Continuous efficient reaction device for glycol ketal or acetal
By combining a condensation tower, an oil-water separator, and a distillation tower in a continuous and efficient reaction unit, the problem of separating impurities caused by the introduction of azeotropic agents is solved, and efficient and low-cost production of diol ketals or acetals is achieved, which has great industrial value.
Patent Information
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- 武汉希音新材料科技有限公司
- Filing Date
- 2024-12-31
- Publication Date
- 2026-05-12
AI Technical Summary
In the prior art, the synthesis methods of diol ketals or acetals require the introduction of azeotropic agents, which increases the types of impurities to be separated and makes it difficult to achieve a complete reaction, especially when diols are used as raw materials.
The system employs a continuous and efficient reaction apparatus, including a condensation tower, an oil-water separator, a distillation tower, and a vacuum system. The reaction is promoted by a catalyst, and the reaction is fully carried out without the introduction of an azeotropic agent. The combined processing of oil-water separation and distillation tower enables efficient separation and recycling of the products.
This technology enables efficient condensation reactions of diol ketals or acetals without azeotropic agents, achieving continuous processing, reducing investment costs, and improving product purity and yield.
Smart Images
Figure CN224220755U_ABST
Abstract
Description
Technical Field
[0001] This application relates to the field of fine chemical production, and in particular to a continuous and efficient reaction apparatus for diol ketals or acetals. Background Technology
[0002] Diol ketals or acetals can be catalytically hydrogenated to produce a series of hydroxy ethers. This is particularly effective for ketones and aldehydes with highly branched carbon chains; condensation with diols followed by hydrogenolysis yields the corresponding hydroxy ethers, avoiding the use of hazardous raw materials such as ethylene oxide, propylene oxide, and butane oxide. It also simplifies the subsequent processing of polyethers.
[0003] In related technologies, the commonly used methods for synthesizing ketals and acetals typically employ azeotropic agents to remove water and promote a complete reaction. This method requires the introduction of additional azeotropic agents, increasing the variety of impurities that can be separated. Furthermore, when using diols as one of the raw materials, the high hygroscopicity of diols makes it difficult to achieve a complete reaction through water removal.
[0004] In view of this, there is an urgent need for a continuous and efficient device for producing diol ketals or acetals that can promote the condensation reaction of ketals or acetals without the introduction of azeotropic agents. Utility Model Content
[0005] This application provides a continuous and efficient reaction apparatus for diol ketals or acetals, which can promote the full condensation reaction of diol ketals or acetals without the introduction of azeotropic agents. The process is continuous, the investment is low, and it has great industrial value.
[0006] Firstly, the continuous and efficient reaction apparatus for diol ketals or acetals provided in this application adopts the following technical solution:
[0007] A continuous and efficient reaction apparatus for diol ketals or acetals, comprising:
[0008] A condensation tower, filled with a catalyst;
[0009] An oil-water separator is connected to the output end of the condensation tower and is used to receive and separate the products to form an oil phase and a water phase. The oil-water separator has a first outlet for outputting the water phase.
[0010] A distillation column is connected to the first outlet of the oil-water separator for receiving and separating the aqueous phase to form diol and water. The distillation column has a second outlet for outputting diol and a third outlet for outputting water.
[0011] The third discharge port is connected to the output end of the condensation tower and is used to replenish the condensation tower with raw materials.
[0012] Furthermore, the third discharge port is connected to a cooling recovery structure, which includes a heat exchanger and a transfer tank connected in sequence.
[0013] Furthermore, the transfer tank is connected to a vacuum system to provide a vacuum environment for the distillation column.
[0014] Furthermore, the input end of the condensation tower is provided with a pretreatment structure, the pretreatment structure including:
[0015] A mixer, the output of which is connected to the input of the condensation tower;
[0016] A pair of feed pipes, both of which are connected to the input end of the mixer.
[0017] Furthermore, a first heater is provided between the pretreatment structure and the condensation tower; or
[0018] The pretreatment structure is equipped with a first heater for heating the raw materials.
[0019] Furthermore, the oil-water separator has a fourth outlet and a fifth outlet for outputting the oil phase, and the fourth outlet or the fifth outlet is connected to the input end of the mixer.
[0020] Furthermore, the distillation column includes a rectification section and a stripping section arranged sequentially from bottom to top. The rectification section is provided with 8 to 10 trays, and the stripping section is provided with 3 to 5 trays.
[0021] Furthermore, the distillation section is connected to the first discharge port via a pipeline, and a second heater is installed on the pipeline.
[0022] Furthermore, the catalyst is at least one of A-15 resin or 732 resin.
[0023] In summary, this application includes at least one of the following beneficial technical effects:
[0024] 1. This application includes an oil-water separator and a distillation column. The oil-water separator can separate the target product, diol ketal or acetal (i.e., the oil phase), from the mixture of diol and water (i.e., the aqueous phase). The aqueous phase is output to the distillation column. After the water is removed by distillation, the separated diol can be used as a raw material to be fed back into the condensation column to carry out a condensation reaction with ketones or aldehydes. It has the characteristics of continuous process, low investment, and no need to carry water with an azeotropic agent to promote the reaction of diol ketal or acetal, and has great industrial value.
[0025] 2. This application includes a mixer and a first heater. Before entering the distillation column, the raw material is preheated by the first heater and then thoroughly mixed in the mixer, thereby promoting the efficient condensation reaction.
[0026] 3. This application includes a vacuum system and a cooling recovery system. The vacuum system provides a vacuum environment for the distillation column, making the distillation process more stable and efficient. The water vapor formed after distillation can be captured by the cooling recovery system and stored in a transfer tank as liquid water for further processing and discharge. Attached Figure Description
[0027] Figure 1 This is a schematic diagram of the continuous and efficient reaction apparatus for glycol ketals or acetals in this application.
[0028] In the diagram, 1 is the condensation tower; 2 is the oil-water separator; 21 is the first discharge port; 22 is the fourth discharge port; 23 is the fifth discharge port; 3 is the distillation tower; 31 is the second discharge port; 32 is the third discharge port; 4 is the cooling recovery structure; 41 is the heat exchanger; 42 is the transfer tank; 5 is the vacuum system; 6 is the pretreatment structure; 61 is the mixer; 62 is the feed pipe; 7 is the first heater; and 8 is the second heater. Detailed Implementation
[0029] The following will be combined with the appendix Figure 1 The technical solution of this application is clearly and completely described. The following embodiments are exemplary and are only used to explain this application, and should not be construed as limiting this application. In the following description, the same reference numerals are used to denote the same or equivalent elements, and repeated descriptions are omitted.
[0030] In the description of this application, it should be understood that the terms "upper", "lower", "inner", "outer", "left", "right", etc., indicate the orientation or positional relationship based on the orientation or positional relationship shown in the accompanying drawings, or the orientation or positional relationship commonly used when the product of this application is in use, or the orientation or positional relationship commonly understood by those skilled in the art. They are only used to facilitate the description of this application and to simplify the description, and are not intended to indicate or imply that the equipment or component referred to must have a specific orientation, or be constructed and operated in a specific orientation. Therefore, they should not be construed as limitations on this application.
[0031] Furthermore, the terms "installation," "connection," and "linking" should be interpreted broadly. For example, they can refer to fixed connections, detachable connections, or integral connections; they can refer to mechanical connections or electrical connections; they can refer to direct connections or indirect connections through an intermediate medium; and they can refer to the internal connection between two components. Those skilled in the art can understand the specific meaning of the above terms in this application based on the specific circumstances.
[0032] It should also be further understood that the term "and / or" as used in this application specification and the corresponding claims refers to any combination of one or more of the listed items and all possible combinations.
[0033] A continuous and efficient reaction apparatus for diol ketals or acetals, as described above. Figure 1 It includes a condensation tower 1, an oil-water separator 2, and a distillation tower 3. The condensation tower 1 is filled with a catalyst. The oil-water separator 2 is connected to the output end of the condensation tower 1 and is used to receive and separate the products to form an oil phase and an aqueous phase.
[0034] During production, raw materials are fed into condensation tower 1 to carry out a condensation reaction and obtain the product. The raw materials include diols, ketones or aldehydes.
[0035] In one specific embodiment, the raw materials are set as ketone and diol, wherein the ketone is set as a long carbon chain structure (which may contain branches or not), specifically set as at least one of C10 to C18 ketones, and the ketone and diol undergo a condensation reaction with the aid of a catalyst to obtain diol ketal and water.
[0036] In another specific embodiment, the raw materials are set as aldehyde and diol, wherein the aldehyde is set as a long carbon chain structure (which may contain branches or not), specifically set as at least one of C10 to C18 aldehydes, and the aldehyde and diol undergo a condensation reaction with the aid of a catalyst to obtain diol acetal and water.
[0037] The catalyst can be specifically configured according to the actual situation, and it is at least set to either A-15 resin or 732 resin. In one specific embodiment, the catalyst is set to A-15 resin, and in another specific embodiment, the catalyst is set to 732 type resin. Both catalysts can promote the condensation reaction.
[0038] Reference Figure 1 The input end of the condensation tower 1 is equipped with a pretreatment structure 6 for pretreatment of the raw materials.
[0039] Specifically, the pretreatment structure 6 includes a mixer 61 and a pair of feed pipes 62. The output end of the mixer 61 is connected to the input end of the condensation tower 1, and both feed pipes 62 are connected to the input end of the mixer 61.
[0040] When the raw materials are fed into the condensation tower 1, the ketone or aldehyde enters the mixer 61 from one feed pipe 62, and the diol enters the mixer 61 from another feed pipe 62. After the diol and ketone or aldehyde are fully mixed in the mixer 61, they are finally sent into the condensation tower 1 to ensure that the condensation reaction can be fully carried out in the condensation tower 1.
[0041] Furthermore, a first heater 7 is provided between the pretreatment structure 6 and the condensation tower 1, or a first heater 7 is provided on the pretreatment structure 6. The first heater 7 heats the raw material to 100-150°C, so that the raw material has a high temperature before entering the condensation tower 1, so that the condensation reaction can proceed fully.
[0042] In one specific embodiment, the first heater 7 is disposed between the pretreatment structure 6 and the condensation tower 1. Specifically, the pretreatment structure 6 and the condensation tower 1 are connected by a pipe, and the first heater 7 is installed on the corresponding pipe. When the raw material is fed from the pretreatment structure 6 into the condensation tower 1, the raw material is fully heated.
[0043] Furthermore, in another specific embodiment, the first heater 7 is disposed on the pretreatment structure 6. The first heater 7 can be disposed on the feed pipe 62 or in the mixer 61. The raw materials are fully heated before or during mixing.
[0044] This means that the raw materials can be heated before mixing, heated and mixed simultaneously, or mixed before heating.
[0045] In addition, the molar ratio of ketone or aldehyde to diol is set to 1:2 to 5 to ensure that the ketone or aldehyde can react more completely and be converted into diol ketal or acetal. The diol that did not participate in the condensation reaction is mixed with the product and discharged from the condensation tower 1 to the oil-water separator 2 in the form of a mixture.
[0046] The oil-water separator 2 can separate the mixture into an oil phase and a water phase. The oil phase is a diol ketal or acetal, and the water phase is water and a diol (the diol is easily soluble in water). Correspondingly, the oil-water separator 2 has a first outlet 21 for outputting the water phase, a fourth outlet 22 for outputting the oil phase, and a fifth outlet 23.
[0047] In one specific embodiment, a portion of the diol ketal or acetal is collected from the fourth outlet 22, and the fifth outlet 23 is connected to the input end of the condensation tower 1. The remaining portion of the diol ketal or acetal re-enters the condensation tower 1 from the fifth outlet 23.
[0048] Furthermore, referring to Figure 1 The distillation column 3 includes a rectification section and a stripping section arranged sequentially from bottom to top. The rectification section is equipped with 8 to 10 trays, and the stripping section is equipped with 3 to 5 trays. The rectification section is connected to the first outlet 21 of the oil-water separator 2 through a pipeline, and a second heater 8 is installed on the pipeline.
[0049] Before the aqueous phase enters the distillation column 3, it is preheated and then distilled to accelerate the distillation separation process. After the action of the stripping section and the rectification section in sequence, the heavier component (diol) is collected at the bottom of the column, and the lighter component (water) evaporates out of the distillation column 3.
[0050] After distillation separation in distillation column 3, the resulting diol has a purity greater than 99.9%.
[0051] Correspondingly, the distillation column 3 has a second outlet 31 for discharging diols and a third outlet 32 for discharging water; the third outlet 32 is connected to the output end of the condensation column 1. The diols obtained by distillation and purification enter the feed pipe 62 through the second outlet 31, and after heating, they are mixed with ketones or aldehydes and further undergo a condensation reaction in the condensation column 1.
[0052] Furthermore, the third discharge port 32 is connected to a cooling recovery structure 4, which includes a heat exchanger 41 and a transfer tank 42 connected in sequence. After the steam evaporates, it enters the heat exchanger 41 and is stored in the transfer tank 42 in the form of liquid water for further processing and discharge.
[0053] Furthermore, the transfer tank 42 is connected to a vacuum system 5, which can provide a vacuum environment for the distillation column 3 and the cooling recovery structure 4. That is, the distillation process and the condensation process are carried out in a vacuum environment, with the vacuum degree set to -0.095 to -0.08, so that the distillation process can be carried out more stably and efficiently.
[0054] The embodiments described in this specific implementation are preferred embodiments of this application and are not intended to limit the scope of protection of this application. Identical components are represented by the same reference numerals. Therefore, all equivalent changes made to the structure, shape, and principle of this application should be included within the scope of protection of this application.
Claims
1. A continuous high efficiency reaction apparatus for diol ketals or acetals, characterized by, include: A condensation tower (1) is filled with a catalyst; An oil-water separator (2) is connected to the output end of the condensation tower (1) and is used to receive and separate products to form an oil phase and a water phase. The oil-water separator (2) has a first outlet (21) for outputting the water phase. The distillation column (3) is connected to the first outlet (21) of the oil-water separator (2) for receiving and separating the aqueous phase to form diol and water. The distillation column (3) has a second outlet (31) for outputting diol and a third outlet (32) for outputting water. The third discharge port (32) is connected to the output end of the condensation tower (1) and is used to replenish the raw materials to the condensation tower (1).
2. The reaction apparatus according to claim 1, wherein The third discharge port (32) is connected to a cooling recovery structure (4), which includes a heat exchanger (41) and a transfer tank (42) connected in sequence.
3. The reaction apparatus of claim 2, wherein The transfer tank (42) is connected to a vacuum system (5) to provide a vacuum environment for the distillation column (3).
4. The reaction apparatus of claim 1, wherein The input end of the condensation tower (1) is provided with a pretreatment structure (6), the pretreatment structure (6) including: The mixer (61) has its output connected to the input of the condensation tower (1); A pair of feed pipes (62) are connected to the input end of the mixer (61).
5. The reaction apparatus of claim 4, wherein A first heater (7) is provided between the pretreatment structure (6) and the condensation tower (1); or The pretreatment structure (6) is provided with a first heater (7) for heating the raw materials.
6. The reaction apparatus of claim 4, wherein The oil-water separator (2) has a fourth outlet (22) and a fifth outlet (23) for outputting the oil phase, and the fourth outlet (22) or the fifth outlet (23) is connected to the input end of the mixer (61).
7. The reaction apparatus of claim 1, wherein The distillation column (3) includes a rectification section and a stripping section arranged sequentially from bottom to top. The rectification section is provided with 8 to 10 trays, and the stripping section is provided with 3 to 5 trays.
8. The reaction apparatus of claim 7, wherein The distillation section is connected to the first discharge port (21) via a pipeline, and a second heater (8) is provided on the pipeline.
9. The reactor of any of claims 1-8, wherein, The catalyst is at least one of A-15 resin or 732 resin.