A method and system for separating and purifying a cyclization oxidation reaction mixture
Patent Information
- Application Number
- CN202311429900.3
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-10-31
- Publication Date
- 2026-11-03
- Estimated Expiration
- 2043-10-31
AI Technical Summary
Existing epichlorohydrin separation methods suffer from problems such as uneven two-phase mixing, poor mass transfer, difficult separation, high water consumption, and high energy consumption.
It adopts a three-stage static mixing process and a multi-stage circulation method, and uses a static mixer with coaxial internal and external mixing components and tangential flow channel design to ensure uniform mixing of the mixed liquid and circulating liquid, enhance mass transfer, and reduce water consumption through multi-stage separation and self-circulation design.
It significantly improves separation efficiency, with methanol recovery rate ≥99.9%, epoxide content in aqueous phase ≤0.01%, and methanol content in organic phase ≤0.01%, achieving efficient and energy-saving separation without generating wastewater or waste residue.
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Figure CN119909411B_ABST
Abstract
Description
Technical Field
[0001] This invention relates to the separation and purification of organic mixtures, specifically to a method and system for the separation and purification of cyclization oxidation reaction mixtures, belonging to the field of chemical separation technology. Background Technology
[0002] Epichlorohydrin, also known as epichlorohydrin, possesses a unique structure (containing epoxy groups and chlorine) that allows it to be used in the synthesis of epoxy resins, glycerol, and chlorohydrin rubber. It can also be used as a solvent for cellulose esters, resins, and cellulose ethers, and as a key raw material in the production of surfactants, plasticizers, stabilizers, ion exchange resins, chemical stabilizers, water treatment agents, and adhesives. Epichlorohydrin has a wide range of applications and is an important chemical raw material and intermediate. Industrial production methods for this type of compound typically include the propylene high-temperature chlorination process, the propylene acetate process, the glycerol process, the direct cyclization oxidation of epichlorohydrin, the acrolein process, and the acetone process. Among these, the direct cyclization oxidation of epichlorohydrin offers a significant advantage in raw material costs and is a relatively mature process. It directly uses hydrogen peroxide to cyclize and oxidize allyl chloride, shortening the process flow and reducing emissions of waste gas, wastewater, and solid waste. Furthermore, the reaction conditions are mild and the yield is high, making it a relatively ideal green production process that requires further exploration.
[0003] Fiber membrane separation technology is a novel hybrid mass transfer technology composed of hydrophilic and hydrophobic fiber membranes. It features high filtration efficiency, maximum effective modulus area, easy cleaning, simple structure, convenient operation, and no secondary pollution during production. In enhanced coalescence separation, fibers can be specially woven to facilitate the capture of liquid particles; stepwise control of porosity can enhance separation efficiency; optimized combinations of oleophilic or oleophobic fibers strengthen droplet collision and capture; and the difference in surface tension between the two phases in epoxy products creates a velocity difference for separation. Since its inception, fiber membrane separation technology has developed rapidly, and many countries have widely applied it in information, energy, petroleum, chemical, heavy industry, light industry, food, beverage, pharmaceutical, medical, bioengineering, military, and environmental protection fields. However, its development in the chemical field related to the refining of epoxidized products remains unexplored and urgently needs further research.
[0004] Currently, the conventional countercurrent extraction method is used to separate epichlorohydrin. However, the pure countercurrent contact during extraction results in uneven mixing between the two phases, poor mass transfer, and low separation efficiency. The small density difference between the two phases in the extraction tower makes separation difficult. The large water consumption for washing leads to high energy consumption, making it difficult for the equipment to maintain long-term operation.
[0005] Chinese invention patent CN104003961B discloses a method for continuous extraction of epichlorohydrin. The method involves mixing an extractant containing epichlorohydrin, methanol, 3-chloropropene, and water with a first extractant (water) and removing non-condensable gases from the mixture to obtain a mixture containing the extractant and the first extractant. This mixture is then introduced from the bottom of an extraction tower and countercurrently contacted with a second extractant (3-chloropropene) flowing downwards, resulting in an extract phase rich in epichlorohydrin. This invention solves the problem of operational instability in the extraction tower caused by the presence of numerous bubbles and improves the extraction rate of epichlorohydrin in the extract phase, thus achieving continuous extraction of epichlorohydrin.
[0006] Chinese invention patent CN103772327B discloses a method for extracting epichlorohydrin. This method involves continuous extraction of an extract containing epichlorohydrin, methanol, 3-chloropropene, and water in two extraction towers. First, the extract and water are mixed and introduced into the lower end of the first extraction tower, where they are countercurrently contacted with the 3-chloropropene extractant flowing downwards. The resulting epichlorohydrin-rich extract phase is then introduced into the lower end of the second extraction tower, where it is countercurrently contacted with water flowing downwards, yielding a raffinate phase rich in epichlorohydrin and 3-chloropropene. This invention solves the problem of reduced epichlorohydrin yield due to the presence of methanol.
[0007] In summary, existing methods for separating epichlorohydrin suffer from problems such as uneven two-phase mixing, poor mass transfer, difficult separation, high water consumption, and high energy consumption. Summary of the Invention
[0008] To address the problems existing in the prior art, the first objective of this invention is to provide a method for separating and purifying a mixture of cyclization and oxidation reaction solutions. This method employs a three-stage static mixing process, which effectively solves the technical problems of uneven mixing and low mass transfer efficiency, significantly improving the subsequent separation efficiency. Furthermore, by adopting a multi-stage circulation method, the water consumption during the separation process is effectively reduced, while further improving the separation efficiency of methanol and epoxides in the mixture.
[0009] The second objective of this invention is to provide a separation and purification system for a cyclization reaction mixture. The static mixer used in this system consists of an inner mixing component and an outer mixing component arranged in opposite directions with their tangential flow channel openings, which are alternately distributed in the longitudinal height. This ensures uniform mixing of the mixture and the circulating liquid, reduces water consumption, and significantly enhances mass transfer.
[0010] To achieve the above technical objectives, the present invention provides a separation and purification system for a cyclization oxidation reaction mixture, which includes a static mixer, a coalescer, and a circulating pump; the static mixer 1 (1) is connected to the inlet of coalescer D-501 (10), the coalescer D-503 (12) and coalescer D-505 (14) are connected in series with the light phase outlet of coalescer D-501, and the coalescer D-502 (11) and coalescer D-504 (13) are connected in series with the heavy phase outlet of coalescer D-501; a static mixer is also provided between the coalescers, and the heavy phase outlets of coalescer D-502, D-503, D-504 and D-505 are connected to the static mixer at the inlet of the previous coalescer through the circulating pump.
[0011] As a preferred embodiment, the static mixer comprises a mixing chamber (101), an upper sealing flange (102), and a lower sealing flange (103).
[0012] As a preferred embodiment, the mixing cavity contains an inner mixing component (105) and an outer mixing component (104) coaxially mounted from the inside out.
[0013] As a preferred embodiment, the columnar body (107) of the external mixing component is provided with a tangential flow channel (109).
[0014] As a preferred embodiment, the columnar body (108) of the internal mixing component is provided with a tangential flow channel (110).
[0015] As a preferred embodiment, the static mixer is further provided with a sieve plate (106) at the connection between the lower sealing flange and the mixing chamber.
[0016] As a preferred embodiment, the sieve plate is provided with sieve holes evenly distributed around the circumference.
[0017] As a preferred embodiment, the tangential flow channels of the inner mixing component and the tangential flow channels of the outer mixing component are arranged in a cross pattern in the longitudinal height.
[0018] As a preferred embodiment, the tangential flow channels of the inner mixing component are arranged in opposite directions to the tangential flow channels of the outer mixing component.
[0019] The static mixers used in this invention all adopt a horizontal structure and are independently designed based on hydraulic parameters. From top to bottom, they are connected in sequence: an upper sealing flange, a mixer cavity, and a lower sealing flange. The mixer cavity contains mixing components 104 and 105 and a sieve plate. The upper sealing flange has a material inlet at its top and a water outlet at its bottom. The side wall of the mixer cavity has a water inlet, and the material inlet and outlet are connected via the sieve plate. A cavity structure is formed between the inner wall of the mixer cavity and the outer wall of the mixing components, which maintains pressure balance between the outer and inner cavities, preventing excessive local pressure from causing liquid backflow. A cavity structure is formed between mixing components 104 and 105 as a mixing zone, achieving phased flow. The materials and water collide and mix. The cavity between the mixing components 104 and 105 and the underflow outlet are connected by a sieve plate. The sieve plate can rectify the flow and increase the contact area between the mixed materials, so that the mixed materials can be further mixed. The upper and lower ends of the mixing components are sealed with the upper sealing flange and the lower sealing flange respectively through sealing structures. The cavity between the inner mixer component 104 and the outer mixer component 105 is connected to the inner cavity of the material inlet and water outlet of the mixer through the upper sealing flange, the lower sealing flange and the sieve plate. The columnar body of the inner mixer component is provided with multiple sets of tangential flow channels, and the tangential flow channels of the inner mixing component and the tangential flow channels of the outer mixing component are arranged in opposite directions, which can generate swirling flow between them and promote the mixing of the two phases.
[0020] The present invention also provides a method for separating and purifying a mixture of epoxidation reaction solution, wherein the mixture of hydrogen peroxide and allyl chloride is separated by any of the above-described systems.
[0021] As a preferred embodiment, the cyclization reaction mixture is a mixed solution comprising epichlorohydrin, methanol, 3-chloropropene, MCPD, CPD and water.
[0022] As a preferred embodiment, the separation and purification process of the epoxidation reaction mixture includes:
[0023] 1) The epoxidation mixture is mixed with the D-502 circulating liquid returned by circulation pump 1 and the D503 circulating liquid returned by circulation pump 3 in static mixer 1 and then enters coalescer D-501 for coarse separation. The coarse methanol liquid is discharged from the light phase outlet and the coarse epoxide liquid is discharged from the heavy phase outlet.
[0024] 2) The methanol coarse liquid and the circulating liquid returned by the circulating pump 4 from D-505 are thoroughly mixed in the static mixer 3 and then enter the coalescer D-503 for separation. The methanol primary fine liquid is discharged from the light phase outlet, and the separation residue is discharged from the heavy phase outlet for circulation.
[0025] 3) After the coarse epoxide liquid and the D-504 circulating liquid returned by the circulating pump 2 are fully mixed in the static mixer 2, they enter the coalescer D-502 for separation. The first-stage fine epoxide liquid is discharged from the light phase outlet, and the remaining liquid is discharged from the heavy phase outlet for circulation.
[0026] 4) The first-stage methanol liquid and 3-chloropropene are thoroughly mixed in static mixer 5 and then separated in methanol separator D-505. The second-stage methanol liquid is discharged from the light phase outlet, and the remaining liquid is discharged from the heavy phase outlet for recycling.
[0027] 5) After the epoxide primary purification liquid and water are fully mixed in static mixer 4, they enter coalescer D-504 for separation. The epoxide secondary purification liquid is discharged from the light phase outlet, and the separation residue is discharged from the heavy phase outlet for recycling.
[0028] As a preferred embodiment, the flow ratio of the epoxidation reaction mixture, the D-503 circulating liquid, and the D-502 circulating liquid in the static mixer 1 is 2 to 4:1:1.
[0029] As a preferred embodiment, the extraction flow ratio of the C4-C16 liquid halogenated hydrocarbons to the epoxides in the methanol primary purification liquid in the static mixer 5 is 5-10:1.
[0030] As a preferred embodiment, the C4-C16 liquid halogenated hydrocarbon is at least one selected from 3-chloropropene, 1,2-dibromopropane, 1,6-dibromohexane, bromobenzene, m-dibromobenzene, and 1,4-dichlorobutane, and the purity of the C4-C16 liquid halogenated hydrocarbon is ≥99.3%. More preferably, the C4-C16 liquid halogenated hydrocarbon is 3-chloropropene.
[0031] As a preferred embodiment, the flow ratio of the methanol primary fraction to 3-chloropropene in the static mixer 5 is 1.5 to 3:1, the flow rate is 0.5 to 1.5 m / s, and the pressure drop is 0.05 to 0.4 MPa.
[0032] As a preferred embodiment, the purity of the 3-chloropropene is ≥99.3%.
[0033] As a preferred embodiment, the flow ratio of the epoxide primary purification liquid to water in the static mixer 4 is 1.5 to 2:1, the pressure drop is 0.05 to 0.4 MPa, and the flow velocity is 0.5 to 1.5 m / s.
[0034] As a preferred embodiment, the extraction flow ratio of methanol to water in the primary epoxide fraction in the static mixer 4 is 1 to 3:100.
[0035] As a preferred embodiment, the total epoxide content in the methanol secondary purification solution is ≤0.01%; and the methanol content in the epoxide secondary purification solution is ≤0.01%.
[0036] Compared with the prior art, the beneficial technical effects of the present invention are as follows:
[0037] 1) The separation and purification method provided by the present invention adopts a three-stage static mixing process, which effectively solves the technical problems of uneven mixing and low mass transfer efficiency, and greatly improves the subsequent separation efficiency. Furthermore, the multi-stage circulation method effectively reduces the water consumption in the separation process and further improves the separation efficiency of methanol and epoxide in the mixture.
[0038] 2) The separation and purification system proposed in this invention utilizes a multi-stage circulation and multi-stage separation method to fully ensure the separation of methanol and epoxide. The static mixer used consists of an inner mixing component and an outer mixing component arranged in opposite directions with their tangential flow channel openings, which are alternately distributed in the longitudinal height. This ensures that the mixed liquid and the circulating liquid are mixed evenly, reducing water consumption while significantly enhancing mass transfer.
[0039] 3) The technical solution provided by this invention adopts a self-circulation design, which reduces the injection of fresh water and eliminates the discharge of wastewater and waste residue. The overall process is simple and easy to implement, and the effect is excellent. According to the test, after separating the epoxide mixture using the technical solution provided by this invention, the methanol recovery rate is ≥99.9%, the epoxide content in the aqueous phase is ≤0.01%, and the methanol content in the organic phase is ≤0.01%. Attached Figure Description
[0040] The objects and features of the present invention will become more apparent from the following detailed description with reference to the accompanying drawings. The drawings are provided to offer a further understanding of the invention, and constitute only a part of this specification to further explain the invention, but do not constitute a limitation thereof:
[0041] Figure 1 This is a process flow diagram of the method for refining epoxidized products according to the present invention.
[0042] Among them, 1-static mixer 1, 2-static mixer 2, 3-static mixer 3, 4-static mixer 4, 5-static mixer 5, 6-circulation pump 1, 7-circulation pump 2, 8-circulation pump 3, 9-circulation pump 4, 10-coalescing unit D-501, 11-coalescing unit D-502, 12-coalescing unit D-503, 13-water washing coalescing unit D-504, 14-methanol separator D-505;
[0043] Figure 2 This is a schematic diagram of the static mixer structure independently designed by the present invention.
[0044] Figure 3 This is a front view of the mixing component of the static mixer described in this invention;
[0045] Figure 4 This is a perspective view of the mixing component of the static mixer described in this invention;
[0046] Figure 5 This is a front view of the mixing component of the static mixer described in this invention;
[0047] Figure 6 for Figure 5 AA section view and CC section view in the text;
[0048] Figure 7 for Figure 5 BB section view and DD section view in the middle;
[0049] Figure 8 This is an assembly diagram of the mixing components of the static mixer described in this invention;
[0050] Figures 2-8 In the middle, 101-columnar body, 102-upper sealing flange, 103-lower sealing flange, 104-outer mixing component, 105-inner mixing component, 106-sieve plate, 107-columnar body of the outer mixing component, 108-columnar body of the inner mixing component, 109-tangential flow channel of the outer mixing component, 110-tangential flow channel of the inner mixing component, 111-mixer material inlet, 112-mixer water inlet, 113-mixer water outlet. Detailed Implementation
[0051] The present invention will be further described below with reference to the accompanying drawings and embodiments:
[0052] Through long-term engineering practice and experimental research, the applicant of this invention has identified problems with existing methods, such as difficulty in phase separation and high energy consumption in distillation separation. These methods not only fail to meet environmental protection requirements but also cannot meet the production needs of high-purity methanol recovery. Based on the concept of "high efficiency, separation, and recovery," the applicant proposes a simple method and apparatus for separating refined epoxidized products in the epichlorohydrin oxidation process. The method and apparatus of this invention are highly efficient and energy-saving. During implementation, no excess wastewater, waste residue, or other pollutants are generated, and wastewater is recycled as much as possible. Furthermore, mixed solvents in the wastewater can be recovered, fully realizing the resource management of wastewater.
[0053] The embodiments provided in this invention are all implemented based on the following system, specifically:
[0054] like Figure 1 As shown, during operation, the water washing and extraction devices are arranged in parallel. First, the epoxidation product is piped into static mixer 1 and mixed with circulating water from coalescers D-502 and D-503 before entering coalescer D-501. After coalescence separation, the heavy phase from D-501 is fed into static mixer 2, and the light phase from D-501 is fed into static mixer 3. The light phase from D-501 mixes with circulating water from D-505 returned by circulating pump 4 and enters D-503, while the heavy phase from D-501 mixes with circulating water from D-504 returned by circulating pump 2 and enters D-502. The light phase of the mixed solution separated by D-503 then enters the static mixer. In mixer 5, the heavy phase is returned to static mixer 1 via circulation pump 3. The light phase of the mixed solution separated by D-502 enters static mixer 4, and the heavy phase is returned to static mixer 1 via circulation pump 1. Simultaneously, fresh water is introduced into static mixer 4 and mixed with the outlet solution of the light phase from coalescer D-502 before being introduced into coalescer D-504. The mixed solvent from the heavy phase outlet of coalescer D-504 is sent back to static mixer 2 via circulation pump 2, forming a self-circulating water washing process. The light phase from coalescer D5-503 is introduced into static mixer 5 and mixed with a certain concentration of 99.3% 3-chloropropene before being introduced into methanol separator D-505 to recover methanol. The epoxidation product is separated by a three-stage coalescer to obtain the extracted epoxidation product and the remaining 3-chloropropene mixed solution.
[0055] Furthermore, there is a static mixer 1, a coalescer D-501 connected to the static mixer, static mixers 2 and 3 connected to the coalescer D-501, static mixers 2 and 4 connected to the coalescer D-502, static mixers 3 and 5 connected to the coalescer D-503, coalescer D-504 connected to the static mixer 4, and coalescer D-505 connected to the static mixer 5.
[0056] The three-stage extraction process described in this invention employs a horizontal structure with a specially woven fiber membrane inside. This facilitates the capture of liquid particles, allows for stepwise active control of porosity to enhance separation, and utilizes an optimized combination of oleophilic or oleophobic fibers to strengthen droplet collision and capture. The entire device receives fresh water only from the static mixer 4, and the heavy phase of coalescer D-504 is connected to the static mixer 2, while the heavy phase of coalescer D-502 is connected to the static mixer 1, enabling wastewater recycling. This not only saves on utility costs but also reduces equipment investment and floor space requirements.
[0057] The present invention is further illustrated below with reference to specific embodiments. However, it should be understood that these embodiments are for illustrative purposes only and do not constitute a limitation on the scope of the invention. Test methods in the following embodiments, unless otherwise specified, are generally performed under conventional conditions or as recommended by the manufacturer. Unless otherwise stated, all percentages and parts are by weight.
[0058] Example 1
[0059] A petrochemical company in Baling conducted pilot-scale experiments using the method and apparatus of this invention, and applied the treatment to the reaction unit of the pilot-scale apparatus according to... Figure 2 The process flow diagram shown is a comprehensive application of the separation method for refining epoxidized products in the epichlorohydrin oxidation process. After the treatment, pure methanol is obtained. The process produces no wastewater or waste residue, and at the same time, it realizes resource utilization and generates significant economic benefits.
[0060] The specific operation process and effects are as follows:
[0061] 1) Conditions
[0062] The composition of the material to be extracted (one batch) is as follows: 55.25 kg of continuous material to be extracted is provided, of which methanol accounts for 58.98%, 3-chloropropene accounts for 13.15%, epichlorohydrin accounts for 10.18%, MCPD accounts for 2.06%, CPD accounts for 0.60%, and water accounts for 15.03%.
[0063] Operating conditions: Process water consumption is 5 kg / h, circulation rate is 5 kg / h, and 3-chloropropene is 6.8 kg / h.
[0064] Operating parameters: Considering that each batch of extractable solution is processed every 5 hours, the total feed flow rate of the extractable solution is approximately 12.5 L / h, the feed rate of demineralized water to coalescer D-504 is approximately 2-6 L / h, the water washing water circulation rate is approximately 2-8 L / h, the feed rate of 3-chloropropene to coalescer D-505 is approximately 2-8 L / h, the circulating water circulation rate is approximately 2-8 L / h, the concentration of 3-chloropropene is approximately 99.3%, the temperature is approximately 30-40℃, and the pressure is approximately atmospheric pressure.
[0065] 2) Content determination of results
[0066] For mixed solvents, methanol content was determined by gas chromatography-tandem mass spectrometry or high performance liquid chromatography; water content was determined by Karl Fischer potentiometric titration; and 3-chloropropene content was determined by gas chromatography-tandem mass spectrometry.
[0067] 3) Application effect
[0068] After treatment using this water washing separation method and device, the final organic phase outlet has an epichlorohydrin and 3-chloropropene content of 25.1% and a methanol content of less than 0.01%, while the aqueous phase outlet has a methanol content of 56-57% and an epichlorohydrin content of less than 0.01%.
[0069] Example 2:
[0070] 1) This embodiment provides a method and apparatus for separating refined epoxidized products in an environmentally friendly epichlorohydrin oxidation process. The process flow is the same as above, except that the test conditions are changed to process water consumption of 6 kg / h, circulation volume of 6 kg / h, and 3-chloropropene of 7 kg / h.
[0071] 2) Content determination results: The methanol content of the mixed solvent was determined by gas chromatography-tandem mass spectrometry or high performance liquid chromatography, the water content was determined by Karl Fischer potentiometric titration, and the 3-chloropropene content was determined by gas chromatography-tandem mass spectrometry.
[0072] 3) Application effect
[0073] After treatment using this water washing separation method and device, the final organic phase outlet has an epichlorohydrin and 3-chloropropene content of 23.1%, the average methanol content in the purified oil phase is less than 0.01%, while the methanol content in the aqueous phase outlet is 54-55%, and the epichlorohydrin content is less than 0.01%.
[0074] Comparative Example 1
[0075] 1) The apparatus and process flow used in this comparative example are the same as above, except that the water consumption is 4 kg / h, the circulation rate is 4 kg / h, and the 3-chloropropene is 6.8 kg / h.
[0076] 2) Content determination results: The methanol content of the mixed solvent was determined by gas chromatography-tandem mass spectrometry or high performance liquid chromatography, the water content was determined by Karl Fischer potentiometric titration, and the 3-chloropropene content was determined by gas chromatography-tandem mass spectrometry.
[0077] 3) Application effect
[0078] After treatment using this water washing separation method and apparatus, no large amount of epichlorohydrin and 3-chloropropene were detected at the organic phase outlet, and the epichlorohydrin content in the aqueous phase outlet of the separation system was 2%.
[0079] In summary, by comparing the conditions of the three sets of operating conditions, the method and apparatus for separating refined epoxidized products in the environmentally friendly epichlorohydrin oxidation process provided by this invention, when the process water consumption is 5 kg / h, the circulating water consumption is 5 kg / h, and the 3-chloropropene consumption is 6.8 kg / h, can ensure that all indicators of the organic phase and aqueous phase output from the coalescer D-504 in the existing process meet the process requirements, while also reducing water consumption.
[0080] All documents mentioned in this invention are incorporated herein by reference as if each document were individually incorporated by reference. Furthermore, it should be understood that after reading the foregoing teachings of this invention, those skilled in the art can make various alterations or modifications to this invention, and these equivalent forms also fall within the scope defined by the appended claims.
Claims
1. A separation and purification system for a cyclization oxidation reaction mixture, characterized in that: It includes a static mixer, a coalescer, and a circulating pump; the static mixer 1 (1) is connected to the inlet of coalescer D-501 (10), the coalescer D-503 (12) and coalescer D-505 (14) are connected in series with the light phase outlet of coalescer D-501, and the coalescer D-502 (11) and coalescer D-504 (13) are connected in series with the heavy phase outlet of coalescer D-501; a static mixer is also provided between the coalescers, and the heavy phase outlets of coalescer D-502, D-503, D-504 and D-505 are connected to the static mixer at the inlet of the previous coalescer through a circulating pump; The static mixer comprises a mixing chamber (101), an upper sealing flange (102), and a lower sealing flange (103); the mixing chamber contains an inner mixing component (105) and an outer mixing component (104) coaxially mounted from the inside out; the outer mixing component has a tangential flow channel (109) on its columnar body (107); the inner mixing component has a tangential flow channel (110) on its columnar body (108). The tangential flow channels of the inner mixing component and the outer mixing component are arranged intersectingly in the longitudinal height; the tangential flow channels of the inner mixing component and the outer mixing component are arranged in opposite directions.
2. The separation and purification system for a cyclization oxidation reaction mixture according to claim 1, characterized in that: The static mixer is also provided with a sieve plate (106) at the connection between the lower sealing flange and the mixing chamber; the sieve plate is provided with sieve holes evenly distributed around the circumference.
3. A method for separating and purifying a cyclization oxidation reaction mixture, characterized in that: The system described in claim 1 or 2 is used to separate the epoxidation reaction mixture of hydrogen peroxide and chloropropene; the epoxidation reaction mixture is a mixed solution containing epichlorohydrin, methanol, 3-chloropropene, MCPD, CPD and water.
4. The method for separating and purifying a cyclization oxidation reaction mixture according to claim 3, characterized in that: The separation and purification process of the epoxidation reaction mixture includes: 1) The epoxidation mixture is mixed with the D-502 circulating liquid returned by circulation pump 1 and the D503 circulating liquid returned by circulation pump 3 in static mixer 1 and then enters coalescer D-501 for coarse separation. The coarse methanol liquid is discharged from the light phase outlet and the coarse epoxide liquid is discharged from the heavy phase outlet. 2) The methanol coarse liquid and the circulating liquid returned by the circulating pump 4 from D-505 are thoroughly mixed in the static mixer 3 and then enter the coalescer D-503 for separation. The methanol primary fine liquid is discharged from the light phase outlet, and the separation residue is discharged from the heavy phase outlet for circulation. 3) After the coarse epoxide liquid and the D-504 circulating liquid returned by the circulating pump 2 are fully mixed in the static mixer 2, they enter the coalescer D-502 for separation. The first-stage fine epoxide liquid is discharged from the light phase outlet, and the remaining liquid is discharged from the heavy phase outlet for circulation. 4) The primary methanol fraction and C4~C16 liquid halogenated hydrocarbons are thoroughly mixed in static mixer 5 and then separated in methanol separator D-505. The secondary methanol fraction is discharged from the light phase outlet, and the remaining liquid is discharged from the heavy phase outlet for recycling. 5) After the epoxide primary purification liquid and water are fully mixed in static mixer 4, they enter coalescer D-504 for separation. The epoxide secondary purification liquid is discharged from the light phase outlet, and the remaining liquid is discharged from the heavy phase outlet for recycling.
5. The method for separating and purifying a cyclization oxidation reaction mixture according to claim 4, characterized in that: The flow rate ratio of the epoxidation reaction mixture, D-503 circulating liquid, and D-502 circulating liquid in the static mixer 1 is 2~4:1:
1.
6. The method for separating and purifying a cyclization oxidation reaction mixture according to claim 4, characterized in that: The extraction flow ratio of the C4~C16 liquid halogenated hydrocarbons to the epoxides in the methanol primary purification solution in the static mixer 5 is 5~10:
1.
7. The method for separating and purifying a cyclization oxidation reaction mixture according to claim 6, characterized in that: The C4-C16 liquid halogenated hydrocarbons are at least one of 3-chloropropene, 1,2-dibromopropane, 1,6-dibromohexane, bromobenzene, m-dibromobenzene, and 1,4-dichlorobutane, and the purity of the C4-C16 liquid halogenated hydrocarbons is ≥99.3%.
8. The method for separating and purifying a cyclization oxidation reaction mixture according to claim 4, characterized in that: The flow ratio of the epoxide primary purification liquid to water in the static mixer 4 is 1.5~2:1, the pressure drop is 0.05~0.4MPa, and the flow velocity is 0.5~1.5m / s.
9. The method for separating and purifying a cyclization oxidation reaction mixture according to claim 4, characterized in that: The extraction flow ratio of methanol to water in the primary epoxide fraction in the static mixer 4 is 1~3:
100.
10. The method for separating and purifying a cyclization oxidation reaction mixture according to claim 4, characterized in that: The total epoxide content in the methanol secondary purification solution is ≤0.01%; the methanol content in the epoxide secondary purification solution is ≤0.01%.
Citation Information
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