Reaction purification device for oxazoline products
By designing a reaction purification device for oxazoline products, one-step drying is achieved using vacuum conditions and desiccant, the problem of difficulty in purifying oxazoline compounds is solved, and the product without water is obtained directly, which avoids hydrolysis and opening the ring, which is easy to operate and economical .
Patent Information
- Application Number
- CN202421485890.5
- Authority / Receiving Office
- CN · China
- Patent Type
- Utility models(China)
- Current Assignee / Owner
- Filing Date
- 2024-06-27
- Publication Date
- 2025-01-03
- Estimated Expiration
- 2034-06-27
AI Technical Summary
The prior art is difficult to effectively purify oxazoline compounds because they are hydrophilic compounds, which are easily miscible with water and hydrolyze the rings during distillation, resulting in difficulty in purification.
A reaction purification device for oxazoline products is designed, including a reactor, a distillation column, a condenser, a buffer drying tank and a receiving tank. It uses vacuum conditions and desiccant to achieve one-step drying, avoid hydrolysis of the ring and separate through the distillation column. Oxazoline and water, after condenser condenses, remove water in a buffer drying tank, and the microporous filter prevents the desiccant from entering.
It is possible to directly obtain oxazoline products without water in one step, avoiding the hydrolysis of ring opening, easy operation, economical and cheap reagents, and can control the purification and drying time of the product.
Smart Images
Figure CN222286417U_ABST
Abstract
Description
Technical Field
[0001] This utility model relates to the field of chemical production technology, specifically to a reaction purification device for oxazoline products. Background Technology
[0002] This invention targets an oxazoline product, a five-membered heterocyclic compound containing C, N, and O elements, comprising an oxazoline ring with an OC=N structure and 2-substituted side groups. The structural formula is as follows:
[0003]
[0004] The above structural formulas represent several 2-oxazoline compounds with alkyl side groups, namely methyloxazoline, ethyloxazoline, vinyloxazoline, isopropenyloxazoline, etc.
[0005] The side group usually determines the properties and application scenarios of oxazoline. When it is alkyl, it is usually used in biocompatible polymer materials, and when it is alkenyl, it is used for modification such as thickening and toughening of carboxyl-containing polymers.
[0006] In patents US4203900 and US5034536 published by Dow Chemical Company, a two-step process for preparing 2-oxazoline compounds is described, involving the reaction of an alkanolamine with a carboxylic acid ester followed by distillation. These oxazoline products are primarily obtained through a ring-closure reaction, and the main impurity in the crude oxazoline is water generated during the ring-closure reaction. Because these oxazolines are hydrophilic compounds, miscible with water, and readily undergo ring-opening hydrolysis during heating during distillation, the direct distillation method described in the aforementioned patents is not suitable for purifying the oxazoline products. Utility Model Content
[0007] To address the aforementioned technical problems, this invention provides a reaction purification device for oxazoline products, primarily applicable to the above-mentioned 2-oxazoline compounds with alkyl side groups, including liquid products such as methyloxazoline, ethyloxazoline, vinyloxazoline, and isopropenyloxazoline. It enables the purification of oxazoline products during the reaction process.
[0008] To achieve the above objectives, this utility model provides the following technical solution: a reaction purification device for oxazoline products, comprising a reaction vessel with a liquid inlet and a solid inlet, characterized in that: a distillation column is provided at the top of the reaction vessel, the bottom reflux port of the distillation column is inserted into a corresponding port on the reaction vessel, the top outlet of the distillation column is connected to a condenser, the condensate outlet pipeline of the condenser is connected to the top inlet pipeline of a buffer drying tank, a liquid outlet valve is provided at the bottom of the buffer drying tank and connected to a receiving tank, a microporous filter is provided at the bottom of the buffer drying tank, a desiccant is filled above the microporous filter, gas pipelines are provided at the top of both the buffer drying tank and the receiving tank, a first valve and a vacuum valve are provided on the gas pipeline of the buffer drying tank, a second valve and a vent valve are provided on the gas pipeline of the receiving tank, and the gas pipelines of the buffer drying tank and the receiving tank are connected by a connecting pipe, the two ends of the connecting pipe being located between the first valve and the vacuum valve and between the second valve and the vent valve, respectively.
[0009] In the above scheme, a stirring device is installed inside the reaction vessel. This helps to ensure a uniform reaction.
[0010] In the above scheme, a heating jacket is provided outside the reaction vessel for convenient heating.
[0011] In the above scheme: a pressure gauge is installed on the reaction vessel.
[0012] In the above scheme: a thermometer or temperature sensor is installed inside the reaction vessel.
[0013] In the above scheme: a feed hopper is provided on the solid feed inlet, and a feed valve is provided below the feed hopper; a feed valve is provided on the liquid feed inlet.
[0014] In the above scheme, the desiccant is at least one of water-absorbing resin, Na2SO4, MgSO4, and CaCl2.
[0015] After the reactants, high-boiling-point solvents, and catalysts are fed into the reactor through the liquid and solid feed ports, the vacuum valve is connected to the vacuum unit. The vent valve is closed, and the vacuum unit is turned on to adjust the system to a suitable vacuum level (to provide the vacuum conditions required for the reaction). After the system is appropriately heated, stirring is started to dissolve the solid materials, and then the temperature is gradually increased to the target temperature. At this point, the materials in the system begin to react. The crude oxazoline product is distilled out through a distillation column (the main components are oxazoline products and water produced in the reaction). In the distillation column, high-boiling-point substances (unreacted materials and high-boiling-point solvents) flow back into the reactor from the bottom reflux port, while the relatively low-boiling-point crude oxazoline product is condensed into liquid by a condenser and flows into a buffer drying tank for dehydration and drying. A microporous filter is used to prevent the desiccant from entering the receiver. When the distillate reaches a certain level, it is placed into the receiving tank for further drying of the subsequent fractions.
[0016] This invention offers the following advantages: It directly and in one step yields anhydrous oxazoline product during the reaction process, achieving semi-continuous drying of the crude product and obtaining purified oxazoline. This avoids the hydrolysis and ring-opening that can occur when the crude product is miscible with water during distillation. The drying reagent can be regenerated through high-temperature drying after use. The outflow rate of the crude product can be controlled by a vacuum valve, and the drying time can be controlled by a buffer drying tank. The entire system maintains a consistent pressure, ensuring product purification while maintaining the vacuum state of the system. The operation is simple and feasible, and the reagents are economical and inexpensive. Attached Figure Description
[0017] Figure 1 This is a schematic diagram of the structure of this utility model. Detailed Implementation
[0018] The present invention will be further described below with reference to the accompanying drawings and embodiments.
[0019] Example 1
[0020] like Figure 1 As shown: A reaction purification device for oxazoline products includes a reaction vessel 1, which is provided with a liquid inlet 3 and a solid inlet 14. A feed hopper is provided on the solid inlet 14, and a feed valve is provided below the feed hopper. A feed valve is also provided on the liquid inlet 3.
[0021] A stirring device 15 is installed inside the reactor 1. A heating jacket is installed outside the reactor 1. A pressure gauge 17 is installed on the reactor. A thermometer or temperature sensor 16 is installed inside the reactor 1. The liquid inside the reactor is the reaction raw material 2.
[0022] A distillation column 4 is installed at the top of the reactor 1. The reflux port at the bottom of the distillation column 4 is inserted into the corresponding port on the reactor. The outlet at the top of the distillation column 4 is connected to the condenser 5. The outer layer of the condenser 5 is a cooling water layer, with cooling water inlet and outlet pipes. The inner layer is through which the crude product passes. This is a conventional structure and will not be described in detail here. The condensate outlet pipe of the condenser 5 is connected to the top inlet pipe of the buffer drying tank 6. The bottom of the buffer drying tank 6 is equipped with a liquid outlet valve connected to the receiving tank 10. A microporous filter 9 is installed at the bottom of the buffer drying tank 6. A desiccant 8 is filled above the microporous filter 9, and the distilled crude oxazoline product 7 is above the desiccant 8. The desiccant is at least one of water-absorbing resin, Na2SO4, MgSO4, and CaCl2.
[0023] Both the buffer drying tank 6 and the receiving tank 10 are equipped with gas pipelines at their tops. The gas pipeline in the buffer drying tank is equipped with a first valve and a vacuum valve 13, with the vacuum valve 13 connected to a vacuum unit. The gas pipeline in the receiving tank 10 is equipped with a second valve and a vent valve 12. The gas pipelines of the buffer drying tank and the receiving tank are connected by a connecting pipe, with the two ends of the connecting pipe located between the first valve and the vacuum valve, and between the second valve and the vent valve, respectively. The liquid in the receiving tank 10 is oxazoline product 11.
[0024] Although embodiments of the present invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the present invention, the scope of which is defined by the appended claims and their equivalents.
Claims
1. A reaction purification device for an oxazoline product, comprising a reactor, wherein the reactor is provided with a liquid feed inlet and a solid feed inlet, wherein: A distillation column is arranged at the top of the reactor, and a reflux port at the bottom of the distillation column is plugged into a corresponding socket on the reactor. The column top outlet of the distillation column is connected to a condenser, and a condensate outlet pipeline of the condenser is connected to an inlet pipeline at the top of a buffer drying tank. A liquid outlet valve is arranged at the bottom of the buffer drying tank and is connected to a receiving tank. A microporous filter is arranged at the bottom of the buffer drying tank, and a desiccant is loaded above the microporous filter. Gas pipelines are arranged at the tops of the buffer drying tank and the receiving tank. A first valve and a vacuum valve are arranged on the gas pipeline of the buffer drying tank, and a second valve and a vent valve are arranged on the gas pipeline of the receiving tank. The gas pipelines of the buffer drying tank and the receiving tank are connected via a connecting pipe, and the connection points at both ends of the connecting pipe are respectively located between the first valve and the vacuum valve and between the second valve and the vent valve.
2. The reaction purification device of the oxazoline product according to claim 1, characterized in that: A stirring device is arranged in the reactor.
3. The reaction purification device of the oxazoline product according to claim 1 or 2, characterized in that: A heating jacket is arranged outside the reaction kettle.
4. The reaction purification device for oxazoline products according to claim 3, characterized in that: The reactor is provided with a pressure gauge.
5. The reaction purification device for oxazoline products according to claim 4, characterized in that: A thermometer or a temperature sensor is arranged in the reactor.
6. The reaction purification device for oxazoline products according to claim 5, characterized in that: A feed hopper is arranged on the solid feed port, a feed valve is arranged below the feed hopper, and a feed valve is arranged on the liquid feed port.