An apparatus and method for producing a hemiacetal
By designing a production unit with multi-step reaction and refining processes, the problems of low selectivity and difficult separation in diethylene glycol production have been solved, achieving high selectivity and high purity diethylene glycol production, which is suitable for continuous industrial operation.
Patent Information
- Application Number
- CN202311290202.X
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-10-07
- Publication Date
- 2025-11-21
- Estimated Expiration
- 2043-10-07
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Figure CN119771289B_ABST
Abstract
Description
Technical Field
[0001] This application relates to an apparatus and method for producing alcohol condensation, belonging to the field of chemical technology. Background Technology
[0002] Diethylene glycol, also known as diethylene glycol condensate, is commonly used as an organic solvent, antifreeze, desiccant, softener, and plasticizer. It is widely applied in the oil, resin, nitrocellulose, dye, and other daily chemical industries, as well as in equipment manufacturing. Currently, diethylene glycol products are mostly byproducts of the hydration of ethylene oxide to produce ethylene glycol, typically accounting for 8% to 10% of total ethylene glycol production. In recent years, with the continuous development of my country's polyester industry and the increasing demands of advanced equipment manufacturing, the demand for diethylene glycol has also been rising. Therefore, the fact that diethylene glycol is a byproduct severely limits its production capacity, making the exploration of new diethylene glycol synthesis routes particularly urgent.
[0003] Ethylene glycol dehydration condensation is an excellent green production process for diethylene glycol, characterized by high conversion rates, but it suffers from low selectivity, and the byproducts can form azeotropes with water. This application proposes a product / byproduct separation and purification process to address the product characteristics of this diethylene glycol synthesis method. This process enables continuous production and improves the overall selectivity of diethylene glycol, making it suitable for industrial-scale continuous production. Summary of the Invention
[0004] According to one aspect of this application, an apparatus for producing alcohol condensates is provided, the apparatus comprising a condensation reaction unit A, a separation and purification unit B, an esterification reaction unit C, an esterification separation unit D, a hydrolysis reaction unit E, and a hydrolysis separation unit F connected in sequence.
[0005] The separation and purification unit B is connected to the condensation reaction unit A, the hydrolysis reaction unit E, and the esterification unit C.
[0006] The hydrolysis separation unit F is connected to the condensation reaction unit A, the esterification separation unit D, and the hydrolysis reaction unit E.
[0007] The condensation reaction unit A includes a condensation preheater, a condensation reactor, and a condensation condenser connected in sequence.
[0008] The separation and purification unit B includes a formaldehyde removal tower, a light volatile organic compound removal tower, a condensation wastewater tower, and a product tower connected in sequence.
[0009] The esterification reaction unit C includes an esterification preheater and an esterification reactor connected in sequence.
[0010] The esterification separation unit D includes an impurity oil tower, a deesterification tower, and a concentration tower connected in sequence.
[0011] The hydrolysis reaction unit E includes a hydrolysis preheater and a hydrolysis reactor connected in sequence.
[0012] The hydrolysis separation unit F includes a dealcoholization tower and a recovery tower connected in sequence.
[0013] Optionally, the preheating temperature of the condensation preheater is 100–350°C.
[0014] Optionally, the reaction temperature of the condensation reactor is 100–350°C.
[0015] Optionally, the reaction pressure of the condensation reactor is 100–500 kPaA.
[0016] Optionally, the operating temperature of the condensation condenser is 40–200°C.
[0017] Optionally, the reflux ratio of the formaldehyde removal tower is 150 to 350.
[0018] Optionally, the theoretical number of plates in the formaldehyde removal tower is 10 to 80.
[0019] Optionally, the temperature at the top of the formaldehyde removal tower is 20–50°C.
[0020] Optionally, the operating pressure of the formaldehyde removal tower is 100–300 kPaA.
[0021] Optionally, the reflux ratio of the light-light-removal tower is 0.5 to 20.
[0022] Optionally, the theoretical number of plates in the light-light removal tower is 10 to 80.
[0023] Optionally, the temperature at the top of the light-weight removal tower is 50–150°C.
[0024] Optionally, the operating pressure of the light-light removal tower is 100–300 kPaA.
[0025] Optionally, the reflux ratio of the condensation wastewater tower is 0.01 to 5.
[0026] Optionally, the theoretical number of trays in the condensation wastewater tower is 10 to 80.
[0027] Optionally, the temperature at the top of the condensation wastewater tower is 30–100°C.
[0028] Optionally, the operating pressure of the condensation wastewater tower is 0.1 to 300 kPaA.
[0029] Optionally, the reflux ratio of the product tower is 5 to 30.
[0030] Optionally, the product tower has 10 to 80 theoretical plates.
[0031] Optionally, the top temperature of the product tower is 60–150°C.
[0032] Optionally, the operating pressure of the product tower is 0.1 to 150 kPaA.
[0033] Optionally, the preheating temperature of the esterification preheater is 60–150°C.
[0034] Optionally, the reaction temperature of the esterification reactor is 60–150°C.
[0035] Optionally, the reaction pressure of the esterification reactor is 100–500 kPaA.
[0036] Optionally, the reflux ratio of the impurity oil tower is 20 to 260.
[0037] Optionally, the theoretical number of plates in the impurity oil tower is 10 to 80.
[0038] Optionally, the top temperature of the impurity oil tower is 70–200°C.
[0039] Optionally, the operating pressure of the impurity oil tower is 100–300 kPaA.
[0040] Optionally, the reflux ratio of the deesterification tower is 0.01 to 5.
[0041] Optionally, the number of theoretical plates in the deesterification column is 10 to 50.
[0042] Optionally, the top temperature of the deesterification column is 40–120°C.
[0043] Optionally, the operating pressure of the deesterification tower is 1–300 kPaA.
[0044] Optionally, the reflux ratio of the concentration tower is 0.1 to 5.
[0045] Optionally, the concentration tower has 15 to 80 theoretical plates.
[0046] Optionally, the top temperature of the concentration tower is 40–120°C.
[0047] Optionally, the operating pressure of the concentration tower is 100–300 kPaA.
[0048] Optionally, the preheating temperature of the hydrolysis preheater is 80–350°C.
[0049] Optionally, the reaction temperature of the hydrolysis reactor is 80–350°C.
[0050] Optionally, the reaction pressure of the hydrolysis reactor is 100–500 kPaA.
[0051] Optionally, the reflux ratio of the dealcoholization column is 3 to 30.
[0052] Optionally, the number of theoretical plates in the dealcoholization column is 15 to 80.
[0053] Optionally, the top temperature of the dealcoholization column is 40–120°C.
[0054] Optionally, the operating pressure of the dealcoholization tower is 1–300 kPaA.
[0055] Optionally, the reflux ratio of the recovery tower is 0.05 to 20.
[0056] Optionally, the theoretical number of trays in the recovery tower is 10 to 65.
[0057] Optionally, the temperature at the top of the recovery tower is 40–120°C.
[0058] Optionally, the operating pressure of the recovery tower is 1 to 300 kPaA.
[0059] According to another aspect of this application, a method for producing an alcohol condensate is provided, wherein a raw material containing ethylene glycol is passed into a production apparatus and reacted to obtain diethylene glycol;
[0060] The production equipment is selected from the production equipment described above.
[0061] Optionally, the production method includes the following steps:
[0062] (1) Pass the raw material containing ethylene glycol into the condensation reaction unit A, and the condensation reaction is carried out to obtain the condensation product containing diethylene glycol.
[0063] (2) The condensation product containing diethylene glycol is passed into the separation and purification unit B for purification and separation to obtain diethylene glycol, acetaldehyde, unreacted ethylene glycol, and byproducts containing dioxane.
[0064] The diethylene glycol is discharged from the bottom of the product column;
[0065] The unreacted ethylene glycol enters condensation reaction unit A to continue the reaction;
[0066] (3) Pass the mixture of dioxane-containing byproduct and acetic acid into esterification reaction unit C, and esterify to obtain a product containing ethylene glycol acetate.
[0067] (4) The product containing ethylene glycol acetate is passed into the esterification separation unit D for separation and purification to obtain the purified product containing ethylene glycol acetate and recycled acetic acid.
[0068] (5) Pass the purified product containing ethylene glycol acetate into the hydrolysis reaction unit E for hydrolysis reaction to obtain the product containing ethylene glycol and acetic acid.
[0069] (6) The product containing ethylene glycol is separated by hydrolysis separation unit F and then introduced into condensation reaction unit A as a raw material to participate in the reaction.
[0070] Optionally, in step (1), the raw materials include fresh ethylene glycol, ethylene glycol produced in separation and purification unit B and hydrolysis separation unit F.
[0071] Optionally, in step (3), the acetic acid includes fresh acetic acid and acetic acid produced in the esterification separation unit D cycle.
[0072] As a specific implementation scheme, this application achieves its purpose through the following technical solution:
[0073] (1) Fresh ethylene glycol is mixed with ethylene glycol recovered from separation and purification unit B and hydrolysis separation unit F and then sent to condensation reaction unit A. It is heated to the reaction temperature in condensation preheater and sent to condensation reactor to undergo dehydration condensation reaction. The reaction product is condensed by condensation condenser and then sent to separation and purification unit B.
[0074] (2) The condensation reaction product after condensation is sent to the separation and purification unit B. It is first separated by the dealdehyde tower. The by-product acetaldehyde is separated at the top of the tower, and the dealdehyde material at the bottom of the tower is sent to the light removal tower.
[0075] (3) The light impurities by-products are separated from the top of the light removal tower and sent to the esterification reaction unit C. The dehydrogenation products obtained from the bottom of the tower are sent to the condensation wastewater tower.
[0076] (4) Wastewater is separated at the top of the condensation wastewater tower and sent to the hydrolysis reaction unit E, while the heavy mixture at the bottom of the tower is sent to the product tower.
[0077] (5) The unreacted ethylene glycol feedstock is separated at the top of the product column by distillation and recycled, while diethylene glycol product is obtained at the bottom of the column;
[0078] (6) The by-product light impurities from the top of the light removal tower are sent to the esterification reaction unit C, heated to the reaction temperature by the esterification preheater, and then sent to the esterification reactor. The esterification reaction product is sent to the esterification separation unit D.
[0079] (7) The esterification reaction product first enters the impurity oil tower in the esterification separation unit D, where the impurity oil is separated at the top of the tower and the light-removed product is obtained at the bottom of the tower and sent to the deesterification tower.
[0080] (8) The deesterification tower obtains dilute acetic acid at the top of the tower through distillation, which is sent to the concentration tower, and obtains acetate at the bottom of the tower, which is sent to the hydrolysis reaction unit E.
[0081] (9) Dilute acetic acid is separated into wastewater at the top of the concentration tower. Part of the wastewater is discharged and part of the wastewater is sent to the hydrolysis reaction unit E. The concentration of acetic acid solution at the bottom of the concentration tower meets the standard and is sent to the esterification reaction unit C for recycling as esterification raw material.
[0082] (10) In the hydrolysis reaction unit E, the acetate from the esterification separation unit D and the wastewater are mixed and heated to the reaction temperature by the hydrolysis preheater and sent to the hydrolysis reactor. The hydrolysis reaction products are sent to the hydrolysis separation unit F.
[0083] (11) The hydrolysis reaction product is sent to the hydrolysis separation unit F, first entering the alcohol removal tower, where the hydrolyzed ethylene glycol is obtained at the bottom of the tower and sent to the condensation reaction unit A. The light component obtained at the top of the tower is sent to the recovery tower.
[0084] (12) The dilute acetic acid obtained from the top of the recovery tower is sent to the esterification separation unit D, and the unreacted acetate obtained from the bottom of the tower is sent to the hydrolysis reaction unit E.
[0085] In this application, fresh ethylene glycol is mixed with ethylene glycol recovered from separation and purification unit B and hydrolysis separation unit F, and then undergoes a dehydration condensation reaction in condensation reaction unit A to obtain a condensation product containing diethylene glycol, which is sent to separation and purification unit B. Separation and purification unit B separates diethylene glycol product, acetaldehyde byproduct, unreacted ethylene glycol, wastewater, and dioxane-containing byproduct. Acetaldehyde and diethylene glycol are sent out, unreacted ethylene glycol is returned to condensation reaction unit A, wastewater is sent to hydrolysis reaction unit E, and byproduct is sent to esterification reaction unit C. The dioxane-containing byproduct from separation and purification unit B, together with fresh acetic acid and recycled acetic acid from esterification separation unit D, enters esterification reaction unit C to undergo an esterification reaction to produce ethylene glycol acetate, and the reaction product is sent to esterification separation unit D. Esterification separation unit D separates and purifies the esterification reaction product to obtain ethylene glycol acetate, wastewater, and recycled acetic acid. Recycled acetic acid is returned to esterification reaction unit C, while ethylene glycol acetate and some wastewater are sent to hydrolysis reaction unit E, and the remaining wastewater is discharged. Wastewater and ethylene glycol acetate from esterification separation unit D, wastewater from separation and purification unit B, and wastewater from hydrolysis separation unit F enter hydrolysis reaction unit E, where hydrolysis occurs, partially producing acetic acid and ethylene glycol, which are sent to hydrolysis separation unit F. Recycled ethylene glycol separated in hydrolysis separation unit F is sent to condensation reaction unit A, the separated ethylene glycol acetate is sent to esterification separation unit D, and the separated unreacted ethylene glycol acetate is sent to hydrolysis reaction unit E for recycling.
[0086] In this application, "fresh ethylene glycol" and "fresh acetic acid" refer to ethylene glycol and acetic acid purchased through commercial channels and used directly as raw materials.
[0087] The beneficial effects that this application can produce include:
[0088] The alcohol condensation production apparatus disclosed in this application is used for the separation and purification of diethylene glycol produced by the dehydration condensation reaction of ethylene glycol. The process is continuous and easy to operate, and has industrial feasibility.
[0089] The alcohol production method disclosed in this application involves six units: ethylene glycol condensation reaction, separation and purification, esterification reaction, esterification separation, hydrolysis reaction, and hydrolysis separation. This process achieves the production and purification of diethylene glycol through dehydration condensation, yielding a diethylene glycol product with a molar concentration of 99.9%. Furthermore, the process conversion rate is improved and the separation difficulty is reduced through by-product treatment. The process is continuous, easy to operate, and has industrial feasibility. Attached Figure Description
[0090] Figure 1 This is a schematic diagram of a process for producing an alcohol condensate according to this application.
[0091] Figure 2 This is a process flow diagram of condensation reaction unit A and separation and purification unit B in this application.
[0092] Figure 3 This is a process flow diagram of esterification reaction unit C and esterification separation unit D of this application.
[0093] Figure 4 This is a process flow diagram of hydrolysis reaction unit E and hydrolysis separation unit F.
[0094] Figure 1 In the diagram: A. Condensation reaction unit; B. Separation and purification unit; C. Esterification reaction unit; D. Esterification separation unit; E. Hydrolysis reaction unit; F. Hydrolysis separation unit.
[0095] 1. Condensation preheater; 2. Condensation reactor; 3. Condensation condenser; 4. Dealdehyde removal tower; 5. Light volatile matter removal tower; 6. Condensation wastewater tower; 7. Product tower; 8. Esterification preheater; 9. Esterification reactor; 10. Impurity oil tower; 11. Deesterification tower; 12. Concentration tower; 13. Hydrolysis preheater; 14. Hydrolysis reactor; 15. De-alcoholization tower; 16. Recovery tower. Detailed Implementation
[0096] The present application is described in detail below with reference to the embodiments, but the present application is not limited to these embodiments.
[0097] Unless otherwise specified, all raw materials used in the embodiments of this application were purchased through commercial channels.
[0098] Example 1
[0099] like Figure 1 As shown, the alcohol production unit includes a condensation reaction unit A, a separation and purification unit B, an esterification reaction unit C, an esterification separation unit D, a hydrolysis reaction unit E, and a hydrolysis separation unit F.
[0100] like Figure 2 As shown, condensation reaction unit A includes condensation preheater 1, condensation reactor 2 and condensation condenser 3; the dehydration condensation raw material is heated to the reaction temperature in condensation preheater 1 and sent to condensation reactor 2; the condensation reaction product is condensed by condensation condenser 3 and then sent to separation and purification unit B. Separation and purification unit B includes a formaldehyde removal tower 4, a light impurity removal tower 5, a condensation wastewater tower 6, and a product tower 7. The raw material is fed into the formaldehyde removal tower 4, where acetaldehyde, a byproduct, is separated at the top. The formaldehyde-removed material at the bottom of the formaldehyde removal tower 4 is sent to the light impurity removal tower 5, where light impurities, a byproduct, are separated at the top and sent to the esterification reaction unit C. The dehydrogenation product obtained at the bottom of the tower is sent to the condensation wastewater tower 6. Wastewater is separated at the top of the condensation wastewater tower 6 and sent to the hydrolysis reaction unit E. The heavy mixture at the bottom of the condensation wastewater tower 6 is sent to the product tower 7. The product tower 7 separates unreacted ethylene glycol raw material at the top for recycling through distillation, and diethylene glycol is obtained at the bottom.
[0101] like Figure 3 As shown, esterification reaction unit C includes an esterification preheater 8 and an esterification reactor 9. Acetic acid and by-product light impurities are mixed with recycled acetic acid, heated to the reaction temperature by the esterification preheater 8, and then sent to the esterification reactor 9. The resulting esterification reaction product is sent to the esterification separation unit D. Esterification separation unit D includes an impurity oil tower 10, a deesterification tower 11, and a concentration tower 12. The esterification reaction product is sent to the impurity oil tower 10, where impurity oil is separated at the top and a de-light product is obtained at the bottom, which is sent to the deesterification tower 11. The deesterification tower 11 undergoes distillation to obtain dilute acetic acid at the top, which is sent to the concentration tower 12. Acetic acid ester is obtained at the bottom of the deesterification tower 11 and sent to the hydrolysis reaction unit E. Wastewater is separated from the dilute acetic acid at the top of the concentration tower 12. Part of the wastewater is discharged, and part is sent to the hydrolysis reaction unit E. The acetic acid solution with the required concentration is obtained at the bottom of the concentration tower 12 and is sent to the esterification reaction unit C for recycling as esterification feedstock.
[0102] like Figure 4 As shown, hydrolysis reaction unit E includes a hydrolysis preheater 13 and a hydrolysis reactor 14. Acetic acid ester and wastewater from esterification separation unit D are mixed and heated to the reaction temperature by the hydrolysis preheater 13 before being sent to the hydrolysis reactor 14. The hydrolysis reaction product is sent to hydrolysis separation unit F. Hydrolysis separation unit F includes a dealcoholization tower 15 and a recovery tower 16. The hydrolysis reaction product is sent to the dealcoholization tower 15, where ethylene glycol generated by hydrolysis is obtained at the bottom and sent to condensation reaction unit A. The light component obtained at the top of the dealcoholization tower 15 is sent to the recovery tower 16. The dilute acetic acid obtained at the top of the recovery tower 16 is sent to the esterification separation unit D, and the unreacted acetate obtained at the bottom is sent to the hydrolysis reaction unit E.
[0103] Example 2
[0104] like Figures 1-4As shown, fresh ethylene glycol is mixed with ethylene glycol recovered from separation and purification unit B and hydrolysis separation unit F and then fed into condensation reaction unit A. It is heated to 210°C in condensation preheater 1 and then sent to condensation reactor 2. A dehydration condensation reaction occurs at 210°C and 120 kPa A to obtain a condensation product containing diethylene glycol. The condensation product containing diethylene glycol is condensed to 110°C in condensation condenser 3 and then completely condensed and sent to separation and purification unit B.
[0105] The condensed product containing diethylene glycol is sent to separation and purification unit B, where it is first separated in aldehyde removal tower 4. The pressure at the top of aldehyde removal tower 4 is 150 kPaA, the temperature at the top is 32°C, 30 theoretical plates are set, and the reflux ratio is 305.3. Acetaldehyde with a molar concentration of 99.6% is separated at the top of the tower. The dealdehyde-removed material at the bottom of aldehyde removal tower 4 is sent to light impurity removal tower 5. The pressure at the top of light impurity removal tower 5 is 110 kPaA, the temperature at the top is 91°C, 30 theoretical plates are set, and the reflux ratio is 5. Light impurities are separated at the top of light impurity removal tower 5 and sent to esterification reaction unit C. The dehydrogenation product obtained at the bottom of light impurity removal tower 5 is sent to condensation wastewater tower 6. The top pressure of condensation wastewater tower 6 is 10 kPaA, the top temperature is 46℃, it has 30 theoretical plates, and a reflux ratio of 0.5. Wastewater is separated at the top of condensation wastewater tower 6 and sent to hydrolysis reaction unit E. The heavy mixture at the bottom of condensation wastewater tower 6 is sent to product tower 7. The top pressure of product tower 7 is 5 kPaA, the top temperature is 117℃, it has 40 theoretical plates, and a reflux ratio of 15. Unreacted ethylene glycol feedstock is separated at the top of the tower by distillation and recycled. The bottom of the tower yields diethylene glycol product with a molar concentration of 99.9%. The by-product light impurities from the top of light impurity removal tower 5 are sent to esterification reaction unit C. After being heated to 98℃ by esterification preheater 8, it is sent to esterification reactor 9. Esterification occurs at 98℃ and 110 kPaA to produce ethylene glycol acetate. The ethylene glycol acetate product is sent to esterification separation unit D. The esterification product, ethylene glycol acetate, first enters the impurity oil tower 10 in esterification separation unit D. The top pressure of impurity oil tower 10 is 110 kPaA, the top temperature is 90°C, it has 32 theoretical plates, and a reflux ratio of 180. Impurity oil is separated at the top, and the product obtained at the bottom is sent to the deesterification tower 11. The top pressure of deesterification tower 11 is 30 kPaA, the top temperature is 70°C, it has 20 theoretical plates, and a reflux ratio of 0.08. Through distillation, dilute acetic acid is obtained at the top and sent to the concentration tower 12. Acetic acid is obtained at the bottom and sent to the hydrolysis reaction unit E. The concentration tower 12 has a top pressure of 110 kPaA and a top temperature of 102°C. It has 30 theoretical plates and a reflux ratio of 2. Dilute acetic acid separates into wastewater at the top of the concentration tower 12. Part of the wastewater is discharged, and the rest is sent to the hydrolysis reaction unit E. The bottom of the concentration tower 12 yields a circulating acetic acid solution with the required concentration, which is used as esterification feedstock and recycled to the esterification reaction unit C. In the hydrolysis reaction unit E, acetate from the esterification separation unit D is mixed with wastewater and heated to 150°C by the hydrolysis preheater 13 before being sent to the hydrolysis reactor 14. Hydrolysis occurs under operating conditions of 150°C and 130 kPaA. The resulting hydrolysis product is sent to the hydrolysis separation unit F. The hydrolysis reaction product is sent to the hydrolysis separation unit F, and first enters the dealcoholization tower 15. The top pressure of the dealcoholization tower 15 is 10 kPaA, the top temperature is 56℃, there are 60 theoretical plates, and the reflux ratio is 14. Ethylene glycol generated by hydrolysis is obtained at the bottom of the dealcoholization tower 15 and sent to the condensation reaction unit A. The light component obtained at the top of the tower is sent to the recovery tower 16.The pressure at the top of recovery tower 16 is 30 kPaA, the temperature at the top of the tower is 76℃, there are 20 theoretical plates, and the reflux ratio is 0.2. The dilute acetic acid obtained from the top of recovery tower 16 is sent to the esterification separation unit D, and the unreacted acetate obtained from the bottom of recovery tower 16 is sent to the hydrolysis reaction unit E.
[0106] The above description is merely a few embodiments of this application and is not intended to limit this application in any way. Although this application discloses preferred embodiments as described above, it is not intended to limit this application. Any changes or modifications made by those skilled in the art without departing from the scope of the technical solution of this application using the disclosed technical content are equivalent to equivalent implementation cases and fall within the scope of the technical solution.
Claims
1. A method for producing alcohol condensation, characterized in that, The production method includes: The raw material containing ethylene glycol is fed into the production unit and reacted to obtain diethylene glycol; The production method specifically includes the following steps: (1) The raw material containing ethylene glycol is passed into the condensation reaction unit A and condensation reaction is carried out to obtain the condensation product containing diethylene glycol. (2) The condensation product containing diethylene glycol is passed into the separation and purification unit B for purification and separation to obtain diethylene glycol, acetaldehyde, unreacted ethylene glycol, and byproducts containing dioxane. The diethylene glycol is discharged from the bottom of the product tower (7); The unreacted ethylene glycol enters condensation reaction unit A to continue the reaction; (3) Pass the mixture of dioxane-containing byproduct and acetic acid into esterification reaction unit C for esterification reaction to obtain a product containing ethylene glycol acetate; (4) The product containing ethylene glycol acetate is passed into the esterification separation unit D for separation and purification to obtain the purified product containing ethylene glycol acetate and recycled acetic acid; (5) The purified product containing ethylene glycol acetate is passed into the hydrolysis reaction unit E for hydrolysis reaction to obtain the product containing ethylene glycol and acetic acid; (6) After the product containing ethylene glycol is separated by hydrolysis separation unit F, it is introduced into condensation reaction unit A as a raw material to participate in the reaction.
2. The production method according to claim 1, characterized in that, In step (1), the raw materials include fresh ethylene glycol, ethylene glycol produced in separation and purification unit B and hydrolysis separation unit F; In step (3), the acetic acid includes fresh acetic acid and acetic acid produced in the esterification separation unit D cycle.
3. An apparatus for producing alcohol condensation, applied to the production method according to any one of claims 1-2, characterized in that, The production apparatus includes a condensation reaction unit A, a separation and purification unit B, an esterification reaction unit C, an esterification separation unit D, a hydrolysis reaction unit E, and a hydrolysis separation unit F connected in sequence. The separation and purification unit B is connected to the condensation reaction unit A, the hydrolysis reaction unit E, and the esterification unit C. The hydrolysis separation unit F is connected to the condensation reaction unit A, the esterification separation unit D, and the hydrolysis reaction unit E. The condensation reaction unit A includes a condensation preheater (1), a condensation reactor (2), and a condensation condenser (3) connected in sequence. The separation and purification unit B includes a formaldehyde removal tower (4), a light volatile organic compound removal tower (5), a condensation wastewater tower (6), and a product tower (7) connected in sequence. The esterification reaction unit C includes an esterification preheater (8) and an esterification reactor (9) connected in sequence. The esterification separation unit D includes an impurity oil tower (10), a deesterification tower (11), and a concentration tower (12) connected in sequence. The hydrolysis reaction unit E includes a hydrolysis preheater (13) and a hydrolysis reactor (14) connected in sequence. The hydrolysis separation unit F includes a dealcoholization tower (15) and a recovery tower (16) connected in sequence.
4. The production apparatus according to claim 3, characterized in that, The preheating temperature of the condensation preheater (1) is 100~350℃; The reaction temperature of the condensation reactor (2) is 100~350℃ and the reaction pressure is 100~500kPaA; The operating temperature of the condensation condenser (3) is 40~200℃.
5. The production apparatus according to claim 3, characterized in that, The formaldehyde removal tower (4) has a reflux ratio of 150~350, a theoretical number of trays of 10~80, a top temperature of 20~50 ℃, and an operating pressure of 100~300 kPaA. The reflux ratio of the light-light removal tower (5) is 0.5~20, the theoretical number of trays is 10~80, the top temperature is 50~150 ℃, and the operating pressure is 100~300kPaA.
6. The production apparatus according to claim 3, characterized in that, The reflux ratio of the condensation wastewater tower (6) is 0.01~5, the theoretical number of trays is 10~80, the top temperature is 30~100 ℃, and the operating pressure is 0.1~300kPaA. The product tower (7) has a reflux ratio of 5 to 30, a theoretical number of trays of 10 to 80, a top temperature of 60 to 150 ℃, and an operating pressure of 0.1 to 150 kPaA.
7. The production apparatus according to claim 3, characterized in that, The preheating temperature of the esterification preheater (8) is 60~150℃; The reaction temperature of the esterification reactor (9) is 60~150℃ and the reaction pressure is 100~500kPaA; The reflux ratio of the impurity oil tower (10) is 20~260, the theoretical number of trays is 10~80, the top temperature is 70~200 ℃, and the operating pressure is 100~300kPaA. The deesterification tower (11) has a reflux ratio of 0.01~5, a theoretical number of trays of 10~50, a top temperature of 40~120 ℃, and an operating pressure of 1~300kPaA. The reflux ratio of the concentration tower (12) is 0.1~5, the theoretical number of trays is 15~80, the top temperature is 40~120 ℃, and the operating pressure is 100~300kPaA.
8. The production apparatus according to claim 3, characterized in that, The preheating temperature of the hydrolysis preheater (13) is 80~350℃; The reaction temperature of the hydrolysis reactor (14) is 80~350 ℃ and the reaction pressure is 100~500 kPaA.
9. The production apparatus according to claim 3, characterized in that, The reflux ratio of the dealcoholization column (15) is 3~30, the theoretical number of plates is 15~80, the top temperature is 40~120 ℃, and the operating pressure is 1~300kPaA; The reflux ratio of the recovery tower (16) is 0.05~20, the theoretical number of trays is 10~65, the top temperature is 40~120 ℃, and the operating pressure is 1~300kPaA.
Citation Information
Patent Citations
Refining device and refining method of polymerization product and application
CN119425127A