Allyl tertiary amine synthesis device and synthesis method

Abstract

The invention discloses a synthesis device and a synthesis method of allyl tertiary amine, and belongs to the field of fine chemical engineering. The synthesis device of the allyl tertiary amine comprises a dimethylamine raw material tank, a chloropropene raw material tank, a dimethylamine raw material pump, a chloropropene raw material pump, a microchannel reactor, an intermediate storage tank, a dimethyl allyl crude product tank and a pH control system, a discharge port of the dimethylamine raw material tank is connected with an inlet of the dimethylamine raw material pump, and an outlet of the dimethylamine raw material pump is connected with the micro-channel reactor; a discharge port of the chloropropene raw material tank is connected with an inlet of the chloropropene raw material pump, and an outlet of the chloropropene raw material pump is connected with the microchannel reactor; a discharge port of the micro-channel reactor is connected with an intermediate storage tank, the intermediate storage tank is connected with a dimethyl allyl crude product tank through a pipeline, and an upper organic phase is guided into the dimethyl allyl crude product tank; the pH control system is connected with the micro-channel reactor and is used for controlling the pH of a reaction system in the micro-channel reactor.

Description

Technical Field

[0001] The invention relates to the field of fine chemicals, and in particular to a synthesis device and a synthesis method of tertiary allyl amine. Background Art

[0002] Dimethylallylamine (also known as N,N-dimethylallylamine, DMAA for short) is a chemical compound with the formula C5H 11 An organic compound of nitrogen. At normal pressure, it appears as a colorless liquid with an ammoniacal odor, is flammable, explosive, volatile, and unstable to light. It is almost insoluble in water but dissolves well in organic solvents. Its main uses include as a chemical intermediate for the manufacture of pesticides (such as chloranthate), and in the synthesis of quaternary ammonium compounds, which are used as the basis for a variety of processing aids and additives.

[0003] The traditional synthesis method uses a traditional kettle reactor to react, with dimethylamine and allyl chloride as raw materials, sodium hydroxide as an acid binding agent, and the reaction ratio is n (dimethylamine): n (allyl chloride): n (sodium hydroxide) = 1.05-1.1:1:1. This type of reactor has a small specific surface area, limited heat and mass transfer capacity, and requires more energy consumption to control the reaction temperature. In addition, a long residence time and a high alkaline temperature will cause allyl chloride to hydrolyze rapidly, producing harmful substances such as allyl alcohol, thereby reducing the product yield.

[0004] Patent CN114470840A proposes a new synthesis method, which integrates the three steps of dimethylamine purification, dimethylallylamine synthesis and separation in a reactive distillation column. By using a dimethylamine recovery reactor and a dimethylamine recovery column to recover dimethylamine, a dimethylallylamine product with a content of more than 98% can be obtained at the side line at the bottom of the reactive distillation column. However, this method requires high equipment performance and relies solely on the gravity of the raw materials for mixing, which may lead to problems such as insufficient raw material mixing and low reaction rate.

[0005] Patent CN117229149 mixes dimethylamine aqueous solution and propylene chloride in a first mixer according to the reaction molar ratio, and then enters the first reactor for synthesis reaction. The products after the reaction enter the phase separation tank for stratification treatment to obtain an upper oil phase and a lower water phase. The upper oil phase is purified to obtain a high-purity dimethylallylamine product, while the lower water phase is evaporated and concentrated for raw material recovery. This method realizes the recycling of dimethylamine, reduces raw material consumption, and can obtain low-cost sodium chloride. In addition, this patent also introduces microreactor technology to improve heat and mass transfer problems and increase reaction rate. However, liquid alkali is not added during the tertiary amination reaction, resulting in HCl gas combining with dimethylamine and tertiary amine to form impurities such as dimethylamine hydrochloride and tertiary amine hydrochloride, which will hinder the reaction and reduce the purity and conversion rate of the monomer.

[0006] The present application proposes a novel allyl tertiary amine synthesis device and method. By adding liquid caustic soda in a timely manner during the reaction process, the pH value of the reaction system is maintained between 7 and 12. Liquid caustic soda, as an acid binding agent, can consume the hydrogen chloride gas generated during the main reaction process, prevent HCl gas from combining with dimethylamine and allyl tertiary amine to form impurities, thereby improving the purity and conversion rate of allyl tertiary amine. This improvement helps to overcome the limitations of the prior art and improve the reaction efficiency and product quality. Summary of the invention

[0007] The purpose of the present invention is to provide a synthesis device and a synthesis method of allyl tertiary amine to solve the technical problems mentioned in the above background technology.

[0008] The technical scheme for achieving the purpose of the present invention is: a synthesis device for tertiary allyl amine, comprising a dimethylamine raw material tank, a chloropropylene raw material tank, a dimethylamine raw material pump, a chloropropylene raw material pump, a reactor, an intermediate storage tank, a dimethylallyl crude product tank, and a pH control system; the discharge port of the dimethylamine raw material tank is connected to the inlet of the dimethylamine raw material pump, and the outlet of the dimethylamine raw material pump is connected to the reactor; the discharge port of the chloropropylene raw material tank is connected to the inlet of the chloropropylene raw material pump, and the outlet of the chloropropylene raw material pump is connected to the reactor; the discharge port of the reactor is connected to the intermediate storage tank, and the intermediate storage tank is connected to the reactor through a pipeline. The crude dimethylallyl product tank is used to introduce the upper organic phase into the crude dimethylallyl product tank; the pH control system is connected to the reactor to monitor and control the pH of the reaction system in the reactor in real time; the synthesis device of the allyl tertiary amine of the invention has a simple device structure, and the pH control system is arranged on the synthesis device of the allyl tertiary amine, which can monitor and control the pH of the reaction system in the reactor in real time, reduce the generation of by-products, make the raw materials react fully, improve the utilization rate of the raw materials, the reaction conversion rate, and the purity of the crude dimethylallyl product, and increase the yield of the product.

[0009] Furthermore, the pH control system comprises a liquid alkali raw material tank, a liquid alkali raw material pump, a pH controller, a valve, and a pipeline assembly; the discharge port of the liquid alkali raw material tank is connected to the reactor through the pipeline assembly; the liquid alkali raw material pump and the valve are both arranged on the pipeline assembly; the pH controller is arranged on the reactor and electrically connected to the valve to control the opening degree of the valve; the pH control system of the present invention comprises a liquid alkali raw material tank, a liquid alkali raw material pump, a pH controller, and a valve; the liquid alkali in the liquid alkali raw material tank enters the reactor through the liquid alkali raw material pump; the pH controller monitors the pH of the material in the reactor reaction process in real time, and controls the valve opening degree according to the preset pH value to control the liquid alkali addition flow rate, so that the pH of the material in the reaction process is within the preset pH value range.

[0010] Furthermore, the pipeline assembly includes a main pipeline and multiple branch pipelines, one end of the multiple branch pipelines is connected to the main pipeline, and the other ends of the multiple branch pipelines are dispersedly connected to the side wall of the reactor; one end of the main pipeline away from the branch pipeline is connected to the discharge port of the liquid alkali raw material tank; the liquid alkali raw material pump is arranged on the main pipeline; each branch pipeline is provided with a valve, and each valve is electrically connected to a pH controller.

[0011] The present invention adopts a plurality of branch pipes which are dispersedly connected on the side wall of the reactor, and each branch pipe is provided with a valve, and each valve is electrically connected to a pH controller, so as to realize real-time monitoring and precise control of the pH at the corresponding position of each branch pipe, reduce the phenomenon of by-products generated due to the local pH of the material in the reactor deviating from the preset pH value, further increase the utilization rate of the raw materials, improve the purity of the crude product, and increase the yield of the product.

[0012] Furthermore, the reactor adopts a microchannel reactor; the reactor of the present invention adopts a microchannel reactor, and compared with the traditional kettle reactor, the internal flow channel size is very small, and it has a very large surface area to volume ratio. The heat per unit volume can be quickly transferred to the reactor wall, and then the heat is quickly removed or supplemented by the cooling or heating medium, and the heat transfer capacity is good; and its fluid forms a laminar flow state when flowing in the microchannel, which has a better mixing effect and uniform mass transfer; in addition, the microchannel reactor has a shorter residence time. Compared with the traditional kettle reactor, when used in conjunction with the pH control system, the microchannel reactor will not cause the heat in the reactor to be unable to be effectively dissipated due to poor mass transfer and heat transfer effects, thereby causing the temperature of the reaction system to rise, causing allyl chloride to hydrolyze under alkaline high temperature conditions to generate harmful byproducts such as allyl alcohol, thereby interfering with the normal progress of the reaction. Similarly, due to the short residence time, a large amount of allyl chloride will not be retained in the reactor for a long time, and then hydrolyzed to produce byproducts such as allyl alcohol, resulting in a problem of reduced raw material utilization.

[0013] Furthermore, a jacket is provided outside the microchannel reactor, and a heat exchange medium is passed between the jacket and the microchannel reactor to control the temperature of the microchannel reactor.

[0014] The present invention also provides a method for synthesizing tertiary allyl amine, comprising: feeding a dimethylamine aqueous solution in a dimethylamine raw material tank and allyl chloride in a allyl chloride raw material tank into a reactor through a dimethylamine raw material pump and an allyl chloride raw material pump according to a feed reaction molar ratio, performing a synthesis reaction at a reaction temperature, and controlling the pH of the reaction system within a preset pH value range through a pH control system during the reaction; after the synthesis reaction is completed, the materials enter an intermediate storage tank for static stratification, and after stratification, an upper organic phase and a lower aqueous phase are obtained, and the upper organic phase is introduced into a dimethylallyl crude product tank.

[0015] Furthermore, the method for controlling the pH of the reaction system by the pH control system is as follows: the liquid alkali in the liquid alkali raw material tank enters into each branch pipeline from the main pipeline through the liquid alkali raw material pump, and then enters into the reactor from each branch pipeline, and the pH controller at each branch pipeline in the reactor monitors in real time whether the pH of the material in the reaction process there deviates from the preset pH, and the pH controller controls the flow of liquid alkali through the branch pipeline by controlling the degree of opening of the valve, thereby performing real-time regulation on the pH of the material in the reaction process at each branch pipeline.

[0016] Furthermore, the feed reaction molar ratio of dimethylamine and allyl chloride in the dimethylamine aqueous solution is 1.05-1.1:1.

[0017] Furthermore, the preset pH value range is 7 to 12; the pH of the materials in the reaction process of synthesizing tertiary allyl amine of the present invention is controlled at 7 to 12 to consume the hydrogen chloride generated in the reaction process, reduce the occurrence of side reactions, make the raw materials react fully, thereby increasing the utilization rate of the raw materials, improving the purity of the crude product, and increasing the yield of the product.

[0018] Furthermore, the reaction temperature is below 35° C.; the reaction temperature for synthesizing tertiary allyl amine in the present invention is controlled below 35° C., thereby avoiding the generation of by-products at high temperatures, thereby increasing the utilization rate of raw materials, improving the purity of crude products, and increasing the yield of products.

[0019] By adopting the above technical solution, the present invention has the following beneficial effects:

[0020] (1) The synthesis device of tertiary allyl amine of the present invention is provided with a pH control system, which can monitor and control the pH of the reaction system in the reactor in real time, reduce the generation of by-products, make the raw materials fully react, improve the raw material utilization rate, reaction conversion rate, and purity of the dimethylallyl crude product, and increase the yield of the product.

[0021] (2) The pH control system of the present invention comprises a liquid alkali raw material tank, a liquid alkali raw material pump, a pH controller, and a valve. The liquid alkali in the liquid alkali raw material tank enters the reactor through the liquid alkali raw material pump. The pH controller monitors the pH of the material in the reactor reaction process in real time, and controls the valve opening degree according to the preset pH value to control the liquid alkali addition flow rate, so that the pH of the material in the reaction process is within the preset pH value range.

[0022] (3) The present invention adopts a plurality of branch pipes which are dispersedly connected on the side wall of the reactor, and each branch pipe is provided with a valve, and each valve is electrically connected to a pH controller, so as to realize real-time monitoring and precise control of the pH at the corresponding position of each branch pipe, thereby reducing the phenomenon of by-products produced due to the local pH of the material in the reactor deviating from the preset pH value, further increasing the utilization rate of the raw materials, improving the purity of the crude product, and increasing the yield of the product.

[0023] (4) The reactor of the present invention adopts a microchannel reactor. Compared with the traditional kettle reactor, the internal flow channel size is very small, and it has a very large surface area to volume ratio. The heat per unit volume can be quickly transferred to the reactor wall, and then the heat is quickly removed or supplemented by the cooling or heating medium, and the heat transfer capacity is good; and the fluid forms a laminar flow state when flowing in the microchannel, which has a better mixing effect and uniform mass transfer; in addition, the microchannel reactor has a shorter residence time. Compared with the traditional kettle reactor, when used in conjunction with the pH control system, the microchannel reactor will not cause the heat in the reactor to be unable to be effectively dissipated due to poor mass transfer and heat transfer effects, thereby causing the temperature of the reaction system to rise, causing allyl chloride to hydrolyze under alkaline high temperature conditions to generate harmful byproducts such as allyl alcohol, thereby interfering with the normal progress of the reaction. Similarly, due to the short residence time, a large amount of allyl chloride will not be retained in the reactor for a long time, and then hydrolyzed to produce byproducts such as allyl alcohol, resulting in a problem of reduced raw material utilization.

[0024] (5) The microchannel reactor of the present invention is provided with a jacket on the outside, and a heat exchange medium is passed between the jacket and the microchannel reactor to control the reaction temperature in the microchannel reactor.

[0025] (6) The method for synthesizing tertiary allyl amine of the present invention has a simple process, few by-products, high crude product purity and high yield. The present invention combines a reactor with a pH control system, has a simple process, and controls the pH of the materials during the reaction to consume the hydrogen chloride generated during the reaction, thereby reducing the occurrence of side reactions and allowing the raw materials to fully react, thereby increasing the utilization rate of the raw materials, improving the purity of the crude product, and increasing the yield of the product.

[0026] (7) The reaction temperature for synthesizing tertiary allyl amine in the present invention is controlled below 35° C., thereby avoiding the generation of by-products at high temperatures, thereby increasing the utilization rate of raw materials, improving the purity of crude products, and increasing the yield of products.

[0027] (8) The pH of the materials in the process of synthesizing tertiary allyl amine in the present invention is controlled at 7 to 12 to consume the hydrogen chloride produced in the reaction process, reduce the occurrence of side reactions, allow the raw materials to react fully, and thus increase the utilization rate of the raw materials, improve the purity of the crude product, and increase the yield of the product. BRIEF DESCRIPTION OF THE DRAWINGS

[0028] In order to make the content of the present invention more clearly understood, the present invention is further described in detail below according to specific embodiments and in conjunction with the accompanying drawings, wherein

[0029] Figure 1 It is a schematic structural diagram of the synthesis device of allyl tertiary amine of the present invention.

[0030] The numbers in the accompanying drawings are: dimethylamine raw material tank 101, allyl chloride raw material tank 201, liquid caustic soda raw material tank 301, dimethylamine raw material pump 102, allyl chloride raw material pump 202, liquid caustic soda raw material pump 302, microchannel reactor 401, insulation jacket 402, pH controller 303, valve 304, intermediate storage tank 501, dimethylallyl crude product tank 601. DETAILED DESCRIPTION

[0031] In order to better understand the above technical solution, the above technical solution will be described in detail below in conjunction with the accompanying drawings and specific implementation methods.

[0032] In order to make the purpose, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the drawings in the embodiments of the present invention. Obviously, the described embodiments are part of the embodiments of the present invention, not all of the embodiments. Generally, the components of the embodiments of the present invention described and shown in the drawings here can be arranged and designed in various different configurations.

[0033] Therefore, the following detailed description of the embodiments of the present invention provided in the accompanying drawings is not intended to limit the scope of the invention claimed for protection, but merely represents selected embodiments of the present invention. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0034] It should be noted that similar reference numerals and letters denote similar items in the following drawings, and therefore, once an item is defined in one drawing, further definition and explanation thereof is not required in subsequent drawings.

[0035] In the description of the embodiments of the present invention, it should be understood that the terms "center", "up", "down", "left", "right", "vertical", "horizontal", "inside", "outside", etc. indicate orientations or positional relationships based on the orientations or positional relationships shown in the accompanying drawings, or are the orientations or positional relationships in which the inventive product is conventionally placed when used, or are the orientations or positional relationships conventionally understood by those skilled in the art. They are only for the convenience of describing the present invention and simplifying the description, and do not indicate or imply that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and therefore should not be understood as a limitation on the present invention.

[0036] In the description of the embodiments of the present invention, it is also necessary to explain that, unless otherwise clearly specified and limited, the terms "set", "installed", "connected" and "connected" should be understood in a broad sense. For example, it can be a fixed connection, a detachable connection, or an integral connection; it can be directly connected, or indirectly connected through an intermediate medium, or it can be the internal connection of two components. For ordinary technicians in this field, the specific meanings of the above terms in the present invention can be understood according to specific circumstances. The present invention is further described below in conjunction with the accompanying drawings. The following embodiments are only used to more clearly illustrate the technical solution of the present invention, and cannot be used to limit the scope of protection of the present invention.

[0037] Inventive concept: The dimethylamine aqueous solution in the dimethylamine raw material tank 101 and the allyl chloride in the allyl chloride raw material tank 201 enter the microchannel reactor 401 through the dimethylamine raw material pump 102 and the allyl chloride raw material pump 202 at a reaction molar ratio of 1.05-1.1:1, respectively, and a synthesis reaction is carried out at a reaction temperature below 35°C. During the reaction, when the pH controller monitors in real time that the pH of the material in the reaction process deviates from the preset pH, the pH controller issues an instruction to the valve, and controls the liquid alkali addition flow rate by opening or closing the valve to control the pH of the material in the reaction process within the preset pH range of 7-12. Within the pH range of 7-12, the pH of the material in the reaction process is 7-12 by adding the liquid alkali during the reaction process. The liquid alkali serves as an acid binding agent to consume the hydrogen chloride gas generated by the main reaction, thereby preventing the HCl gas from combining with the dimethylamine and the allyl tertiary amine to generate impurities of dimethylamine hydrochloride and tertiary amine hydrochloride to hinder the main reaction and reduce the purity and conversion rate of the allyl tertiary amine.

[0038] The specific path is as follows:

[0039]

[0040] (Device Example)

[0041] See Figure 1A synthesis device for tertiary allyl amine comprises a dimethylamine raw material tank 101, a chloropropylene raw material tank 201, a dimethylamine raw material pump 102, a chloropropylene raw material pump 202, a microchannel reactor 401, an intermediate storage tank 501, a dimethylallyl crude product tank 601, and a pH control system; the discharge port of the dimethylamine raw material tank 101 is connected to the inlet of the dimethylamine raw material pump 102, and the outlet of the dimethylamine raw material pump 102 is connected to the microchannel reactor 401; the outlet of the chloropropylene raw material tank 2 ... The feed port is connected to the inlet of the allyl chloride raw material pump 202, and the outlet of the allyl chloride raw material pump 202 is connected to the microchannel reactor 401; the discharge port of the microchannel reactor 401 is connected to the intermediate storage tank 501, and the intermediate storage tank 501 is connected to the dimethylallyl crude product tank 601 through a pipeline to introduce the upper organic phase into the dimethylallyl crude product tank 601; the pH control system is connected to the microchannel reactor 401 to monitor and control the pH of the reaction system in the microchannel reactor 401 in real time.

[0042] Among them, the pH control system includes a liquid alkali raw material tank 301, a liquid alkali raw material pump 302, a pH controller 303, a valve 304, and a pipeline assembly; the discharge port of the liquid alkali raw material tank 301 is connected to the microchannel reactor 401 through a pipeline assembly; the pipeline assembly includes a main pipeline and 6 branch pipelines, one end of the 6 branch pipelines is connected to the main pipeline, and the other ends of the 6 branch pipelines are dispersedly connected to the side wall of the microchannel reactor 401; one end of the main pipeline away from the branch pipeline is connected to the discharge port of the liquid alkali raw material tank 301; the liquid alkali raw material pump 302 is arranged on the main pipeline; each branch pipeline is provided with a valve, each valve is electrically connected to a pH controller 303, and the pH controller 303 controls the degree of valve opening.

[0043] A jacket 402 is disposed outside the microchannel reactor 401 , and a heat exchange medium is passed between the jacket 402 and the microchannel reactor 401 to control the temperature of the microchannel reactor 401 .

[0044] Method Example 1

[0045] The 41.6% dimethylamine aqueous solution in the dimethylamine raw material tank 101 and the allyl chloride in the allyl chloride raw material tank 201 enter the microchannel reactor 401 through the dimethylamine raw material pump 102 and the allyl chloride raw material pump 202 at 6.00kg / h and 4.04kg / h respectively, and the synthesis reaction is carried out at a reaction temperature below 35 degrees Celsius. The pH control system controls the addition flow rate of 40% liquid caustic soda to control the pH of the materials in the reaction process to 7-12; wherein the total flow rate of the liquid caustic soda is 5.28kg / h.

[0046] After the dimethylamine aqueous solution and allyl chloride were fed for 1 hour, the materials after the synthesis reaction were put into the intermediate storage tank 501 for static stratification. After stratification, an upper organic phase and a lower aqueous phase were obtained. The upper organic phase entered the dimethylallyl crude product tank 601. The purity of tertiary allyl amine in the upper organic phase was measured to be 96.1%. The upper organic phase was 4.27 kg, and the lower aqueous phase was 11.05 kg. The yield of tertiary allyl amine was 92.4%.

[0047] Method Example 2

[0048] A method for synthesizing tertiary allyl amines. A dimethylamine aqueous solution with a concentration of 41.6% in a dimethylamine raw material tank 101 and allyl chloride in an allyl chloride raw material tank 201 enter a microchannel reactor 401 through a dimethylamine raw material pump 102 and an allyl chloride raw material pump 202 at a rate of 6.28 kg / h and 4.04 kg / h, respectively. A synthesis reaction is performed at a reaction temperature below 35 degrees Celsius. The pH of the materials in the reaction process is controlled to be 7-12 by controlling the addition flow rate of liquid caustic soda with a concentration of 40% through a pH control system. The total flow rate of the liquid caustic soda is 5.28 kg / h.

[0049] After the dimethylamine aqueous solution and allyl chloride were fed for 1 hour, the materials after the synthesis reaction were put into the intermediate storage tank 501 for static stratification. After stratification, an upper organic phase and a lower aqueous phase were obtained. The upper organic phase entered the dimethylallyl crude product tank 601. The purity of tertiary allyl amine in the upper organic phase was measured to be 96.8%. The upper organic phase was 4.27 kg, and the lower aqueous phase was 11.33 kg. The yield of tertiary allyl amine was 95.1%.

[0050] Method Example 3

[0051] A method for synthesizing tertiary allyl amines. A dimethylamine aqueous solution with a concentration of 41.6% in a dimethylamine raw material tank 101 and allyl chloride in an allyl chloride raw material tank 201 enter a microchannel reactor 401 through a dimethylamine raw material pump 102 and an allyl chloride raw material pump 202 at a rate of 9.42 kg / h and 6.06 kg / h, respectively. A synthesis reaction is performed at a reaction temperature below 35 degrees Celsius. The pH of the materials in the reaction process is controlled to be 7-12 by controlling the addition flow rate of liquid caustic soda with a concentration of 40% through a pH control system. The total flow rate of the liquid caustic soda is 7.92 kg / h.

[0052] After the dimethylamine aqueous solution and allyl chloride were fed for 1 hour, the materials after the synthesis reaction were put into the intermediate storage tank 501 for static stratification. After stratification, an upper organic phase and a lower aqueous phase were obtained. The upper organic phase entered the dimethylallyl crude product tank 601. The purity of tertiary allyl amine in the upper organic phase was measured to be 98.1%. The upper organic phase was 6.42 kg, and the lower aqueous phase was 16.98 kg. The yield of tertiary allyl amine was 95.3%.

[0053] Method Comparative Example 1

[0054] In an intermittent stirring reactor with stirring and cooling to 0-10°C, 6.28kg of 41.6% dimethylamine aqueous solution was added at one time, and the reaction temperature was controlled at 5-15°C, and 5.28kg of 40% sodium hydroxide and 4.04kg / h of propylene chloride were added alternately. After the addition was completed, the temperature was raised to 30-50°C with stirring, and the reaction time was controlled at 4 hours. The purity of the tertiary allyl amine in the upper organic phase was 91%, the weight of the upper organic phase was 3.87kg, the weight of the lower aqueous phase was 11.73, and the yield of the tertiary allyl amine was 86.3%. The lower aqueous phase was analyzed using a muffle furnace, and the sodium chloride content was 2.67kg.

[0055] Method Comparative Example 2

[0056] The dimethylamine aqueous solution and allyl chloride enter the microchannel reactor at flow rates of 6.00 kg / h and 4.04 kg / h, respectively. No liquid alkali is added during the reaction, and the temperature of the entire microreactor is controlled to be less than 35° C. by the jacket.

[0057] After the dimethylamine aqueous solution and allyl chloride were fed for 1 hour, the mixture was allowed to stand for stratification to obtain an upper organic phase and a lower aqueous phase. The purity of the tertiary allyl amine in the upper organic phase was measured to be 94.0%. The upper organic phase was 4.00 kg, and the lower aqueous phase was 6.04 kg. The yield of the tertiary allyl amine was 89.1%.

[0058] The specific embodiments described above further illustrate the objectives, technical solutions and beneficial effects of the present invention in detail. It should be understood that the above description is only a specific embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent substitutions, improvements, etc. made within the spirit and principles of the present invention should be included in the protection scope of the present invention.

Claims

1. A synthesis device for tertiary allyl amine, characterized in that: The invention comprises a dimethylamine raw material tank (101), a chloropropylene raw material tank (201), a dimethylamine raw material pump (102), a chloropropylene raw material pump (202), a reactor, an intermediate storage tank (501), a dimethylallyl crude product tank (601), and a pH control system; the discharge port of the dimethylamine raw material tank (101) is connected to the inlet of the dimethylamine raw material pump (102), and the outlet of the dimethylamine raw material pump (102) is connected to the reactor; the discharge port of the chloropropylene raw material tank (201) is connected to the inlet of the chloropropylene raw material pump (202), and the outlet of the chloropropylene raw material pump (202) is connected to the reactor; the discharge port of the reactor is connected to the intermediate storage tank (501), and the intermediate storage tank (501) is connected to the dimethylallyl crude product tank (601) through a pipeline, and the upper organic phase is introduced into the dimethylallyl crude product tank (601); The pH control system is connected to the reactor to monitor and control the pH of the reaction system in the reactor in real time.

2. The synthesis device of tertiary allyl amine according to claim 1, characterized in that: The pH control system comprises a liquid alkali raw material tank (301), a liquid alkali raw material pump (302), a pH controller (303), a valve (304), and a pipeline assembly; the discharge port of the liquid alkali raw material tank (301) is connected to the reactor via the pipeline assembly; the liquid alkali raw material pump (302) and the valve (304) are both arranged on the pipeline assembly; the pH controller (303) is arranged on the reactor and electrically connected to the valve to control the opening degree of the valve.

3. The synthesis device of tertiary allyl amine according to claim 2, characterized in that: The pipeline assembly comprises a main pipeline and a plurality of branch pipelines, one end of the plurality of branch pipelines is connected to the main pipeline, and the other ends of the plurality of branch pipelines are dispersedly connected to the side wall of the reactor; one end of the main pipeline away from the branch pipeline is connected to the discharge port of the liquid alkali raw material tank (301); the liquid alkali raw material pump (302) is arranged on the main pipeline; each branch pipeline is provided with a valve, and each valve is electrically connected to a pH controller (303).

4. The synthesis device of tertiary allyl amine according to claim 1, characterized in that: The reactor is a microchannel reactor (401).

5. The synthesis device of tertiary allyl amine according to claim 4, characterized in that: A jacket is arranged outside the microchannel reactor, and a heat exchange medium is passed between the jacket and the microchannel reactor to control the temperature of the microchannel reactor.

6. A method for synthesizing allyl tertiary amine based on the allyl tertiary amine synthesis device according to any one of claims 1 to 5, characterized in that: include: The dimethylamine aqueous solution in the dimethylamine raw material tank (101) and the allyl chloride in the allyl chloride raw material tank (201) are respectively fed into the reactor through the dimethylamine raw material pump (102) and the allyl chloride raw material pump (202) according to the feed reaction molar ratio, and a synthesis reaction is carried out at the reaction temperature. During the reaction, the pH of the reaction system is controlled within a preset pH value range through a pH control system; after the synthesis reaction is completed, the materials enter the intermediate storage tank (501) for static stratification, and after stratification, an upper organic phase and a lower aqueous phase are obtained, and the upper organic phase is introduced into a dimethylallyl crude product tank (601).

7. The method for synthesizing tertiary allyl amine according to claim 6, characterized in that: The pH control system comprises a liquid alkali raw material tank (301), a liquid alkali raw material pump (302), a pH controller (303), a valve (304), and a pipeline assembly; the pH control system controls the pH of the reaction system in the following manner: the liquid alkali in the liquid alkali raw material tank (301) enters each branch pipeline from the main pipeline through the liquid alkali raw material pump (302), and then enters the reactor from each branch pipeline; the pH controller (303) at each branch pipeline in the reactor monitors in real time whether the pH of the material in the reaction process at the branch pipeline deviates from the preset pH; the pH controller (303) controls the flow of the liquid alkali passing through the branch pipeline by controlling the opening degree of the valve (304), thereby regulating the pH of the material in the reaction process at each branch pipeline in real time.

8. The method for synthesizing tertiary allyl amine according to claim 6, characterized in that: The feed reaction molar ratio is n(dimethylamine):n(propylene chloride)=1.05-1.1:

1.

9. The method for synthesizing tertiary allyl amine according to claim 6, characterized in that: The preset pH value range is 7-12.

10. The method for synthesizing tertiary allyl amine according to claim 6, characterized in that: The reaction temperature is below 35°C.

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