Organic amine hydrochloride recovery device

Abstract

The utility model relates to an organic amine hydrochloride recovery device, which includes a sealed reactor, and also includes a stirring assembly arranged in the reactor along the longitudinal direction, for uniformly mixing the organic amine salt hydrochloride aqueous solution, solid alkali and saturated sodium chloride aqueous solution sent into the reactor; an inert gas delivery pipe runs through the reactor along the longitudinal direction and is sealed and connected to the reactor, and the gas outlet of the inert gas delivery pipe is located above the liquid level in the reactor, for increasing the gas pressure in the reactor; the U-shaped infusion tube is an inverted U-shaped tube, including an input end and an output end, the input end is arranged below the organic amine sodium chloride aqueous solution liquid level boundary layer of the reactor, and the output end of the U-shaped infusion tube is located outside the reactor; a stratification tank is arranged outside the reactor, and is connected to the output end of the U-shaped infusion tube, for collecting the organic amine and saturated sodium chloride aqueous solution sent by the U-shaped infusion tube, so that it can be statically stratified in the stratification tank. The utility model improves the reaction efficiency.

Description

Technical Field

[0001] The utility model relates to the technical field of chemical process and engineering, in particular to an organic amine hydrochloride recovery device. Background Art

[0002] Organic amines are a class of organic compounds that contain nitrogen atoms connected to carbon atoms through carbon-nitrogen bonds and hydrogen atoms. Organic amines are widely used in chemistry and biology. They can be used as reactants, solvents, catalysts or intermediates to synthesize chemicals such as drugs, dyes, plastics, pesticides, etc. In biology, organic amines are also components of some diazo compounds in organisms, such as amino acids and bases. In the field of medicine, organic amine drugs include many important drugs, such as opioid analgesics, antihistamines, antidepressants, etc. Therefore, the research and application of organic amines are of great significance to the fields of medicinal chemistry and biology.

[0003] When organic amines participate in the reaction in the form of acid-binding agents (such as hydrochloric acid, sulfuric acid, etc.), corresponding salts, such as hydrochlorides or sulfates, are generated. Such salts may have different physicochemical properties, such as solubility, stability, etc., which may affect the reaction process or the properties of the product. Therefore, recovering free organic amines from organic amine salts not only saves costs by reusing them, but also helps to optimize chemical reactions and processing steps by adjusting physical and chemical properties, thereby improving the efficiency and feasibility of the overall synthesis.

[0004] The currently commonly used organic amine hydrochloride recovery device needs to add the aqueous solution of organic amine hydrochloride into the reactor, start the stirring component, and add alkali to the reactor under stirring when recovering organic amine. When the pH value in the reactor shows alkalinity, stop adding alkali, and then send the solution in the reactor to the distiller to distill out the organic amine. Since the distilled organic amine has a certain solubility in water or the organic amine is miscible with water, it cannot be sent to the extraction device for direct layer separation, and it needs to be sent to the distillation tower for distillation and water removal. Therefore, the existing organic amine hydrochloride recovery device is a system composed of multiple reaction devices. The neutralization and layer recovery of organic amine hydrochloride needs to be completed step by step through multiple reaction equipment, which leads to low reaction efficiency. Utility Model Content

[0005] The purpose of the utility model is to overcome the above problems existing in the prior art and to provide an organic amine hydrochloride recovery device, which can simultaneously complete the neutralization and stratification recovery of the organic amine hydrochloride, thereby improving the reaction efficiency.

[0006] The utility model provides an organic amine hydrochloride recovery device, comprising a reaction kettle, wherein the reaction kettle is a sealed reaction kettle, and further comprises:

[0007] A stirring assembly is disposed in the reactor in the longitudinal direction and is used to uniformly mix the organic ammonium salt hydrochloride aqueous solution, the solid alkali and the saturated sodium chloride aqueous solution fed into the reactor;

[0008] An inert gas delivery pipe runs through the reactor in the longitudinal direction and is sealed with the reactor, wherein the gas outlet of the inert gas delivery pipe is located above the liquid level in the reactor and is used to increase the gas pressure in the reactor;

[0009] The U-shaped infusion tube is an inverted U-shaped tube, including an input end and an output end, wherein the input end is arranged below the interface layer of the organic amine-sodium chloride aqueous solution in the reactor, and the output end of the U-shaped infusion tube is located outside the reactor;

[0010] The stratification tank is arranged outside the reactor and is connected with the output end of the U-shaped infusion tube. It is used to collect the organic amine and saturated sodium chloride aqueous solution sent out by the U-shaped infusion tube and make them stand and stratify in the stratification tank.

[0011] Preferably, the output end of the U-shaped infusion tube in the stratified tank is arranged close to the inner wall of the stratified tank.

[0012] Preferably, a guide plate is obliquely provided on the output end of the U-shaped infusion tube, the high end of the guide plate is fixedly connected to the output end of the U-shaped infusion tube, and a gap is reserved between the low end of the guide plate and the inner wall of the stratified tank.

[0013] Preferably, the input end of the U-shaped infusion tube is located 9 to 11 cm below the interface layer of the organic amine-sodium chloride aqueous solution.

[0014] Preferably, a pH meter for detecting the pH value of the liquid is provided in the reactor, a controller is provided on the reactor, and the pH meter is electrically connected to the controller.

[0015] Preferably, the bottom wall of the stratification tank is a conical structure, and a discharge pipe is provided at the bottom of the stratification tank.

[0016] Preferably, a sight glass observation window is provided on the side wall close to the bottom wall of the reactor.

[0017] Preferably, a liquid return pipe is provided at the bottom of the reactor to form a closed loop with the top of the reactor, and a lifting pump is provided on the liquid return pipe, and the lifting pump is connected to the second delivery port.

[0018] Preferably, a heating element is provided in the reactor, and a first inlet, a second inlet and a third inlet are provided on the reactor, the first inlet is used for feeding a solid base for freeing the organic amine from the organic amine hydrochloride aqueous solution, the second inlet is used for feeding a saturated sodium chloride aqueous solution for stratifying the organic amine and water, the third inlet is used for feeding an organic amine salt hydrochloride aqueous solution, and the first inlet, the second inlet and the third inlet are all provided with sealing covers.

[0019] Preferably, the inert gas delivery pipe, the U-shaped liquid delivery pipe and the discharge pipe are all provided with valves.

[0020] Compared with the prior art, the beneficial effects of the utility model are:

[0021] The utility model provides a reaction device of an organic amine hydrochloride recovery device, which avoids using multiple reactors to separate the organic amine in multiple steps, thereby improving the reaction rate.

[0022] The specific operation of the utility model is as follows: the utility model adds solid alkali into the reaction kettle, and under the disturbance of the stirring component, the organic amine aqueous solution in the organic amine salt hydrochloride aqueous solution will be freed and inorganic salt will be precipitated. At this time, a saturated sodium chloride aqueous solution is added to the organic amine solution. At this time, the precipitated inorganic salt and the saturated sodium chloride aqueous solution are fully mixed and contacted with the organic amine solution under the disturbance of the stirring component. Since the density of the saturated sodium chloride aqueous solution is further increased after the inorganic salt is precipitated, the density difference between the organic amine and the salt solution becomes larger, so that stratification occurs in the reaction kettle. In this process, it is not necessary to send the solution generated by the solid base and the organic amine salt hydrochloride aqueous solution into the distiller for distillation and rectification, so as to achieve the extraction and stratification of the organic amine. Instead, the inert gas is introduced into the reactor through the inert gas delivery pipe, which increases the pressure above the liquid surface in the reactor, so that the organic amine and a small amount of sodium chloride aqueous solution located at the interface layer of the organic amine-sodium chloride aqueous solution can be sent from the input end of the U-shaped infusion tube into the stratification tank connected to the output end of the U-shaped infusion tube for further stratification. The stratification does not require multiple reaction devices to be completed in multiple steps, thereby improving the stratification efficiency. BRIEF DESCRIPTION OF THE DRAWINGS

[0023] Figure 1 It is a schematic diagram of an organic amine hydrochloride recovery device I of the utility model;

[0024] Figure 2 It is a schematic diagram of an organic amine hydrochloride recovery device II of the utility model.

[0025] Description of reference numerals:

[0026] 1. Reactor, 2. Inert gas delivery pipe, 3. Stratification tank, 4. U-shaped infusion tube, 5. Stirring assembly, 6. Discharge pipe, 7. Sight glass observation window. DETAILED DESCRIPTION

[0027] The following is combined with Figure 1-2, the specific implementation of the utility model is described in detail, but it should be understood that the protection scope of the utility model is not limited by the specific implementation. Based on the embodiments of the utility model, all other embodiments obtained by ordinary technicians in this field without making creative work are within the scope of protection of the utility model.

[0028] The inventors have found that the existing organic amine hydrochloride recovery process is to neutralize, then distill and rectify, which has complicated steps and high energy consumption.

[0029] In order to solve the problems existing in the above-mentioned prior art, the utility model provides an organic amine hydrochloride recovery device.

[0030] Refer to the attached Figure 1-2 As shown, in the embodiment, an organic amine hydrochloride recovery device includes a reactor 1, which is a sealed reactor, and also includes: a stirring component 5, an inert gas delivery pipe 2, a U-shaped infusion pipe 4 and a stratification tank 3, wherein the stirring component 5 is arranged in the reactor 1 along the longitudinal direction and is driven by a motor to mix the organic amine salt hydrochloride aqueous solution, solid alkali and saturated sodium chloride aqueous solution fed into the reactor 1; the inert gas delivery pipe 2 penetrates the reactor 1 along the longitudinal direction and is sealed with the reactor 1, and the gas outlet of the inert gas delivery pipe 2 is located in the liquid in the reactor 1. The U-shaped infusion tube 4 is an inverted U-shaped tube, which includes an input end and an output end. The input end is arranged below the liquid level boundary layer of the organic amine-sodium chloride aqueous solution in the reactor 1, and the output end of the U-shaped infusion tube 4 is located outside the reactor 1, which is used to send the liquid in the reactor 1 out of the reactor 1 under the action of external pressure; the stratification tank 3 is arranged outside the reactor 1 and is connected with the output end of the U-shaped infusion tube 4, which is used to collect the organic amine and the saturated sodium chloride aqueous solution sent by the U-shaped infusion tube 4, so that they are statically stratified in the stratification tank 3.

[0031] The stirring assembly 5 includes a rotating shaft and a plurality of stirring blades, wherein the rotating shaft is longitudinally arranged in the reactor 1, the plurality of stirring blades are evenly spaced on the rotating shaft along the axial length direction of the rotating shaft, and the top end of the rotating shaft is connected to the motor.

[0032] Working principle:

[0033] When it is necessary to separate the organic ammonium salt hydrochloride aqueous solution, solid alkali needs to be added into the reactor 1. Under the disturbance of the stirring component 5, the organic amine aqueous solution in the organic amine salt hydrochloride aqueous solution will be freed and inorganic salt will precipitate. At this time, a saturated sodium chloride aqueous solution is added to the organic amine solution. At this time, the precipitated inorganic salt and the saturated sodium chloride aqueous solution are fully mixed and contacted with the organic amine solution under the disturbance of the stirring component 5. Since the density of the saturated sodium chloride aqueous solution is further increased after the inorganic salt is precipitated, the density difference between the organic amine and the salt solution becomes larger, so that stratification occurs in the reactor 1. In this process, it is not necessary to send the solution generated by the solid base and the organic amine salt hydrochloride aqueous solution into the distiller for distillation and then rectification, so that the extraction and stratification of the organic amine can be achieved. Instead, the inert gas is introduced into the reactor 1 through the inert gas delivery pipe, which increases the pressure above the liquid surface in the reactor, so that the organic amine and a small amount of sodium chloride aqueous solution located at the organic amine-sodium chloride aqueous solution liquid surface boundary layer can be sent from the U-shaped infusion tube input 4 end into the stratification tank 3 connected to the U-shaped infusion tube 4 output end for further stratification. The stratification does not require multiple reaction devices to be completed in multiple steps, thereby improving the stratification efficiency.

[0034] Specifically, the output end of the U-shaped infusion tube 4 in the stratified tank 3 is arranged close to the inner wall of the stratified tank 3 to avoid disturbance of the liquid sent into the stratified tank 3 .

[0035] Specifically, in order to further avoid the disturbance of the stratified liquid surface caused by the liquid delivered from the output end of the U-shaped infusion tube 4, a guide plate is obliquely provided on the output end of the U-shaped infusion tube 4, and the high end of the guide plate is fixedly connected to the output end of the U-shaped infusion tube 4. A gap is reserved between the low end of the guide plate and the inner wall of the stratified tank 3, and the width of the gap is 1-3mm, which helps the liquid falling from the guide plate to form a liquid film layer in the gap, thereby reducing the disturbance of the falling liquid on the liquid in the stratified tank 3.

[0036] Specifically, the input end of the U-shaped infusion tube 4 is located 9 to 11 cm below the interface layer of the organic amine-sodium chloride aqueous solution, in order to ensure that the organic amine after stratification can be fully delivered into the stratification tank 3 through the U-shaped infusion tube 4 under the premise of pressurization.

[0037] Specifically, a pH meter for detecting the pH value of the liquid is provided in the reactor 1, and a controller is provided on the reactor 1. The pH meter is electrically connected to the controller, and the pH value of the pH meter is used to determine whether to add a sufficient amount of solid alkali, thereby ensuring that the organic amine salt hydrochloride aqueous solution reacts completely with the solid alkali.

[0038] Specifically, the bottom wall of the stratification tank 3 is a conical structure. In order to quickly discharge the stratified sodium chloride aqueous solution, a discharge pipe 6 is provided at the bottom of the stratification tank 3 .

[0039] Specifically, a mirror observation window 7 is provided on the side wall close to the bottom wall of the reactor 1 for observing the situation at the bottom of the reactor 1 .

[0040] Specifically, in order to improve the utilization rate of the sodium chloride aqueous solution, a liquid return pipe is provided at the bottom of the reactor 1 to form a closed loop with the top of the reactor 1, and a lifting pump is provided on the liquid return pipe, which is connected to the second injection port.

[0041] Specifically, a heating element is provided in the reactor 1 to increase the reaction rate of the solid base and the organic amine salt hydrochloride aqueous solution in the reactor 1 and promote the forward progress of the reaction. The reactor 1 is provided with a first inlet, a second inlet and a third inlet. The first inlet is used to feed the solid base that frees the organic amine from the organic amine hydrochloride aqueous solution, the second inlet is used to feed the saturated sodium chloride aqueous solution that separates the organic amine and water, and the third inlet is used to feed the organic amine salt hydrochloride aqueous solution. The first inlet, the second inlet and the third inlet are all provided with sealing covers.

[0042] Specifically, valves are provided on the inert gas delivery pipe 2, the U-shaped infusion pipe 4 and the discharge pipe 6, which can timely control when the inert gas delivery pipe 2, the U-shaped infusion pipe 4 and the discharge pipe 6 are connected to the recovery device.

[0043] Although the embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. An organic amine hydrochloride recovery device, comprising a reactor (1), wherein the reactor (1) is a sealed reactor, characterized in that: Also includes: A stirring assembly (5) is disposed in the reaction kettle (1) along the longitudinal direction and is used to uniformly mix the organic amine salt hydrochloride aqueous solution, the solid alkali and the saturated sodium chloride aqueous solution fed into the reaction kettle (1); An inert gas delivery pipe (2) passes through the reactor (1) in the longitudinal direction and is sealedly connected to the reactor (1); a gas outlet of the inert gas delivery pipe (2) is located above the liquid level in the reactor (1) and is used to increase the gas pressure in the reactor (1); The U-shaped liquid infusion tube (4) is an inverted U-shaped tube, comprising an input end and an output end, wherein the input end is arranged below the liquid interface layer of the organic amine-sodium chloride aqueous solution in the reaction kettle (1), and the output end of the U-shaped liquid infusion tube (4) is located outside the reaction kettle (1); The stratification tank (3) is arranged outside the reaction kettle (1) and is connected to the output end of the U-shaped infusion tube (4). It is used to collect the organic amine and saturated sodium chloride aqueous solution sent out by the U-shaped infusion tube (4) and allow them to be statically stratified in the stratification tank (3).

2. The organic amine hydrochloride recovery device according to claim 1, characterized in that: The output end of the U-shaped infusion tube (4) located in the stratified tank (3) is arranged close to the inner wall of the stratified tank (3).

3. The organic amine hydrochloride recovery device according to claim 1, characterized in that: A guide plate is obliquely provided on the output end of the U-shaped infusion tube (4), the upper end of the guide plate is fixedly connected to the output end of the U-shaped infusion tube (4), and a gap is reserved between the lower end of the guide plate and the inner wall of the stratified tank (3).

4. The organic amine hydrochloride recovery device according to claim 1, characterized in that: The input end of the U-shaped infusion tube (4) is located 9 to 11 cm below the boundary layer of the organic amine-sodium chloride aqueous solution.

5. The organic amine hydrochloride recovery device according to claim 1, characterized in that: The reactor (1) is provided with a pH meter for detecting the pH value of the liquid. The reactor (1) is provided with a controller, and the pH meter is electrically connected to the controller.

6. The organic amine hydrochloride recovery device according to claim 1, characterized in that: The bottom wall of the stratified tank (3) is a conical structure, and a discharge pipe (6) is provided at the bottom of the stratified tank (3).

7. The organic amine hydrochloride recovery device according to claim 1, characterized in that: A mirror observation window (7) is provided on the side wall close to the bottom wall of the reaction kettle (1).

8. The organic amine hydrochloride recovery device according to claim 1, characterized in that: The bottom of the reaction kettle (1) is provided with a liquid return pipe which forms a closed loop with the top of the reaction kettle (1), and the liquid return pipe is provided with a lifting pump which is connected to the second delivery port.

9. The organic amine hydrochloride recovery device according to claim 1, characterized in that: The reactor (1) is provided with a heating element. The reactor (1) is provided with a first inlet, a second inlet and a third inlet. The first inlet is used for feeding a solid base to release the organic amine from the organic amine hydrochloride aqueous solution. The second inlet is used for feeding a saturated sodium chloride aqueous solution to separate the organic amine and water. The third inlet is used for feeding an organic amine salt hydrochloride aqueous solution. The first inlet, the second inlet and the third inlet are all provided with sealing covers.

10. The organic amine hydrochloride recovery device according to claim 6, characterized in that: The inert gas delivery pipe (2), the U-shaped liquid delivery pipe (4) and the discharge pipe (6) are all provided with valves.

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