Alkaline hydrolysis device for fluoromalonate

Abstract

The invention discloses a fluoromalonate alkaline hydrolysis device which comprises a feeding mechanism, a hydrolysis reaction mechanism and an alcohol recovery mechanism. The alcohol recovery mechanism comprises an alcohol recovery tank, an alcohol discharge pipe, an alcohol discharge control valve, a condenser, a vacuum pipeline and a pipeline control valve. The hydrolysis reaction mechanism comprises a hydrolysis reaction kettle, a heat exchange coil pipe, a kettle discharge pipe connected with the hydrolysis reaction kettle, a kettle discharge control valve arranged on the kettle discharge pipe and a kettle feed pipe for entering the hydrolysis reaction kettle along the kettle discharge pipe; a gas phase pipe is connected between the hydrolysis reaction kettle and the alcohol recovery tank; the heat exchange coil pipe comprises a spiral pipe body located in the hydrolysis reaction kettle, an inlet end connected with one tail end of the spiral pipe body and an outlet end connected with the other tail end of the spiral pipe body, the outlet end and the inlet end are both assembled on the hydrolysis reaction kettle, and the kettle feeding pipe is located beside the spiral pipe body. The fluoromalonate alkaline hydrolysis device provided by the invention can improve the fluoromalonate preparation efficiency and the alcohol recovery efficiency and purity.

Description

Technical Field

[0001] The present invention relates to the field of chemical equipment, in particular to an alkaline hydrolysis device for fluoromalonate. Background Art

[0002] As is well known, the reverse reaction of esterification is the hydrolysis of carboxylic acid esters into the corresponding carboxylic acids and alcohols. Carboxylic acid esters are commonly used in the chemical industry as solvents or plasticizers, or are produced as by-products or main products in a variety of reactions. Because carboxylic acid esters are low-value solvents, they can be hydrolyzed into the corresponding carboxylic acids and alcohols through a hydrolysis reaction followed by conventional separation procedures (such as distillation and crystallization), both of which have higher value.

[0003] Ester hydrolysis is typically carried out in a homogeneous medium using either an acid or base catalyst. Using bases as catalysts has the disadvantage of potentially forming metal salts, while using acids as catalysts, due to the low miscibility of water and carboxylic acid esters, results in a water-oil two-phase reaction, often requiring the use of a mixed solvent. This significantly complicates the subsequent separation and purification of the resulting carboxylic acid. Furthermore, liquid acids can cause significant equipment corrosion, incomplete reactions, or prolonged reaction times.

[0004] Fluoromalic acid is an important fluorine-containing organic compound. Firstly, it is a key intermediate in the synthesis of various pharmaceuticals, used in the preparation of nonsteroidal anti-inflammatory drugs, antiviral drugs, antitumor drugs, and antidepressants, and participates in the synthesis of anesthetics, analgesics, and drugs for the treatment of cardiovascular diseases. Secondly, in the industrial and materials fields, it is mainly used to synthesize high-performance fluorine-containing materials, prepare high-performance polymers such as polyurethane and polyester, and synthesize fuel cell proton exchange membranes, high-temperature resistant fibers, composite materials, and adhesives. In the electroplating industry, it is used as a polishing agent or aluminum surface treatment agent.

[0005] Currently, to obtain fluoromalonic acid, one must first obtain fluoromalonate, which is obtained by alkaline hydrolysis of fluoromalonic ester.

[0006] However, existing equipment for hydrolyzing fluoromalonates has the disadvantages of low efficiency in preparing fluoromalonates and low recovery efficiency and purity of hydrolysis alcohol.

[0007] Therefore, there is an urgent need for an alkaline hydrolysis device for fluoromalonate that improves the efficiency of preparing fluoromalonate and the recovery efficiency and purity of alcohol. Summary of the Invention

[0008] The object of the present invention is to provide a fluoromalonate alkaline hydrolysis device which improves the efficiency of preparing fluoromalonate and the recovery efficiency and purity of alcohol.

[0009] To achieve the above-mentioned objectives, the alkaline hydrolysis apparatus for fluoromalonate of the present invention comprises a feeding mechanism, a hydrolysis reaction mechanism for hydrolyzing the raw materials fed by the feeding mechanism, and an alcohol recovery mechanism for recovering alcohol from the hydrolysis reaction mechanism. The alcohol recovery mechanism comprises an alcohol recovery tank, an alcohol discharge pipe connected to the alcohol recovery tank, an alcohol discharge control valve disposed on the alcohol discharge pipe, a condenser mounted on the gas phase pipe, a vacuum pipeline connected to the alcohol recovery tank, and a pipeline control valve disposed on the vacuum pipeline. The hydrolysis reaction mechanism includes a hydrolysis reactor, a heat exchange coil, a reactor discharge pipe connected to the hydrolysis reactor, a reactor discharge control valve provided on the reactor discharge pipe, and a reactor feed pipe for the raw materials added by the feeding mechanism to enter the hydrolysis reactor. The gas phase pipe is connected between the hydrolysis reactor and the alcohol recovery tank. The heat exchange coil includes a spiral tube body located in the hydrolysis reactor and spirally extending in the height direction of the hydrolysis reactor, an inlet end connected to one end of the spiral tube body, and an outlet end connected to the other end of the spiral tube body. The outlet end and the inlet end are both assembled on the hydrolysis reactor; the reactor feed pipe is located on the side of the spiral tube body.

[0010] Compared with the prior art, the heat exchange coil of the hydrolysis reaction mechanism and the condenser and vacuum pipeline of the alcohol recovery mechanism are coordinated to change the vacuum degree in the hydrolysis reactor through the vacuum pipeline, thereby correspondingly reducing the boiling point of the liquid in the hydrolysis reactor. On the one hand, the hydrolysis reaction speed is effectively increased and the reaction time is shortened, thereby improving the efficiency of preparing fluoromalonate, and on the other hand, the recovery efficiency and purity of the alcohol are improved.

[0011] Preferably, the alkaline hydrolysis device for fluoromalonate of the present invention further comprises a nitrogen delivery pipe and a delivery pipe control valve provided on the nitrogen delivery pipe, and the kettle feed pipe is located outside the hydrolysis reactor and is connected to the nitrogen delivery pipe and the feeding mechanism respectively.

[0012] Preferably, the feeding mechanism comprises a fluoromalonate raw material tank with a fluoromalonate feed pipe and a first control valve, a pure water tank with a pure water feed pipe and a second control valve, and an alkali liquid tank with an alkali liquid feed pipe and a third control valve. The kettle feed pipe is located outside the hydrolysis reactor and is connected to the fluoromalonate feed pipe, the pure water feed pipe and the alkali liquid feed pipe, respectively. The first control valve is provided on the fluoromalonate feed pipe, the second control valve is provided on the pure water feed pipe, and the third control valve is provided on the alkali liquid feed pipe.

[0013] Preferably, the nitrogen delivery pipe is also connected to the top of the fluoromalonate raw material tank, the fluoromalonate feed pipe is connected to the bottom of the fluoromalonate raw material tank, the pure water feed pipe is connected to the bottom of the pure water tank, and the alkali solution feed pipe is connected to the bottom of the alkali solution tank.

[0014] Preferably, the connection points of the kettle feed pipe with the fluoromalonate feed pipe, the pure water feed pipe and the alkali solution feed pipe are arranged in sequence along the feeding direction of the kettle feed pipe.

[0015] Preferably, the hydrolysis reaction mechanism also includes a stirring motor installed on the top of the hydrolysis reactor and a stirring paddle located inside the hydrolysis reactor, the stirring paddle includes a rod body passing through the space surrounded by the spiral tube body and a blade located directly below the spiral tube body, and the rod body is connected to the stirring motor.

[0016] Preferably, the kettle feed pipe passes through the hydrolysis reactor from the top of the hydrolysis reactor, the end of the kettle feed pipe located in the hydrolysis reactor is suspended, and the end of the kettle feed pipe located in the hydrolysis reactor is also adjacent to the bottom of the hydrolysis reactor.

[0017] Preferably, the hydrolysis reaction mechanism further comprises a thermal insulation jacket, which is externally mounted on the side and bottom of the hydrolysis reactor, and the reactor feed pipe is connected to the bottom of the hydrolysis reactor while being surrounded by the thermal insulation jacket.

[0018] Preferably, the gas phase pipe is connected to the top of the hydrolysis reactor and the alcohol recovery tank respectively, and the vacuum pipe is connected to the top of the alcohol recovery tank.

[0019] Preferably, the outlet and inlet are both located on the side of the hydrolysis reactor. BRIEF DESCRIPTION OF THE DRAWINGS

[0020] Figure 1 It is a plan view of the alkaline hydrolysis apparatus for fluoromalonate of the present invention.

[0021] Figure 2 It is a plan view of the feeding mechanism and nitrogen delivery pipe assembled together in the alkaline hydrolysis device for fluoromalonate of the present invention.

[0022] Figure 3 It is a plan view of the hydrolysis reaction mechanism in the alkaline hydrolysis apparatus for fluoromalonate of the present invention.

[0023] Figure 4 It is a plan view of the alcohol recovery mechanism in the alkaline hydrolysis device for fluoromalonate of the present invention. DETAILED DESCRIPTION

[0024] In order to explain the technical content and structural features of the present invention in detail, the following is a further description in conjunction with the embodiments and the accompanying drawings.

[0025] See also Figures 1 to 4 The alkaline hydrolysis device 100 of the fluoromalonate of the present invention includes a feeding mechanism 10, a hydrolysis reaction mechanism 20 for hydrolyzing the raw materials added by the feeding mechanism 10, and an alcohol recovery mechanism 30 for recovering alcohol in the hydrolysis reaction mechanism 20.

[0026] The alcohol recovery mechanism 30 includes an alcohol recovery tank 31, an alcohol discharge pipe 32 connected to the alcohol recovery tank 31, an alcohol discharge control valve 33 provided on the alcohol discharge pipe 32, a condenser 34 mounted on the gas phase pipe 40, a vacuum pipe 35 connected to the alcohol recovery tank 31, and a pipe control valve 36 provided on the vacuum pipe 35. Figure 1 and Figure 4 As an example, the vacuum pipe 35 is connected to the top 311 of the alcohol recovery tank 31. Obviously, according to actual needs, the vacuum pipe 35 can also be connected to other positions of the alcohol recovery tank 31. Figure 1 and Figure 4 in addition, the alcohol discharge control valve 33 and the pipeline control valve 36 may be selected as a manual valve or an electrically controlled valve, and the electrically controlled valve is such as but not limited to the solenoid valve.

[0027] Meanwhile, the hydrolysis reaction mechanism 20 comprises a hydrolysis reactor 21, a reactor discharge pipe 22 connected to the hydrolysis reactor 21, a reactor discharge control valve 23 provided on the reactor discharge pipe 22, a reactor feed pipe 24 for feeding the raw materials added by the feeding mechanism 10 into the hydrolysis reactor 21, and a heat exchange coil 25 for heat exchange. The heat exchange coil 25 comprises a heat exchange coil 25 located in the hydrolysis reactor 21 and in the height direction of the hydrolysis reactor 21 (see FIG. 2 ). Figure 1 The spiral tube body 251 spirally extends in the vertical direction, the inlet end 252 connected to one end of the spiral tube body 251 and the outlet end 253 connected to the other end of the spiral tube body 251, the outlet end 253 and the inlet end 252 are both assembled on the hydrolysis reactor 21, and optionally, Figure 1 and Figure 3 As an example, the outlet end 253 and the inlet end 252 are both located on the side 213 of the hydrolysis reactor 21. This design makes it easier for the insulation jacket 28 described below to be placed on the bottom 212 and the side 213 of the hydrolysis reactor 21. In addition, the outlet end 253 is also arranged on the opposite side of the inlet end 252. For example, Figure 1 and Figure 3 In the embodiment, the outlet end 253 is located on the right side of the side portion 213 of the hydrolysis reactor 21, and the inlet end 252 is located on the left side of the side portion 213 of the hydrolysis reactor 21, but not in the Figure 1 and Figure 3Limits shown.

[0028] Furthermore, the kettle feed pipe 24 is located beside the spiral tube body 271. Figure 1 and Figure 3 As an example, the kettle feed pipe 24 passes through the hydrolysis reactor 21 from the top 211 of the hydrolysis reactor 21, which makes it easier to connect the feeding mechanism 10 with the kettle feed pipe 24. The end 244 of the kettle feed pipe 24 located in the hydrolysis reactor 21 is suspended, and the end 244 of the kettle feed pipe 24 located in the hydrolysis reactor 21 is also adjacent to the bottom 212 of the hydrolysis reactor 21. The purpose of this design is to allow the raw materials added by the feeding mechanism 10 and entering through the kettle feed pipe 24 to be directly fed into the bottom 212 of the hydrolysis reactor 21. The gas phase pipe 40 is connected between the hydrolysis reactor 21 and the alcohol recovery tank 31. Optionally, Figure 1 and Figure 4 As an example, the gas phase pipe 40 is connected to the top 211 of the hydrolysis reactor 21 and the top 311 of the alcohol recovery tank 31, respectively, to ensure that the gas of the hydrolysis reaction in the hydrolysis reactor 21 is transported to the alcohol recovery tank 31 more promptly, and the gas is converted into liquid by the condenser 34 and falls into the alcohol recovery tank 31; Obviously, according to actual needs, the gas phase pipe 40 can also be connected to other positions of the hydrolysis reactor 21 and the alcohol recovery tank 31, respectively, so it is not used as shown in FIG. Figure 1 and Figure 4 More details are given below.

[0029] like Figure 1 and Figure 2 As shown, as an example, the alkaline hydrolysis device 100 of fluoromalonate of the present invention further includes a nitrogen delivery pipe 50 and a delivery pipe control valve 60 provided on the nitrogen delivery pipe 40. At this time, the kettle feed pipe 24 is located at a position 24a outside the hydrolysis reactor 21 and is connected to the nitrogen delivery pipe 50 and the feeding mechanism 10 respectively; the nitrogen delivery pipe 50 and the delivery pipe control valve 60 are used to deliver nitrogen, and the nitrogen is used to protect the organic material from being oxidized; specifically, as an example, the nitrogen delivered by the nitrogen delivery pipe 50 is high-purity nitrogen, and the delivery pipe control valve 60 can be selected as a manual valve or an electric control valve, and the electric control valve is, for example, but not limited to, a solenoid valve.

[0030] Another example Figures 1 to 2As shown, as an example, the feeding mechanism 10 includes a fluoromalonate raw material tank 11 with a fluoromalonate feed pipe 111 and a first control valve 112, a pure water tank 12 with a pure water feed pipe 121 and a second control valve 122, and an alkali liquid tank 13 with an alkali liquid feed pipe 131 and a third control valve 132. At this time, the position 24a of the kettle feed pipe 24 located outside the hydrolysis reactor 21 is connected to the fluoromalonate feed pipe 111, the pure water feed pipe 121 and the alkali solution feed pipe 131 respectively, so as to obtain the connection 241 between the kettle feed pipe 24 and the fluoromalonate feed pipe 111, the connection 242 between the kettle feed pipe 24 and the pure water feed pipe 121, and the connection 243 between the kettle feed pipe 24 and the alkali solution feed pipe 131. Optionally, as an example, the connection 241, the connection 242 and the connection 243 are along the feeding direction of the kettle feed pipe 24 (see Figure 1 (from top to bottom in the middle) are arranged in sequence, and the status is shown in Figure 1 and Figure 2 Obviously, according to actual needs, the connection 241, the connection 242 and the connection 243 can also be in other order relationships, so it is not necessary to Figure 1 and Figure 2 Limits shown. In addition, a first control valve 112 is provided on the fluoromalonate feed pipe 111 to allow the fluoromalonate raw material in the fluoromalonate raw material tank 11 to be transported to the kettle feed pipe 24 when the first control valve 112 is opened, and to block the fluoromalonate raw material in the fluoromalonate raw material tank 11 from being transported to the kettle feed pipe 24 when the first control valve 112 is closed; a second control valve 122 is provided on the pure water feed pipe 121 to allow the pure water in the pure water tank 12 to be transported to the kettle feed pipe 24 when the second control valve 122 is opened, and to block the pure water in the pure water tank 12 from being transported to the kettle feed pipe 24 when the second control valve 122 is closed; a third control valve 132 is provided on the alkali liquid feed pipe 131 to allow the alkali liquid raw material in the alkali liquid tank 13 to be transported to the kettle feed pipe 24 when the third control valve 132 is opened, and to block the alkali liquid raw material in the alkali liquid tank 13 from being transported to the kettle feed pipe 24 when the third control valve 132 is closed. Specifically, Figure 1 and Figure 2In the embodiment, as an example, the nitrogen delivery pipe 50 is also connected to the top 11a of the fluoromalonate raw material tank 11, so that the nitrogen delivery pipe 50 can deliver nitrogen to the fluoromalonate raw material tank 11, thereby better preventing the oxidation of the fluoromalonate raw material in the fluoromalonate raw material tank 11; in addition, the fluoromalonate feed pipe 111 is connected to the bottom 11a of the fluoromalonate raw material tank 11, the pure water feed pipe 121 is connected to the bottom 123 of the pure water tank 12, and the alkali liquid feed pipe 131 is connected to the bottom 133 of the alkali liquid tank 13, so as to improve the timeliness of the response of the raw materials in them to the kettle feed pipe 24. Among them, the kettle feed pipe 24 is connected to the fluoromalonate feed pipe 111, the pure water feed pipe 121, the alkali solution feed pipe 131 and the nitrogen delivery pipe 50 at a position 24a outside the hydrolysis reactor 21, respectively, so that the fluoromalonate raw material, pure water, alkali solution and nitrogen gas uniformly enter the bottom 212 of the hydrolysis reactor 21, and the high-purity nitrogen gas delivered by the nitrogen delivery pipe 50 purges the materials remaining in the kettle feed pipe 24, thereby improving the measurement accuracy. In addition, a kettle feed control valve 29 can be installed at the position 24a of the kettle feed pipe 24 outside the hydrolysis reactor 21, so that the fluoromalonate raw material, pure water, alkali solution and nitrogen gas are allowed to uniformly enter the hydrolysis reactor 21 along the kettle feed pipe 24 only after the kettle feed control valve 29 is opened. It should be noted that the first control valve 112 , the second control valve 122 and the third control valve 132 can be manual valves or electrically controlled valves, and the electrically controlled valves are, for example but not limited to, electromagnetically controlled valves.

[0031] like Figure 1 and Figure 3 As shown, as an example, the hydrolysis reaction mechanism 20 further includes a stirring motor 26 mounted on the top 211 of the hydrolysis reactor 21 and a stirring paddle 27 located within the hydrolysis reactor 21. The stirring paddle 27 includes a rod 271 extending through the space enclosed by the spiral tube 251 and a paddle 272 located directly below the spiral tube 251. The rod 271 is connected to the stirring motor 26. Therefore, with the cooperation of the heat exchange coil 25, the stirring effect is enhanced, thereby further shortening the hydrolysis reaction time. In addition, the hydrolysis reaction mechanism 20 further includes a heat preservation jacket 28, which is externally mounted on the side 213 and bottom 212 of the hydrolysis reactor 21. The kettle feed pipe 24 is connected to the bottom 212 of the hydrolysis reactor 21 so as to be surrounded by the heat preservation jacket 28. With the help of the heat preservation jacket 28, the heat loss from the hydrolysis reactor 21 to the outside is effectively reduced.

[0032] Compared with the prior art, the heat exchange coil 25 of the hydrolysis reaction mechanism 20 and the condenser 34 and vacuum pipe 35 of the alcohol recovery mechanism 30 cooperate to change the vacuum degree in the hydrolysis reactor 21 through the vacuum pipe 35, thereby correspondingly lowering the boiling point of the liquid in the hydrolysis reactor 21. This effectively increases the hydrolysis reaction speed and shortens the reaction time, thereby improving the efficiency of preparing fluoromalonate, and also improves the recovery efficiency and purity of the alcohol.

[0033] The above disclosure is only a preferred embodiment of the present invention and cannot be used to limit the scope of the present invention. Therefore, equivalent changes made according to the claims of the present invention are all within the scope of the present invention.

Claims

1. A fluoromalonate alkaline hydrolysis device, comprising a feeding mechanism, a hydrolysis reaction mechanism for hydrolyzing a raw material added by the feeding mechanism, and an alcohol recovery mechanism for recovering alcohol in the hydrolysis reaction mechanism, wherein the alcohol recovery mechanism comprises an alcohol recovery tank, an alcohol discharge pipe connected to the alcohol recovery tank, and an alcohol discharge control valve provided on the alcohol discharge pipe; the hydrolysis reaction mechanism comprises a hydrolysis reactor, a reactor discharge pipe connected to the hydrolysis reactor, a reactor discharge control valve provided on the reactor discharge pipe, and a reactor feed pipe for the raw material added by the feeding mechanism to enter the hydrolysis reactor; a gas phase pipe is connected between the hydrolysis reactor and the alcohol recovery tank, characterized in that The hydrolysis reaction mechanism also includes a heat exchange coil, which includes a spiral tube body located in the hydrolysis reactor and spirally extending in the height direction of the hydrolysis reactor, an inlet end connected to one end of the spiral tube body, and an outlet end connected to the other end of the spiral tube body. The outlet end and the inlet end are both assembled on the hydrolysis reactor, and the reactor feed pipe is located on the side of the spiral tube body. The alcohol recovery mechanism also includes a condenser assembled on the gas phase pipe, a vacuum pipe connected to the alcohol recovery tank, and a pipeline control valve provided on the vacuum pipe.

2. The alkaline hydrolysis device for fluoromalonate according to claim 1, characterized in that: It also includes a nitrogen delivery pipe and a delivery pipe control valve arranged on the nitrogen delivery pipe. The kettle feed pipe is located outside the hydrolysis reactor and is connected to the nitrogen delivery pipe and the feeding mechanism respectively.

3. The alkaline hydrolysis device for fluoromalonate according to claim 2, characterized in that: The feeding mechanism includes a fluoromalonate raw material tank with a fluoromalonate feed pipe and a first control valve, a pure water tank with a pure water feed pipe and a second control valve, and an alkali liquid tank with an alkali liquid feed pipe and a third control valve. The kettle feed pipe is located outside the hydrolysis reactor and is connected to the fluoromalonate feed pipe, the pure water feed pipe and the alkali liquid feed pipe respectively. The first control valve is provided on the fluoromalonate feed pipe, the second control valve is provided on the pure water feed pipe, and the third control valve is provided on the alkali liquid feed pipe.

4. The alkaline hydrolysis device for fluoromalonate according to claim 3, characterized in that: The nitrogen delivery pipe is also connected to the top of the fluoromalonate raw material tank, the fluoromalonate feed pipe is connected to the bottom of the fluoromalonate raw material tank, the pure water feed pipe is connected to the bottom of the pure water tank, and the alkali solution feed pipe is connected to the bottom of the alkali solution tank.

5. The alkaline hydrolysis device for fluoromalonate according to claim 3, characterized in that: The connection points of the kettle feed pipe with the fluoromalonate feed pipe, the pure water feed pipe and the alkali solution feed pipe are arranged in sequence along the feeding direction of the kettle feed pipe.

6. The alkaline hydrolysis device for fluoromalonate according to claim 1, characterized in that: The hydrolysis reaction mechanism also includes a stirring motor installed on the top of the hydrolysis reactor and a stirring paddle located in the hydrolysis reactor. The stirring paddle includes a rod body passing through the space surrounded by the spiral tube body and a blade located directly below the spiral tube body. The rod body is connected to the stirring motor.

7. The alkaline hydrolysis device for fluoromalonate according to claim 1, characterized in that: The kettle feed pipe passes through the hydrolysis reactor from the top of the hydrolysis reactor, and the end of the kettle feed pipe located in the hydrolysis reactor is suspended, and the end of the kettle feed pipe located in the hydrolysis reactor is also adjacent to the bottom of the hydrolysis reactor.

8. The alkaline hydrolysis device for fluoromalonate according to claim 1, characterized in that: The hydrolysis reaction mechanism further comprises a heat-insulating jacket, which is externally mounted on the side and bottom of the hydrolysis reactor. The reactor feed pipe is connected to the bottom of the hydrolysis reactor while being surrounded by the heat-insulating jacket.

9. The alkaline hydrolysis device for fluoromalonate according to claim 1, characterized in that: The gas phase pipe is connected to the top of the hydrolysis reactor and the alcohol recovery tank respectively, and the vacuum pipeline is connected to the top of the alcohol recovery tank.

10. The alkaline hydrolysis device for fluoromalonate according to claim 1, characterized in that: The outlet port and the inlet port are both located on the side of the hydrolysis reactor.

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