is connected with a spray water inlet pipeline, and the outside of the reaction kettle is provided with a temperature control sleeve.
[0010] The inside of the condenser is provided with a condenser coil, and the condenser coil is connected with the heat exchanger through a connecting pipeline.
[0011] The condenser coil inside the condenser can condense the gaseous substances generated in the reaction kettle, so that they are converted into liquid, which is convenient for subsequent phase separation operation. At the same time, the condenser coil is connected with the heat exchanger through the connecting pipeline, which can transfer the heat released in the condensation process to the materials in the heat exchanger, realize the recycling of heat, improve the energy utilization rate, and reduce the energy waste in the production process.
[0012] The main phase separator is connected with the reaction kettle through a return pipeline, the main phase separator and the auxiliary phase separator are provided with an auxiliary phase separator pipeline, and the auxiliary phase separator is connected with the return pipeline through an auxiliary phase separator outlet pipeline.
[0013] The main phase separator receives liquid materials from the condenser and performs preliminary phase separation. Since the mixture produced in the production process of dioctyl phthalate has complex components, a single phase separator cannot achieve sufficient separation, so the main phase separator first separates the mixture into different phases, and part of the materials returns to the reaction kettle through the return pipeline, which can continue to participate in the reaction or be treated in a cycle.
[0014] The auxiliary phase separator is connected with the main phase separator, and the material separated by the main phase separator is further separated by the auxiliary phase separator, so as to make up the defect that the single phase separator cannot separate completely.
[0015] The filter is internally provided with a filter plate, the filter is provided with a washing water inlet, the connection between the decoloring kettle and the filter is located below the filter plate, and the connection between the heat exchanger and the filter is located above the filter plate.
[0016] The filter is internally provided with a filter plate, which is used for filtering the material after decoloring, and intercepting solid impurities and unreacted substances. The filter is provided with a washing water inlet, which can wash the filter plate, ensure the filtering effect and prevent blockage.
[0017] The working principle of the utility model is as follows:
[0018] In the reaction kettle, with phthalic anhydride and 2-ethylhexanol as the main raw materials, esterification reaction was carried out under the action of acid catalyst (such as sulfuric acid, catalyst dosage was 0.5%-1.5% of the total mass of raw materials). The reaction temperature was controlled at 180-230℃, the reaction pressure was maintained at 0.1-0.3MPa, and the reaction time was 3-5 hours. The stirring paddle in the reaction kettle was driven by a stirring motor, and the stirring speed was controlled at 80-120r / min to ensure that the raw materials were fully mixed and reacted. After the reaction was completed, the inner wall of the reaction kettle was scraped and cleaned by driving the scraper, and the spray disc was opened at the same time, the spray water pressure was 0.2-0.4MPa, and the reaction kettle was cleaned. The reacted material was condensed by a condenser, the cooling medium temperature in the condenser coil was controlled at 20-30℃, so that the gaseous material was changed into liquid and entered the main phase separator. The main phase separator was preliminarily separated, the separation temperature was controlled at 60-80℃, and the separation time was 15-30 minutes. Part of the separated material (about 10%-20%) returned to the reaction kettle through the return pipeline, and the other part entered the auxiliary phase separator through the auxiliary phase separator pipeline for further separation. The separation temperature of the auxiliary phase separator was 50-70℃, the separation time was 20-40 minutes, and the separated material was returned to the return pipeline through the auxiliary phase separator pipeline. The separated material in the main phase separator entered the neutralization tank, and an appropriate amount of alkaline neutralizing agent (such as sodium hydroxide solution, concentration was 10%-20%) was added into the neutralization tank, the neutralization reaction temperature was controlled at 40-60℃, and the reaction time was 10-20 minutes, so that the pH value of the material was adjusted to 6-8. The neutralized material entered the water washing tank for water washing operation. The water washing temperature was 40-50℃, the water washing time was 15-30 minutes, and the water washing times was 2-3 times to remove the residual alkaline substances, salts and other water-soluble impurities in the material. The water-washed material entered the decolorization kettle, and an appropriate amount of decolorizing agent (such as activated carbon, dosage was 0.5%-1.5% of the mass of the material) was added, the decolorization temperature was controlled at 80-100℃, and the decolorization time was 30-60 minutes to decolorize the material. The decolorized material entered the filter, the pore size of the filter plate was 0.1-0.5μm, and the filtration operation was carried out under the pressure of 0.1-0.3MPa to intercept solid impurities and unreacted substances. The flushing water inlet on the filter was periodically flushed at a pressure of 0.2-0.4MPa to ensure the filtering effect. The filtered material entered the heat exchanger, and the heat transferred by the condenser coil was used to preheat the material, and then the material was continuously heated to a temperature of 120-150℃ to provide a suitable feed temperature for the subsequent rectification tower. The preheated material entered the rectification tower, the top temperature of the rectification tower was controlled at 180-200℃, the bottom temperature was controlled at 250-280℃, and the operating pressure was 0.05-0.1MPa. Through rectification operation, dioctyl phthalate was separated from the material according to the boiling point difference between dioctyl phthalate and other impurities, and finally high-purity dioctyl phthalate product with purity ≥99.5% was obtained.
[0019] Compared with the prior art, the utility model has the advantages of:
[0020] Adopt the utility model phthalic acid dioctyl ester separation and purification device, the reation kettle is connected with the main phase separator through the condenser, is connected with the auxiliary phase separator on the main phase separator, forms the double phase separator structure, can more fully carry out the phase separation, improves the separation effect, reduces the product residue, promotes the product yield and the purity;The anchor type stirring paddle driven by the stirring motor is equipped in the reation kettle, the scraper is equipped on the top, the scraper is connected with the hydraulic cylinder, can scrape and clean the reation kettle inner wall rapidly and effectively after production ends, cooperates the spray tray and the spray water inlet pipeline, can clean the reation kettle fast and cleanly, reduces the cross contamination between different batches production;The condenser coil in the condenser is connected with the heat exchanger through the connecting pipeline, realizes the effective recovery and utilization of heat, improves the energy utilization rate, reduces the production cost. BRIEF DESCRIPTION OF DRAWINGS
[0021] Figure 1 It is the structure schematic view of the utility model phthalic acid dioctyl ester separation and purification device;
[0022] In the drawing: 1, reation kettle;2, condenser;3, main phase separator;4, neutralization tank;5, water washing tank;6, decoloring kettle;7, filter;8, heat exchanger;9, rectifying column;10, scraper;11, spray tray;12, anchor type stirring paddle;13, hydraulic cylinder;14, spray water inlet pipeline;15, stirring motor;16, obtuse angle discharger;17, condenser coil;18, auxiliary phase separator;19, return pipeline;20, into auxiliary phase separator pipeline;21, out auxiliary phase separator pipeline;22, filter plate;23, flush water inlet;24, connecting pipeline. DETAILED DESCRIPTION
[0023] In order to make the utility model purpose, technical scheme more clearly, under the following, to the utility model with further detailed description.
[0024] Example 1
[0025] As Figure 1As shown, the dioctyl phthalate separation and purification device comprises a reaction kettle 1, the reaction kettle 1 is connected with a water washing tank 5 through a neutralization tank 4, the water washing tank 5 is connected with a filter 7 through a decoloring kettle 6, the filter 7 is connected with a rectifying tower 9 through a heat exchanger 8, the reaction kettle 1 is connected with a main phase separator 3 through a condenser 2, and the main phase separator 3 is connected with an auxiliary phase separator 18. The inside of the reaction kettle 1 is provided with an anchor stirring paddle 12 driven by a stirring motor 15, the upper portion of the anchor stirring paddle 12 is provided with a scraper 10, and the scraper 10 is connected with a hydraulic cylinder 13. The inside of the reaction kettle 1 is provided with a spraying disc 11, the spraying disc 11 is connected with a spraying water inlet pipeline 14, the outside of the reaction kettle 1 is provided with a temperature control sleeve, the lower portion of the reaction kettle 1 is provided with an obtuse angle discharger 16, the inside of the condenser 2 is provided with a condenser coil pipe 17, the condenser coil pipe 17 is connected with the heat exchanger 8 through a connecting pipeline 24. The main phase separator 3 is connected with the reaction kettle 1 through a return pipeline 19, a pipeline for entering the auxiliary phase separator 20 is arranged between the main phase separator 3 and the auxiliary phase separator 18, and the auxiliary phase separator 18 is connected with the return pipeline 19 through a pipeline for discharging the auxiliary phase separator 21. The main phase separator 3 receives liquid material from the condenser and performs preliminary phase separation. Since the mixture produced in the production process of the dioctyl phthalate is complex in composition, a single phase separator is difficult to realize sufficient separation, the main phase separator 3 preliminarily separates the mixture into different phases, and part of the material returns to the reaction kettle 1 through the return pipeline 19 to continue to participate in the reaction. The inside of the filter 7 is provided with a filter plate 22, the filter 7 is provided with a flushing water inlet 23, the connection between the decoloring kettle 6 and the filter 7 is located below the filter plate 22, and the connection between the heat exchanger 8 and the filter 7 is located above the filter plate 22.
[0026] The dioctyl phthalate separation and purification device has the following steps during work:
[0027] (1) The material is reacted in the reaction kettle 1, the reacted material is condensed by the condenser 2 and then enters the main phase separator 3, part of the material separated by the main phase separator 3 returns to the reaction kettle 1 through the return pipeline 19, another part of the material separated by the main phase separator 3 enters the auxiliary phase separator 18 through the pipeline for entering the auxiliary phase separator 20 for further separation, and the material separated by the auxiliary phase separator 18 returns to the return pipeline 19 through the pipeline for discharging the auxiliary phase separator 21; (2) The material separated by the main phase separator 3 enters the neutralization tank 4, the water washing tank 5, the decoloring kettle 6, the filter 7, the heat exchanger 8 and the rectifying tower 9 in sequence, and the material is subjected to neutralization in the neutralization tank 4, water washing in the water washing tank 5, decoloring in the decoloring kettle 6, filtering in the filter 7, heat exchange in the heat exchanger 8 and rectification in the rectifying tower 9, and finally high-purity dioctyl phthalate product is obtained.
Claims
1. A dioctyl phthalate separation and purification apparatus, characterized by, Including the reaction kettle (1), the reaction kettle (1) is connected with water washing tank (5) through neutralization tank (4), water washing tank (5) is connected with filter (7) through decoloring kettle (6), filter (7) is connected with rectifying column (9) through heat exchanger (8), reaction kettle (1) is connected with main phase separator (3) through condenser (2), main phase separator (3) is connected with auxiliary phase separator (18).
2. The dioctyl phthalate separation and purification apparatus according to claim 1, characterized by The inside of the reaction kettle (1) is provided with an anchor stirring paddle (12) driven by a stirring motor (15), the upper part of the anchor stirring paddle (12) is provided with a scraper (10), the scraper (10) is connected with a hydraulic cylinder (13), the lower part of the reaction kettle (1) is provided with an obtuse angle discharger (16).
3. The dioctyl phthalate separation and purification apparatus according to claim 2, characterized by The inside of the reaction kettle (1) is provided with a spraying disc (11), the spraying disc (11) is connected with a spraying water inlet pipeline (14), the outside of the reaction kettle (1) is provided with a temperature control sleeve.
4. The dioctyl phthalate separation and purification apparatus according to claim 1, characterized by The inside of the condenser (2) is provided with a condenser coil (17), the condenser coil (17) is connected with the heat exchanger (8) through a connecting pipeline (24).
5. The dioctyl phthalate separation and purification apparatus according to claim 1, characterized by The main phase separator (3) is connected with the reaction kettle (1) through a return pipeline (19), the main phase separator (3) and the auxiliary phase separator (18) are provided with an auxiliary phase separator inlet pipeline (20), the auxiliary phase separator (18) is connected with the return pipeline (19) through an auxiliary phase separator outlet pipeline (21).
6. The dioctyl phthalate separation and purification apparatus according to claim 1, characterized by The inside of the filter (7) is provided with a filter plate (22), the filter (7) is provided with a flushing water inlet (23), the connection between the decoloring kettle (6) and the filter (7) is located below the filter plate (22), the connection between the heat exchanger (8) and the filter (7) is located above the filter plate (22).