Reactor for continuously synthesizing trialkyl phosphite by nitrogen-nitrogen dimethylaniline method

Abstract

The utility model provides a reactor for continuously synthesizing trialkyl phosphite by a nitrogen-nitrogen dimethylaniline method. According to the reactor, a reaction cavity is formed between reactor shells, the upper portion of the reactor is provided with a discharging port and an emptying port, the lower portion of the reactor is provided with an emptying port, a left stirring base and a right stirring base, and one side of each shell is provided with a phosphorus trichloride feeding pipe, an acid binding agent, an alkanol feeding pipe and an ammonia gas feeding pipe and is communicated with the reaction cavity; a first adjusting control valve, a first intelligent flow meter, a second adjusting control valve, a second intelligent flow meter, a third adjusting control valve and a third intelligent flow meter are respectively mounted on the three feeding pipes, and two sets of stirring mechanisms are respectively mounted in the reaction cavity. According to the reactor, raw materials can continuously enter the reactor for reaction, the yield of the product to phosphorus trichloride reaches 98-100%, the occupied area of the reactor is only one fifth of that of similar equipment, the operation is simple and convenient, the automation degree is high, and the production safety and physical and psychological health of workers are ensured.

Description

Technical Field

[0001] The utility model relates to the technical field of chemical equipment and chemical reactors, in particular to a reactor for continuously synthesizing trialkyl phosphite by a nitrogen-nitrogen dimethylaniline method. Background Art

[0002] Reactors are also called reactors in the chemical industry. The chemical reactors commonly used in the prior art are all tank-type, and the materials used to make them are also divided into various types, such as enamel, stainless steel, carbon steel, ceramics, etc. At present, the industrial production of trialkyl phosphite has triethylamine continuous process and nitrogen-nitrogen dimethylaniline intermittent process. The current domestic large-scale industrial production adopts triethylamine continuous process. Although the nitrogen-nitrogen dimethylaniline process has reported continuous production patents, there is no report on the enterprises that truly use nitrogen-nitrogen dimethylaniline to continuously produce such products. The enterprises that produce such products all use nitrogen-nitrogen dimethylaniline intermittent process to produce such products. The process of using triethylamine continuous process to produce such products is very perfect, and the industrial yield of phosphorus trichloride is almost 98%. However, using nitrogen-nitrogen dimethylaniline intermittent process to produce such products, its yield of phosphorus trichloride can only reach about 80%, which is much lower than the triethylamine continuous process. If the yield of phosphorus trichloride can reach the same yield as that of the continuous triethylamine method when the nitrogen-nitrogen dimethylaniline method is used for production, the cost will be greatly reduced. When the continuous triethylamine method is used to produce such products, the wastewater contains about 17% sodium chloride, which must be recycled, otherwise it will pollute the environment. The recycled sodium chloride has a very narrow use. When the nitrogen-nitrogen dimethylaniline method is used to continuously produce such products, the wastewater contains only about 17% ammonium chloride. When the wastewater is treated, ammonium chloride that can be used as fertilizer is recycled, which is cheap and has a good market.

[0003] When triethylamine is used to continuously produce this type of product, a large amount of energy (steam) is required, because a large amount of solvent with a content of about 8% needs to be evaporated. The steam consumption per ton of product is about 3 tons more than that of nitrogen-nitrogen dimethylaniline, and its energy consumption is much higher than the latter. The use of this type of product produced by the triethylamine method is not as wide as that of the latter. In short, the continuous production of trialkyl phosphite by the nitrogen-nitrogen dimethylaniline method has become a target to be conquered. In order to solve the normal operation of this process, the key equipment used in this method, namely the synthesis reactor, must be solved. Summary of the invention

[0004] The purpose of the utility model is to provide a reactor for continuously synthesizing trialkyl phosphite by the nitrogen-nitrogen dimethylaniline method. The technical problem to be solved by the utility model is: by means of a reasonably designed reactor, the key technical problem of continuously producing trialkyl phosphite by the nitrogen-nitrogen dimethylaniline method instead of the triethylamine method is solved.

[0005] To achieve the above purpose, the technical solution of the utility model is:

[0006] A reactor for continuously synthesizing trialkyl phosphite by a nitrogen-nitrogen dimethylaniline method, comprising: a reactor shell, a discharge port, a mounting frame, a venting port, a No. 1 regulating control valve, a No. 1 intelligent flow meter, a No. 2 intelligent flow meter, a No. 3 intelligent flow meter, a No. 3 regulating control valve, a No. 2 regulating control valve, a phosphorus trichloride feed pipe, an acid binding agent, an alkanol feed pipe, an ammonia feed pipe, a right stirring seat, a reaction chamber, a drain port, a left stirring seat, a control console, and a stirring mechanism, wherein the stirring mechanism comprises: a connecting rod, a blade, a left stirring shaft, a left drive assembly, a right drive assembly, and a right stirring shaft. The reactor forms a reaction chamber between the reactor shells. A discharge port is arranged on one side of the upper part of the reactor shell, a vent port is arranged in the middle of the top, a drain port is arranged in the middle of the lower part of the reactor shell, a phosphorus trichloride feed pipe, an acid binding agent, an alkanol feed pipe, and an ammonia feed pipe are installed on the other side of the reactor shell and are connected with the reaction chamber, a No. 1 regulating control valve and a No. 1 intelligent flow meter are installed on the phosphorus trichloride feed pipe, a No. 2 regulating control valve and a No. 2 intelligent flow meter are installed on the acid binding agent and the alkanol feed pipes, a No. 3 regulating control valve and a No. 3 intelligent flow meter are installed on the ammonia feed pipe, a right stirring seat and a left stirring seat are respectively installed at the lower part of the reactor shell, and two sets of stirring mechanisms are respectively installed in the reaction chamber.

[0007] The stirring mechanism in the reactor is equipped with two mounting frames on the upper part of the reactor shell, and a left driving component and a right driving component are respectively installed on the two mounting frames. The left driving component is equipped with a left stirring shaft, and the right driving component is equipped with a right stirring shaft. The left stirring shaft and the right stirring shaft are respectively equipped with connecting rods and blades, and the ends of the left stirring shaft and the right stirring shaft are respectively connected to the left stirring seat and the right stirring seat.

[0008] The left driving assembly, the right driving assembly, the No. 1 regulating control valve, the No. 1 intelligent flow meter, the No. 2 regulating control valve, the No. 2 intelligent flow meter, the No. 3 regulating control valve and the No. 3 intelligent flow meter in the reactor are respectively connected to the control console by wires.

[0009] The left drive assembly and the right drive assembly include a drive motor and a reducer. Figure 1 The arrow in the middle indicates the direction of material flow.

[0010] Compared with the prior art, the positive effects of the utility model are:

[0011] 1. Under the conditions that meet the process requirements, the reactor can allow the solvent, alkyl alcohol, acid-binding agent nitrogen-nitrogen dimethylaniline and reducing agent ammonia to continuously enter the reactor for reaction after being measured by the intelligent flow meter;

[0012] 2. The products and solvents produced by the reactor continuously flow out of the reactor and enter the next continuous process;

[0013] 3. The reaction product produced by the reactor is continuously washed with water, and the water-washed product is analyzed and calculated by gas chromatography, and the yield of phosphorus trichloride of the product reaches 98-100%;

[0014] 4. Compared with similar equipment, the reactor has a much smaller volume. To produce the same amount of product, the reactor occupies only one fifth of the floor space of similar equipment.

[0015] 5. This reactor can continuously produce this type of product in the same space, increasing the output five times;

[0016] 6. Since the reactor adopts the continuous process of all processes, the quality of the product is extremely stable, and there is no phenomenon of high and low product quality when the batch method is produced;

[0017] 7. The reactor is reasonably designed, simple and convenient to operate, can be operated by remote control, and has a high degree of automation, which ensures the production safety and physical and mental health of workers and reduces the difficulty and intensity of operation for operators. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] In order to more clearly illustrate the technology of the utility model, the drawings required for use in the implementation are briefly introduced. The drawings described below are only exemplary, and for ordinary technicians in this field, other implementation drawings can be derived from the provided drawings without creative work.

[0019] The structures, proportions, sizes, etc. of the drawings shown in this specification are only used to match the contents disclosed in the specification so as to facilitate the understanding and reading of those skilled in the art, and are not used to limit the conditions under which the present invention can be implemented. Any structural modification, change in proportion or adjustment in size should still fall within the scope of the technical contents disclosed in the present invention without affecting the effects and purposes that can be achieved by the technology of the present invention.

[0020] Figure 1 , a schematic diagram of the main structure of a reactor for continuous synthesis of trialkyl phosphite;

[0021] Figure 2 , intelligent flow meter, regulating control valve and control console connection block diagram.

[0022] In the figure: 1. reactor shell, 2. connecting rod, 3. blade, 4. left stirring shaft, 5. discharge port, 6. mounting frame, 7. left drive assembly, 8. venting port, 9. right drive assembly, 10. right stirring shaft, 11. No. 1 regulating control valve, 12. No. 1 intelligent flow meter, 13. No. 2 intelligent flow meter, 14. No. 3 intelligent flow meter, 15. No. 3 regulating control valve, 16. No. 2 regulating control valve, 17. phosphorus trichloride feed pipe, 18. acid binding agent, alkanol feed pipe, 19. ammonia feed pipe, 20. right stirring seat, 21. reaction chamber, 22. exhaust port, 23. left stirring seat, 24. control console. DETAILED DESCRIPTION

[0023] The technical solution of the present utility model is further described clearly and completely below in conjunction with the accompanying drawings.

[0024] See attached Figure 1-2 , the installation and connection of the device, the discharge port 5 is set on one side of the upper part of the reactor shell 1, the venting port 8 is set in the middle of the top, the drain port 22 is set in the middle of the lower part of the reactor shell 1, and the right stirring seat 20 and the left stirring seat 23 are respectively installed in the lower part of the reactor shell 1. The phosphorus trichloride feed pipe 17, the acid binding agent, the alkanol feed pipe 18, and the ammonia feed pipe 19 are installed on the other side of the reactor shell 1 and connected with the reaction chamber 21, the No. 1 regulating control valve 11 and the No. 1 intelligent flow meter 12 are installed on the phosphorus trichloride feed pipe 17, the No. 2 regulating control valve 16 and the No. 2 intelligent flow meter 13 are installed on the acid binding agent and the alkanol feed pipe 18, and the No. 3 regulating control valve 15 and the No. 3 intelligent flow meter 14 are installed on the ammonia feed pipe 19.

[0025] Two mounting frames 6 are installed on the upper part of the reactor shell 1, the left drive assembly 7 and the right drive assembly 9 are respectively installed on the two mounting frames 6, the connecting rod 2 and the blade 3 are respectively installed on the left stirring shaft 4 and the right stirring shaft 10, the left stirring shaft 4 is installed on the left drive assembly 7, and the right stirring shaft 10 is installed on the right drive assembly 9, and the ends of the left stirring shaft 4 and the right stirring shaft 10 are respectively connected to the left stirring seat 23 and the right stirring seat 20.

[0026] The left drive assembly 7, the right drive assembly 9, the No. 1 regulating control valve 11, the No. 1 intelligent flow meter 12, the No. 2 regulating control valve 16, the No. 2 intelligent flow meter 13, the No. 3 regulating control valve 15, and the No. 3 intelligent flow meter 14 are connected to the control console 24 by wires and pipelines respectively.

[0027] Before use, the process parameters of the left drive assembly 7, the right drive assembly 9, the No. 1 regulating control valve 11, the No. 1 intelligent flow meter 12, the No. 2 regulating control valve 16, the No. 2 intelligent flow meter 13, the No. 3 regulating control valve 15, and the No. 3 intelligent flow meter 14 are delivered to the console 24. When in use, the operator starts the left drive assembly 7 and the right drive assembly 9 through the console 24, and the left drive assembly 7 and the right drive assembly 9 respectively drive the left stirring shaft 4 and the right stirring shaft 10 to rotate, and at the same time drive the connecting rod 2 and the blade 3 installed on the left stirring shaft 4 and the right stirring shaft 10 to rotate. Phosphorus trichloride, acid binding agent, alkanol, and ammonia enter the reaction chamber 21 simultaneously through the No. 1 regulating control valve 11, No. 1 intelligent flow meter 12, No. 2 regulating control valve 16, No. 2 intelligent flow meter 13, No. 3 regulating control valve 15, and No. 3 intelligent flow meter 14 installed on the phosphorus trichloride feed pipe 17, acid binding agent, alkanol feed pipe 18, and ammonia feed pipe 19, and are fully stirred by the connecting rod 2 and blades 3 on the rotating right stirring shaft 10, and react while stirring. Figure 1 The mixture moves in the direction of the middle arrow, and the connecting rod 2 and the blade 3 on the left stirring shaft 4 are fully stirred and reacted again. Most of the finished products are discharged through the discharge port 5 and enter the next process. A small amount of finished products are returned to the right stirring shaft 10 for recycling. The gas generated by the reaction is discharged through the vent 8. Therefore, the reactor can operate continuously if the process and equipment conditions allow.

[0028] The No. 1 intelligent flow meter 12, the No. 2 intelligent flow meter 13, and the No. 3 intelligent flow meter 14 are used to measure the amount of raw materials entering, and the No. 1 regulating control valve 11, the No. 2 regulating control valve 16, and the No. 3 regulating control valve 15 are used to control the amount of raw materials added.

[0029] When the reactor is stopped or repaired, the remaining materials in the reaction chamber 21 can be emptied by opening the drain port 22 .

[0030] The above is only a non-limiting implementation method of the utility model, and a large number of embodiments can be derived. For ordinary technicians in this field, without departing from the creative concept of the present invention and without making creative work, several modified and improved embodiments can be made, which all fall within the scope of protection of the present invention.

Claims

1. A reactor for continuously synthesizing trialkyl phosphite by the nitrogen-nitrogen dimethylaniline method, comprising: A reactor shell (1), a discharge port (5), a mounting frame (6), a venting port (8), a No. 1 regulating control valve (11), a No. 1 intelligent flow meter (12), a No. 2 intelligent flow meter (13), a No. 3 intelligent flow meter (14), a No. 3 regulating control valve (15), a No. 2 regulating control valve (16), a phosphorus trichloride feed pipe (17), an acid binding agent, an alkanol feed pipe (18), an ammonia feed pipe (19), a right stirring seat (20), a reaction chamber (21), a drain port (22), a left stirring seat (23), a control console (24), and a stirring mechanism, wherein the stirring mechanism comprises: a connecting rod (2), a blade (3), a left stirring shaft (4), a left drive assembly (7), a right drive assembly (9), and a right stirring shaft (10), characterized in that: the reactor forms a reaction chamber (21) between the reactor shells (1), and the reactor shell (1) has a plurality of upper and lower surfaces. A discharge port (5) is provided on one side of the reactor shell (1), a vent port (8) is provided in the middle of the top, a drain port (22) is provided in the middle of the lower part of the reactor shell (1), a phosphorus trichloride feed pipe (17), an acid binding agent, an alkanol feed pipe (18), and an ammonia feed pipe (19) are installed on the other side of the reactor shell (1) and are connected to the reaction chamber (21), a No. 1 regulating control valve (11) and a No. 1 intelligent flow meter (12) are installed on the phosphorus trichloride feed pipe (17), a No. 2 regulating control valve (16) and a No. 2 intelligent flow meter (13) are installed on the acid binding agent and alkanol feed pipes (18), a No. 3 regulating control valve (15) and a No. 3 intelligent flow meter (14) are installed on the ammonia feed pipe (19), a right stirring seat (20) and a left stirring seat (23) are respectively installed at the lower part of the reactor shell (1), and two sets of stirring mechanisms are respectively installed in the reaction chamber (21).

2. The reactor for continuously synthesizing trialkyl phosphite by the nitrogen-nitrogen dimethylaniline method according to claim 1, characterized in that: The stirring mechanism in the reactor has two mounting frames (6) mounted on the upper part of the reactor shell (1); a left driving assembly (7) and a right driving assembly (9) are mounted on the two mounting frames (6), respectively; a left stirring shaft (4) is mounted on the left driving assembly (7), and a right stirring shaft (10) is mounted on the right driving assembly (9); a connecting rod (2) and a blade (3) are mounted on the left stirring shaft (4) and the right stirring shaft (10), respectively; and the ends of the left stirring shaft (4) and the right stirring shaft (10) are connected to a left stirring seat (23) and a right stirring seat (20), respectively.

3. The reactor for continuously synthesizing trialkyl phosphite by the nitrogen-nitrogen dimethylaniline method according to claim 1, characterized in that: The left drive assembly (7), the right drive assembly (9), the No. 1 regulating control valve (11), the No. 1 intelligent flow meter (12), the No. 2 regulating control valve (16), the No. 2 intelligent flow meter (13), the No. 3 regulating control valve (15), and the No. 3 intelligent flow meter (14) in the reactor are connected to the control console (24) by wires and pipelines, respectively.

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