A recrystallization purification apparatus for preparing triphenyl phosphite and its usage method

Abstract

This invention discloses a recrystallization purification apparatus and its method for preparing triphenyl phosphite. The apparatus includes a crystallization tank for triphenyl phosphite, wherein a filtration section and a crystallization section are arranged sequentially from top to bottom. A transmission assembly is located at the upper part of the crystallization tank, and the transmission assembly passes through the filtration section and the crystallization section sequentially from top to bottom. The triphenyl phosphite solution to be crystallized is introduced into the crystallization tank through the inlet, and passes through the filtration section and the crystallization section in sequence, filtering out impurities in the triphenyl phosphite solution before being guided to the crystallization section for recrystallization. This invention enables double filtration of the triphenyl phosphite solution, and the filter disc can be easily and quickly disassembled for cleaning and replacement of the internal filter screen.

Description

Technical Field

[0001] This invention relates to a recrystallization purification apparatus for preparing triphenyl phosphite and its method of use. Background Technology

[0002] Triphenylphosphite (TPP) is an organophosphorus compound. It is a colorless to pale yellow crystal or powder, insoluble in water at room temperature, but soluble in many organic solvents, such as ethanol and dimethylformamide.

[0003] Triphenyl phosphite has many applications; it is commonly used as a catalyst, reducing agent, and binder in organic synthesis. Because it can react with hydrogen to produce compounds such as triphenylphosphine and alcohols, it is widely used in pharmaceuticals, pesticides, rubber, and resins.

[0004] In addition, triphenyl phosphite can be used to prepare other compounds, such as triphenylphosphine oxide, diphenyl phosphate, and aromatic sulfonyl chloride. In organic synthesis, it can be used as a dehalogenating agent for halogenated hydrocarbons, an addition agent for ketones, and a dehalogenating agent for alkyl halides.

[0005] Recrystallization of triphenyl phosphite can remove impurities and impurities, thereby improving the purity of the compound. High-purity triphenyl phosphite can be used to prepare other compounds or as a catalyst, ensuring the effectiveness and reliability of the reaction.

[0006] Existing recrystallization devices for triphenyl phosphite on the market have complex structures, requiring transfer and batch operation, which affects the recrystallization efficiency of triphenyl phosphite. In addition, they need to be disassembled and cleaned, which is quite troublesome. Therefore, a recrystallization and purification device for preparing triphenyl phosphite and its usage method are proposed. Summary of the Invention

[0007] The purpose of this invention is to provide a recrystallization purification apparatus for preparing triphenyl phosphite and a method for using it, so as to solve the problems mentioned in the background art.

[0008] To solve the above-mentioned technical problems, the present invention provides the following technical solution: a recrystallization purification apparatus for preparing triphenyl phosphite, comprising a crystallization tank for triphenyl phosphite, wherein a filtration section and a crystallization section are arranged sequentially from top to bottom in the crystallization tank, and a transmission assembly is arranged in the upper part of the crystallization tank, the transmission assembly passing through the filtration section and the crystallization section sequentially from top to bottom.

[0009] The triphenyl phosphite solution to be crystallized is introduced into the crystallization tank through the inlet, and then passes through the filtration section and the crystallization section in sequence. After filtering out the impurities inside the triphenyl phosphite solution, it is then sent to the crystallization section for recrystallization.

[0010] Preferably, the filtration section includes a filter cylinder disposed in the crystallization tank, the bottom of the filter cylinder is provided with a bottom plate, and the two sides of the bottom plate are provided with mesh plates. The mesh plates are fan-shaped and have a plurality of mesh holes on their surface.

[0011] Preferably, filter elements are provided on both sides below the base plate. The filter elements include a filter disc located directly below the mesh plate. A frame groove is provided in the middle of the filter disc, and a filter screen is provided inside the frame groove.

[0012] Preferably, the filter disc has an inner cavity, a spring is connected in the inner cavity, a top pressure plate is provided below the spring, a positioning rod is connected to the bottom end of the top pressure plate, and a lever for adjusting the position of the positioning rod is connected to one side of the positioning rod.

[0013] Preferably, a sliding groove for sliding the lever is provided on one side of the filter disc.

[0014] Preferably, the filter tank has channels on both sides for connecting filter elements, and one side of the channel has a positioning hole that cooperates with the positioning rod.

[0015] Preferably, the crystallization section includes a crystallization cylinder disposed in the crystallization tank, the lower part of the crystallization cylinder is rounded arc-shaped, and a discharge port is opened in the middle of the crystallization cylinder.

[0016] Preferably, the transmission assembly includes a motor disposed on the upper part of the crystallization tank, the output end of the motor being connected to the input end of a rotating shaft, the rotating shaft extending from the filter cylinder into the crystallization tank;

[0017] A shaft cylinder is provided on the outer periphery of the rotating shaft located in the filter cylinder. The two sides of the shaft cylinder are connected to the stirring plate through connecting rods, and the connecting rods are in the shape of "L". The stirring plate is attached to the surface of the bottom plate.

[0018] A sleeve is provided around the outer periphery of the rotating shaft located in the crystallization cylinder, and a sealing cylinder is provided around the sleeve. The sealing cylinder is connected to a scraper rod through a support rod, and the scraper rod is attached to the inner wall of the crystallization cylinder.

[0019] Preferably, a sealing plug is provided on the side of the support rod away from the scraper rod, and the sealing plug is located inside the sealing cylinder.

[0020] Preferably, the bottom of the crystallization tank is provided with support legs around its perimeter, and an observation hole is provided on the outer side of the crystallization tank.

[0021] A method for using a recrystallization purification apparatus for preparing triphenyl phosphite includes the following steps:

[0022] Step (A): The triphenyl phosphite solution to be crystallized is introduced into the filter cylinder of the crystallization tank through the feed port at the top of the tank, and then the motor is started;

[0023] Step (B): The motor drives the connecting rod on the outer periphery of the bushing to rotate through the rotating shaft. The connecting rod stirs and mixes the triphenyl phosphite solution in the filter tube evenly through the stirring rod, so that the solution is discharged through the screen plate. Large particles of impurities or undissolved triphenyl phosphite are filtered out by the screen plate, thus achieving coarse filtration.

[0024] Step (C): The triphenyl phosphite solution is introduced into the filter tray along the mesh plate and then filtered through the filter screen in the filter tray to achieve secondary filtration.

[0025] Step (D): The triphenyl phosphite solution after secondary filtration is guided into the crystallization cylinder by gravity. At the same time, the rotating shaft drives the surrounding support rods to rotate through the sleeve. The support rods stir the solution by scraping the material against the inner wall of the crystallization cylinder. The high heat in the crystallization cylinder evaporates the solution, completing the recrystallization of triphenyl phosphite.

[0026] Step (E): Then open the discharge port located at the bottom of the crystallizer to discharge the recrystallized triphenyl phosphite;

[0027] Step (F): After the recrystallization process is completed, pull up the lever to move the top pressure plate in the inner cavity to compress the spring, so that the positioning rod moves out of the positioning hole and disconnects the filter plate from the crystallization tank.

[0028] Step (G): Remove the filter disc from the channel, clean and replace the filter screen, and then reset the filter disc.

[0029] Compared with the prior art, the beneficial effects of the present invention are:

[0030] This invention, through its filtration and crystallization sections, enables dual filtration of triphenyl phosphite solutions. Furthermore, the filter disc can be easily and quickly disassembled, facilitating the cleaning and replacement of the internal filter screen.

[0031] Compared to traditional split designs, which require transferring the triphenyl phosphite solution, making the operation cumbersome and prone to dust contamination during transfer, thus affecting the purity of the triphenyl phosphite, this invention adopts an integrated design. After filtration, the triphenyl phosphite solution is transferred to the crystallization cylinder by gravity. The heat generated by the resistance within the crystallization cylinder enables rapid crystallization of the triphenyl phosphite solution. Simultaneously, the crystallized particles slide along the cylinder wall to the discharge port, achieving rapid discharge. Attached Figure Description

[0032] Figure 1 This is a schematic diagram of the overall structure of an embodiment of the present invention;

[0033] Figure 2 This is a partial cross-sectional structural diagram of an embodiment of the present invention;

[0034] Figure 3 This is an enlarged schematic diagram of the structure at point A in an embodiment of the present invention;

[0035] Figure 4 This is a schematic diagram of the internal structure of an embodiment of the present invention;

[0036] Figure 5 This is an enlarged schematic diagram of the structure at point B in an embodiment of the present invention;

[0037] Figure 6 This is a schematic diagram of a half-section structure according to an embodiment of the present invention;

[0038] Figure 7 This is an enlarged schematic diagram of the structure at point C in an embodiment of the present invention;

[0039] Figure 8 This is a schematic diagram of the filter section structure according to an embodiment of the present invention;

[0040] Figure 9 This is a schematic diagram of the filter disc structure according to an embodiment of the present invention.

[0041] In the diagram: 1. Crystallization tank; 101. Filter section; 1011. Filter cylinder; 1012. Bottom plate; 1013. Mesh plate; 102. Crystallization section; 103. Observation hole; 104. Support leg; 105. Discharge port; 106. Positioning hole; 2. Transmission assembly; 201. Motor; 202. Rotary shaft; 203. Shaft cylinder; 204. Connecting rod; 205. Stirring plate; 206. Sleeve; 207. Sealing cylinder; 208. Support rod; 2081. Sealing plug; 209. Scraper rod; 3. Filter element; 301. Filter disc; 302. Inner cavity; 303. Spring; 304. Top pressure plate; 3041. Actuating rod; 305. Positioning rod; 306. Moving groove; 307. Frame groove; 308. Filter screen; 4. Crystallization cylinder. Detailed Implementation

[0042] To address the problems of complex structures in existing recrystallization devices for triphenyl phosphite, which affect recrystallization efficiency and require disassembly and cleaning, resulting in cumbersome subsequent cleaning, this invention provides a recrystallization and purification device for preparing triphenyl phosphite and its usage method. The technical solution of this invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described invention is only a part of this invention, not all of it. All other inventions obtained by those skilled in the art based on this invention without inventive effort are within the scope of protection of this invention.

[0043] Please see Figure 1-8 This invention provides a recrystallization purification apparatus for preparing triphenyl phosphite, comprising a crystallization tank 1 for preparing triphenyl phosphite. The crystallization tank 1 has a filtration section 101 and a crystallization section 102 arranged sequentially from top to bottom. A transmission assembly 2 is arranged at the upper part of the crystallization tank 1, and the transmission assembly 2 passes through the filtration section 101 and the crystallization section 102 sequentially from top to bottom.

[0044] The triphenyl phosphite solution to be crystallized is introduced into the crystallization tank 1 through the inlet, and then passes through the filter section 101 and the crystallization section 102 in sequence. After filtering out the impurities inside the triphenyl phosphite solution, it is guided to the crystallization section 102 for recrystallization.

[0045] The further filtration section 101 includes a filter cylinder 1011 disposed in the crystallization tank 1. A bottom plate 1012 is disposed at the bottom of the filter cylinder 1011. Mesh plates 1013 are disposed on both sides of the bottom plate 1012. The mesh plates 1013 are fan-shaped and have a plurality of mesh holes on their surface.

[0046] Further, filter elements 3 are provided on both sides below the bottom plate 1012. The filter elements 3 include a filter disc 301 located directly below the mesh plate 1013. A frame groove 307 is provided in the middle of the filter disc 301, and a filter screen 308 is provided inside the frame groove 307.

[0047] The filter disc 301 further has an inner cavity 302 inside, a spring 303 is connected in the inner cavity 302, a top pressure plate 304 is provided below the spring 303, a positioning rod 305 is connected to the bottom end of the top pressure plate 304, and a lever 3041 for adjusting the position of the positioning rod 305 is connected to one side of the positioning rod 305.

[0048] Furthermore, a movable groove 306 is provided on one side of the filter disc 301 for sliding the lever 3041.

[0049] Furthermore, channels for connecting filter elements 3 are provided on both sides of the filter tank, and a positioning hole 106 that cooperates with the positioning rod 305 is provided on one side of the channel.

[0050] The further crystallization section 102 includes a crystallization cylinder 4 disposed in the crystallization tank 1. The lower part of the crystallization cylinder 4 is rounded and arc-shaped, and a discharge port 105 is provided in the middle of the crystallization cylinder 4.

[0051] The further transmission component 2 includes a motor 201 disposed on the upper part of the crystallization tank 1. The output end of the motor 201 is connected to the input end of the rotating shaft 202, which extends from the filter cartridge 1011 into the crystallization cylinder 4.

[0052] A shaft cylinder 203 is provided on the outer periphery of the rotating shaft 202 located in the filter cylinder 1011. The two sides of the shaft cylinder 203 are connected to the stirring plate 205 through the connecting rod 204, and the connecting rod 204 is in the shape of "L". The stirring plate 205 is attached to the surface of the bottom plate 1012.

[0053] Furthermore, a sleeve 206 is provided on the outer periphery of the rotating shaft 202 located in the crystallization cylinder 4, and a sealing cylinder 207 is provided around the sleeve 206. The sealing cylinder 207 is connected to a scraper rod 209 through a support rod 208, and the scraper rod 209 is attached to the inner wall of the crystallization cylinder 4.

[0054] A sealing plug 2081 is provided on the side of the support rod 208 away from the scraper rod 209, and the sealing plug 2081 is located inside the sealing cylinder 207.

[0055] Furthermore, support legs 104 are provided around the bottom of the crystallization tank 1, and observation holes 103 are provided on the outside of the crystallization tank 1.

[0056] A method for using a recrystallization purification apparatus for preparing triphenyl phosphite includes the following steps:

[0057] Step (A): The triphenyl phosphite solution to be crystallized is introduced into the filter cartridge 1011 of the crystallization tank 1 through the feed port at the top of the tank, and then the motor 201 is started;

[0058] Step (B): The motor 201 drives the connecting rod 204 on the outer periphery of the bushing to rotate through the rotating shaft 202. The connecting rod 204 stirs and mixes the triphenyl phosphite solution in the filter cylinder 1011 evenly through the stirring rod, so that the solution is discharged through the screen plate 1013. Large particles of impurities or undissolved triphenyl phosphite are filtered out by the screen plate 1013, thus achieving coarse filtration.

[0059] Step (C): The triphenyl phosphite solution is introduced through the mesh plate 1013 into the filter plate 301, and then filtered through the filter screen 308 in the filter plate 301 to achieve secondary filtration.

[0060] Step (D): The triphenyl phosphite solution after secondary filtration is guided into the crystallization cylinder 4 by gravity. At the same time, the rotating shaft 202 drives the surrounding support rods 208 to rotate through the sleeve 206. The support rods 208 stir the solution by scraping the material rods 209 against the inner wall of the crystallization cylinder 4. The high heat in the crystallization cylinder 4 evaporates the solution, completing the recrystallization of triphenyl phosphite.

[0061] Step (E): Then open the discharge port 105 located at the bottom of the crystallizer 4 to discharge the recrystallized triphenyl phosphite;

[0062] After step (F) recrystallization is completed, pull up lever 3041 to move top pressure plate 304 in inner cavity 302 to compress spring 303, so that positioning rod 305 moves out of positioning hole 106 and disconnects filter plate 301 from crystallization tank 1.

[0063] Step (G): Remove the filter disc 301 from the channel, clean and replace the filter screen 308, and then reset the filter disc 301.

[0064] The recrystallization purification apparatus for preparing triphenyl phosphite and its method of use, as disclosed in this invention, have the following advantages:

[0065] The present invention, through the filtration section 101 and the crystallization section 102, can perform dual filtration of triphenyl phosphite solution. Simultaneously, the filter disc 301 can be easily and quickly disassembled, facilitating the cleaning and replacement of its internal filter screen 308.

[0066] Compared to the traditional split design, which requires transferring the triphenyl phosphite solution, making the operation cumbersome and prone to dust contamination during the transfer process, thus affecting the purity of the triphenyl phosphite, this invention adopts an integrated design. After filtration, the triphenyl phosphite solution is transferred to the crystallization cylinder 4 by gravity. The heat generated by the resistance in the crystallization cylinder 4 enables rapid crystallization of the triphenyl phosphite solution. At the same time, the crystallized particles slide along the wall of the crystallization cylinder 4 to the discharge port 105, enabling rapid discharge.

[0067] Although the invention has been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made to these inventions without departing from the principles and spirit of the invention, the scope of which is defined by the appended claims and their equivalents.

Claims

1. A recrystallization and purification apparatus for preparing triphenyl phosphite, characterized in that: The crystallization tank (1) for triphenyl phosphite is provided with a filter section (101) and a crystallization section (102) arranged sequentially from top to bottom. A transmission assembly (2) is provided at the upper part of the crystallization tank (1), and the transmission assembly (2) passes through the filter section (101) and the crystallization section (102) sequentially from top to bottom. The filter section (101) includes a filter cylinder (1011) disposed in the crystallization tank (1). A bottom plate (1012) is provided at the bottom of the filter cylinder (1011). Mesh plates (1013) are provided on both sides of the bottom plate (1012). The mesh plates (1013) are fan-shaped and have several mesh holes on their surface. Filter elements () are provided on both sides below the bottom plate (1012). 3) The filter element (3) includes a filter disc (301) disposed directly below the mesh plate (1013). A frame groove (307) is provided in the middle of the filter disc (301), and a filter screen (308) is disposed inside the frame groove (307). An inner cavity (302) is provided inside the filter disc (301), and a spring (303) is connected in the inner cavity (302). A top pressure plate (304) is provided below the spring (303), and a positioning rod (305) is connected to the bottom end face of the top pressure plate (304). A lever (3041) for adjusting the position of the positioning rod (305) is connected to one side of the positioning rod (305). A moving groove (306) for sliding the lever (3041) is provided on one side of the filter disc (301). The crystallization tank (1) has channels on both sides for connecting the filter element (3), and a positioning hole (106) that cooperates with the positioning rod (305) is provided on one side of the channel. The triphenyl phosphite solution to be crystallized is introduced into the crystallization tank (1) through the inlet and passes through the filter section (101) and the crystallization section (102) in sequence. The impurities inside the triphenyl phosphite solution are filtered and then sent to the crystallization section (102) for recrystallization.

2. The recrystallization and purification apparatus for preparing triphenyl phosphite according to claim 1, characterized in that: The crystallization section (102) includes a crystallization cylinder (4) disposed in the crystallization tank (1). The lower part of the crystallization cylinder (4) is rounded and arc-shaped, and a discharge port (105) is provided in the middle of the crystallization cylinder (4).

3. The recrystallization and purification apparatus for preparing triphenyl phosphite according to claim 2, characterized in that: The transmission assembly (2) includes a motor (201) disposed on the upper part of the crystallization tank (1), the output end of the motor (201) is connected to the input end of a rotating shaft (202), and the rotating shaft (202) extends from the filter cylinder (1011) into the crystallization cylinder (4); A shaft cylinder (203) is provided on the outer periphery of the rotating shaft (202) located in the filter cylinder (1011). The two sides of the shaft cylinder (203) are connected to the stirring plate (205) through connecting rods (204), and the connecting rods (204) are in the shape of "L". The stirring plate (205) is attached to the surface of the bottom plate (1012). A sleeve (206) is provided on the outer periphery of the rotating shaft (202) located in the crystallizing cylinder (4). A sealing cylinder (207) is provided around the sleeve (206). A scraper rod (209) is connected to the sealing cylinder (207) through a support rod (208). The scraper rod (209) is attached to the inner wall of the crystallizing cylinder (4). A sealing plug (2081) is provided on the side of the support rod (208) away from the scraper rod (209), and the sealing plug (2081) is located inside the sealing cylinder (207).

4. The recrystallization and purification apparatus for preparing triphenyl phosphite according to claim 3, characterized in that: The bottom of the crystallization tank (1) is provided with support legs (104) around its perimeter, and an observation hole (103) is provided on the outside of the crystallization tank (1).

5. A method of using the recrystallization and purification apparatus for preparing triphenyl phosphite according to any one of claims 1-4, characterized in that: Includes the following steps: Step (A): The triphenyl phosphite solution to be crystallized is introduced into the filter cartridge (1011) of the crystallization tank (1) through the feed port at the top of the tank, and then the motor (201) is started. Step (B): The motor (201) drives the connecting rod (204) on the outer periphery of the bushing to rotate through the rotating shaft (202). The connecting rod (204) stirs and mixes the triphenyl phosphite solution in the filter cylinder (1011) evenly through the stirring rod, so that the solution is discharged through the screen plate (1013). Large particles of impurities or undissolved triphenyl phosphite are filtered out by the screen plate (1013), thus achieving coarse filtration. Step (C): The triphenyl phosphite solution is exported through the mesh plate (1013) and introduced into the filter plate (301) along the mesh plate (1013). It passes through the filter screen (308) in the filter plate (301) to achieve secondary filtration. Step (D): The triphenyl phosphite solution after secondary filtration is guided into the crystallization cylinder (4) by gravity. At the same time, the rotating shaft (202) drives the surrounding support rods (208) to rotate through the sleeve (206). The support rods (208) stir the solution by adhering to the inner wall of the crystallization cylinder (4) through the scraper rod (209). The high heat in the crystallization cylinder (4) evaporates the solution, completing the recrystallization of triphenyl phosphite. Step (E): Then open the discharge port (105) located at the bottom of the crystallization cylinder (4) to discharge the recrystallized triphenyl phosphite; After step (F) recrystallization is completed, pull up the lever (3041) to move the top pressure plate (304) in the inner cavity (302) to squeeze the spring (303), so that the positioning rod (305) moves out of the positioning hole (106) and disconnects the filter plate (301) from the crystallization tank (1); Step (G): Remove the filter disc (301) from the channel, clean and replace the filter screen (308) therein, and then reset the filter disc (301).

Images