Sampling detection device prepared based on 2, 4, 5-trifluorophenylacetic acid and method thereof

Abstract

The invention discloses a sampling detection device prepared based on 2, 4, 5-trifluorophenylacetic acid and a method thereof, and relates to the technical field of sampling detection. The device comprises a base, a reaction assembly is arranged on the left side of the top of the base, an air inlet assembly is arranged on the top of the reaction assembly, six reaction plates are arranged in the reaction assembly, catalytic lamps are arranged in the six reaction plates, a conveying assembly is arranged on the right side of the reaction assembly, and a detection assembly is arranged on the right side of the top of the base. The top of the detection assembly is provided with an extraction assembly. In the vertical movement process of the decomposition vessel, a finished product material is effectively prevented from being centered and accumulated at a fixed point, the material can be conveniently soaked by a solvent, meanwhile, the material can be accelerated to be fully dissolved in the solvent when the filter plate rotates, and it is guaranteed that components contained in extracted liquid are uniform; the situation that the detection precision is reduced due to the fact that the detection result error is large when sample liquid is detected is avoided.

Description

Technical Field

[0001] The present invention relates to the field of sampling detection technology, and in particular to a sampling detection device and method based on the preparation of 2,4,5-trifluorophenylacetic acid. Background Art

[0002] 2,4,5-Trifluorophenylacetic acid is usually a white crystalline solid or a white to off-white solid, and the solubility of 2,4,5-trifluorophenylacetic acid in water is low. At the same time, 2,4,5-trifluorophenylacetic acid is an important intermediate for the synthesis of the antidiabetic drug sitagliptin. It has good efficacy, few side effects, good safety and tolerance in the treatment of diabetes, and has broad market prospects.

[0003] Patent announcement number CN214584234U discloses a sampling and detection device based on the preparation of methyl oxyphenylacetate, including a box body, a cover plate and a sampling mechanism, the cover plate is located at the upper end of the box body, the sampling mechanism is fixedly installed inside the right side of the box body, the second card slot is opened at the upper right end of the box body, the second card slot is located above the first channel, the liquid storage tank is located below the first channel, a transparent glass is fixedly installed on the right side of the liquid storage tank, and a scale line is engraved on the outer end of the glass. The upper left end of the liquid storage tank is connected to the lower right end of the liquid storage tank through the second channel, and the lower end of the liquid storage tank is connected to a control mechanism. The lower end surface of the right side of the cover plate is fixedly connected to a second snap ring matching the second card slot, and a third channel is installed on the upper end of the second snap ring. A one-way valve is fixedly installed in the middle end of the third channel, and an air bag is fixedly connected to the top of the third channel. The staff observes the scale on the transparent glass on the right side of the liquid storage tank to quantitatively and accurately sample the liquid.

[0004] However, the device currently has some shortcomings: the device prompts staff to achieve accurate sampling by observing the scale, but it is difficult to sample and test solid materials after dissolving them with a solvent, resulting in certain limitations in the detection type, and it is difficult to disturb the sample so that it is fully dissolved in the solvent when testing the sample, which in turn leads to increased errors in the test results. Summary of the invention

[0005] In view of the shortcomings of the prior art, the present invention provides a sampling and detection device and method based on the preparation of 2,4,5-trifluorophenylacetic acid, which solves the problems raised in the above background technology.

[0006] To achieve the above object, the present invention is implemented by the following technical scheme: a sampling and detection device based on the preparation of 2,4,5-trifluorophenylacetic acid, comprising a base, a reaction assembly is arranged on the left side of the top of the base, an air intake assembly is arranged on the top of the reaction assembly, six reaction plates are arranged inside the reaction assembly, and catalytic lamps are arranged inside the six reaction plates, a conveying assembly is arranged on the right side of the reaction assembly, a detection assembly is arranged on the right side of the top of the base, an extraction assembly is arranged on the top of the detection assembly, and the left side of the extraction assembly is connected and fixedly installed on the right side of the top of the conveying assembly; An anti-error device is provided inside the extraction component, an anti-solidification device is provided above the anti-error device, and an anti-delay device is provided inside the anti-solidification device; The anti-error device comprises an electric telescopic rod, the bottom of which is fixedly mounted at the bottom edge of the inner wall of the extraction component, a fine-mesh plate is fixedly mounted on the outer wall of the fixed end of the electric telescopic rod, a decomposition dish is fixedly mounted on the top of the telescopic end of the electric telescopic rod, a plurality of electric doors are hinged at the bottom of the decomposition dish, an electric rotating rod is rotatably mounted at the bottom center of the inner wall of the decomposition dish, a plurality of filter plates are fixedly mounted on the outer wall of the electric rotating rod, a U-shaped groove is provided at the bottom of the filter plate, a round rod is fixedly mounted on the inner wall of the U-shaped groove of the filter plate, friction rings are fixedly mounted on the outer walls of the round rods at both ends away from the axis of the filter plate, a spiral mesh plate is fixedly mounted on the outer wall of the round rod, and before the finished material enters the interior of the extraction component, the electric telescopic rod is started, and the telescopic end of the electric telescopic rod drives the decomposition dish to move back and forth up and down, and at the same time, the electric telescopic rod is fixed The fine-pored mesh plate is limited and stationary at the end, and the finished material falling from the extraction component is received by the decomposition dish during the reciprocating up and down movement. At the same time, the solvent is injected into the extraction component and then falls into the decomposition dish and soaks the finished material. At the same time, the electric rotating rod is started. When the electric rotating rod rotates, it drives the filter plate to rotate and stirs the material and solvent inside the decomposition dish. After the decomposition is completed, the staff remotely controls the electric door to open through the electronic module. The electric door flips downward with the hinge axis as the axis to cause the liquid inside the decomposition dish to fall, and the fine-pored mesh plate blocks the material residue, and the detection liquid falls and is discharged; when the filter plate revolves, it drives the round rod to revolve, and the round rod drives the friction ring to revolve and rub along the bottom of the inner wall of the decomposition dish and generate a rotational force. When the friction ring rotates, it drives the round rod to rotate along the inner wall of the U-shaped groove of the filter plate, and the round rod drives the spiral mesh plate to rotate.

[0007] According to the above technical solution, the plurality of filter plates are equidistantly distributed on the outer wall of the electric rotating rod, the outer wall of the friction ring contacts the bottom of the inner wall of the decomposition dish, and the spiral mesh plate is located on the side of the friction ring close to the axis of the filter plate.

[0008] According to the above technical scheme, the anti-curing device includes a friction wheel, a reciprocating screw, a transmission ring and a U-shaped scraper, the bottom of the friction wheel is rotatably installed on the top of one end of the filter plate close to the inner wall of the decomposition dish, the bottom of the reciprocating screw is rotatably installed at the center of the top of the friction wheel, the transmission ring penetrates inside and is movably installed on the outer wall of the reciprocating screw, and the U-shaped scraper is fixedly installed on the outer wall of the transmission ring away from the electric rotating rod. When the filter plate revolves, it drives the friction wheel to revolve, and when the friction wheel revolves along the inner wall of the decomposition dish, friction is generated. At this time, the friction wheel starts to rotate along the top of the filter plate through the friction force, and drives the reciprocating screw to rotate when the friction wheel rotates. When the reciprocating screw rotates, it limits the built-in block of the transmission ring through the reciprocating spiral groove on its outer wall, and drives the transmission ring to slide down and reset along the outer wall of the reciprocating screw through the reciprocating spiral groove. The transmission ring drives the U-shaped scraper to slide down and reset along the outer wall of the filter plate. In the process that the U-shaped scraper gradually covers the outer wall of the filter plate, the movement resistance between the filter plate and the solvent will gradually increase, and the U-shaped scraper scrapes the filter plate.

[0009] According to the above technical solution, the outer wall of the friction wheel contacts the inner wall of the decomposition dish, and the inner wall of the U-shaped scraper is slidably connected to the outer wall of the filter plate.

[0010] According to the above technical scheme, the anti-curing device also includes a hollow plate, an arc plate, a vertical rod and a bent plate, the end of the hollow plate away from the inner wall of the decomposition dish is hinged to the outer wall of the U-shaped scraper through a torsion spring, the arc plate is hinged to the end of the hollow plate close to the inner wall of the decomposition dish near the electric rotating rod, the outer wall of the arc plate contacts the inner wall of the decomposition dish, both ends of the vertical rod are fixedly installed inside the hollow plate, the bent plate passes through and is fixedly installed on the outer wall of the vertical rod, the U-shaped scraper revolves and moves vertically up and down, driving the hollow plate to move synchronously, the hollow plate drives the arc plate to move synchronously along the inner wall of the decomposition dish, the arc plate is pushed by the hollow plate to cause its own hinge axis to start rotating, at this time the arc plate rotates with the hinge axis as the axis and is adjusted to a suitable sliding angle, the subsequent arc plate removes the finished product powder attached to the inner wall of the decomposition dish due to the centrifugal force of the filter plate rotation, and at the same time the hollow plate drives the vertical rod to move synchronously, the vertical rod drives the bent plate to move synchronously, and the bent plate expands the contact area between the solvent and the finished product through its own arc surface.

[0011] According to the above technical scheme, the anti-delay device includes a heating component, a pressure plate, a positioning plate, a transmission rod and a plurality of heat-conducting plates. The back of the heating component is fixedly installed on the outer wall of the U-shaped scraper, the bottom of the pressure plate close to the outer wall of the filter plate is fixedly installed on the top of the U-shaped scraper, the bottom of the positioning plate close to the center of the decomposition dish is fixedly installed on the top edge of the electric rotating rod, the top of the transmission rod is fixedly installed on the bottom edge of the positioning plate, and a plurality of heat-conducting plates are fixedly installed on the outer wall of the transmission rod. When the U-shaped scraper revolves and moves downward, it drives the heating component to move synchronously, thereby expanding the movement range of the heating component. At the same time, the heating component drives the pressure plate to move synchronously. When the pressure plate moves downward, it will slide downward along the outer wall of the transmission rod. At this time, the positioning plate limits the transmission rod. When the pressure plate slides, it drives the spirally connected transmission rod to generate a rotating force and start to rotate. When the transmission rod rotates, it drives the heat-conducting plate to rotate. When the heat-conducting plate rotates, it disturbs the solvent around the heating component.

[0012] According to the above technical solution, the outer wall of the transmission rod passes through and is threadedly connected to the inside of the pressure plate, a plurality of the heat conducting plates are equidistantly distributed on the outer wall of the transmission rod, and a slide groove begins to be formed on the outer wall of the heat conducting plate.

[0013] The cam is secured to the bottom of the heat exchanger and is located adjacent to the bottom of the heat exchanger when the friction between the rollers is greater than the limit of the spring.

[0014] A sampling and detection method for a sampling and detection device prepared based on 2,4,5-trifluorophenylacetic acid comprises the following steps: S1: firstly, 2,4,5-trifluorotoluene is used as a raw material, chlorine is used as a chlorinating agent, and photocatalytic chloromethylation is performed inside a reaction component to synthesize 2,4,5-trifluorobenzyl chloride. Then, 2,4,5-trifluorobenzyl chloride is reacted with a cyanating agent inside the reaction component to obtain 2,4,5-trifluorophenylacetonitrile. Finally, 2,4,5-trifluorophenylacetonitrile is hydrolyzed inside the reaction component to obtain 2,4,5-trifluorophenylacetic acid. S2: During the reaction process, the reaction component is a Corning microchannel reactor, and the catalytic lamps in the center of the six reaction plates inside are 100 W for the first and fifth lamps, and 250 W for the three in the middle. Then, when feeding, chlorine is introduced into the first reaction plate through the air intake component, and the amount of chlorine is manually controlled. After the finished product is manufactured, the finished product is transported to the inside of the extraction component through the conveying component, and the solvent is injected into the inside of the extraction component through the top pipe of the extraction component to dissolve the finished product. Then, the extraction component drips the solution to be tested on the top of the detection component through the bottom dropper for purity detection; S3: Before the finished material enters the extraction component, the electric telescopic rod is started, and the telescopic end of the electric telescopic rod drives the decomposition dish to move up and down reciprocatingly. At the same time, the fixed end of the electric telescopic rod limits the fine-pore mesh plate to be stationary. During the reciprocating up and down movement of the decomposition dish, the finished material falling from the extraction component is received; S4: At the same time, the solvent is injected into the extraction component and then falls into the decomposition dish and soaks the finished material. At the same time, the electric rotating rod is started. When the electric rotating rod rotates, it drives the filter plate to rotate and stirs the material and solvent inside the decomposition dish. After the decomposition is completed, the staff remotely controls the electric door to open through the electronic module. The electric door flips downward with the hinge axis as the axis to make the liquid inside the decomposition dish fall, and the fine-pored mesh plate blocks the material residue, and the detection liquid falls and is discharged.

[0015] The present invention provides a sampling detection device and method based on the preparation of 2,4,5-trifluorophenylacetic acid. It has the following beneficial effects: (1) The present invention, through the setting of the error prevention device, cooperates with the electric telescopic rod, the fine mesh plate, the decomposition dish, the electric door, the electric rotating rod, the filter plate, the round rod, the friction ring and the spiral mesh plate, effectively avoids the finished material from being centered and piled up at a fixed point during the vertical movement of the decomposition dish, and facilitates the solvent to soak the material. At the same time, when the filter plate rotates, the material is accelerated to be fully dissolved in the solvent, ensuring that the components contained in the extracted liquid are relatively uniform, avoiding large errors in the test results when the sample liquid is tested, thereby reducing the detection accuracy; at the same time, the spiral mesh plate is used to spirally stir the material precipitated at the bottom of the inner wall of the decomposition dish, so that the undissolved precipitated material is stirred by the spiral mesh plate to reduce the viscosity with the bottom of the inner wall of the decomposition dish, so that it is convenient to dissolve again in the solvent under the flushing of the solvent, and further ensure that the material can be fully dissolved in the solvent on the original basis, preventing the material residue from remaining and avoiding the increase of the detection accuracy error due to equipment reasons.

[0016] (2) The present invention adopts the setting of the anti-solidification device, and cooperates with the filter plate, friction wheel, reciprocating screw, transmission ring, U-shaped scraper, hollow plate, arc plate, vertical rod and bent plate. The U-shaped scraper is used to scrape the finished product powder remaining on the surface of the filter plate to avoid the powder residue from filling the filter holes. Then, the filter plate is covered with the U-shaped scraper, so that no solvent passes through the filter holes of the filter plate, and the scouring force between the two is reduced, so that the bubbles generated during the revolution of the filter plate gradually explode to avoid the bubbles containing finished product powder to reduce the purity of the solvent, and to avoid excessive accumulation of bubbles to produce foam; and the arc plate is used to scrape the residue attached to the inner wall of the decomposition dish, so that the residue after the reaction between the solvent and the finished product is completed is discharged from the decomposition dish in time and falls to the top of the fine-pore mesh plate, so as to avoid the solidification of the residue and prevent the chemical components in the residue from continuously corroding the decomposition dish and affecting the next detection result; and the curved surface of the bent plate is used to guide the solvent and the finished product to be more fully contacted and mixed at the same rotation frequency.

[0017] (3) The present invention adopts the setting of the anti-delay device, and cooperates with the U-shaped scraper, the heating component, the pressure plate, the positioning plate, the transmission rod, the heat conducting plate, the sliding plate, the fixing block, the cross bar and the friction roller. The heat conducting plate increases the frequency of the solvent moving toward the heating component within the same reaction time, so that the solvent can be heated evenly and quickly heated up, thereby optimizing the plasma reaction of the material ion source and the solvent, improving the sensitivity and accuracy of the detection, and effectively shortening the waiting time of the precipitation to be detected; at the same time, the friction roller is used to rotate and brush away the powder residue attached to the outer wall of the heat conducting plate, so as to ensure the cleanliness of the outer wall of the heat conducting plate, avoid the outer wall of the heat conducting plate being covered with powder residue, thereby reducing the thermal conductivity of the heat conducting plate, and avoid uneven temperature rise of the solvent inside the decomposition dish, resulting in the overall temperature difference of the solvent, thereby affecting the plasma reaction, causing the detection result to change frequently and it is difficult to obtain an accurate average value. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] Figure 1 A schematic diagram of the present invention as a whole; Figure 2 It is a schematic diagram of the internal structure of the present invention as a whole; Figure 3 It is a schematic diagram of the error prevention device of the present invention; Figure 4 This is a schematic diagram of the error prevention device of the present invention from a top perspective; Figure 5 It is a schematic diagram of the anti-curing device of the present invention; Figure 6 It is a schematic diagram showing the overall structure of the anti-curing device of the present invention; Figure 7 It is a schematic diagram of the anti-delay device of the present invention; Figure 8 It is a schematic diagram showing the overall structure of the anti-delay device of the present invention.

[0019] In the figure: 1. base; 2. reaction component; 21. air intake component; 22. reaction plate; 23. catalytic lamp; 3. conveying component; 31. detection component; 32. extraction component; 4. error prevention device; 41. electric telescopic rod; 42. fine mesh plate; 43. decomposition dish; 44. electric door; 45. electric rotating rod; 46. filter plate; 47. round rod; 48. friction ring; 49. spiral mesh plate; 5. anti-curing device; 51. friction wheel; 52. reciprocating screw rod; 53. transmission ring; 54. U-shaped scraper; 55. hollow plate; 56. arc plate; 57. vertical rod; 58. bending plate; 6. anti-delay device; 61. heating component; 62. pressure plate; 63. positioning plate; 64. transmission rod; 65. heat conduction plate; 66. sliding plate; 67. fixed block; 68. cross bar; 69. friction roller. DETAILED DESCRIPTION

[0020] The technical solutions in the embodiments of the present invention will be described clearly and completely below in conjunction with the drawings in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, rather than all the embodiments.

[0021] See also Figure 1-Figure 8 One embodiment of the present invention is: a sampling and detection device based on the preparation of 2,4,5-trifluorophenylacetic acid, comprising a base 1, a reaction assembly 2 is arranged on the left side of the top of the base 1, an air intake assembly 21 is arranged on the top of the reaction assembly 2, six reaction plates 22 are arranged inside the reaction assembly 2, and catalytic lamps 23 are arranged inside the six reaction plates 22, a conveying assembly 3 is arranged on the right side of the reaction assembly 2, a detection assembly 31 is arranged on the right side of the top of the base 1, an extraction assembly 32 is arranged on the top of the detection assembly 31, and the left side of the extraction assembly 32 is connected and fixedly installed on the right side of the top of the conveying assembly 3; An anti-error device 4 is provided inside the extraction component 32, an anti-solidification device 5 is provided above the anti-error device 4, and an anti-delay device 6 is provided inside the anti-solidification device 5; The error prevention device 4 includes an electric telescopic rod 41, the bottom of which is fixedly installed at the bottom edge of the inner wall of the extraction component 32, a fine-mesh screen 42 is fixedly installed on the outer wall of the fixed end of the electric telescopic rod 41, a decomposition dish 43 is fixedly installed on the top of the telescopic end of the electric telescopic rod 41, a plurality of electric doors 44 are hinged at the bottom of the decomposition dish 43, an electric rotating rod 45 is rotatably installed at the bottom center of the inner wall of the decomposition dish 43, a plurality of filter plates 46 are fixedly installed on the outer wall of the electric rotating rod 45, a U-shaped groove is provided at the bottom of the filter plate 46, a round rod 47 is fixedly installed on the inner wall of the U-shaped groove of the filter plate 46, friction rings 48 are fixedly installed on the outer walls of the two ends of the round rod 47 away from the axis of the filter plate 46, a spiral mesh plate 49 is fixedly installed on the outer wall of the round rod 47, and the above-mentioned cooperation with the decomposition dish 43 vertically moves During the process, the finished material is effectively prevented from being centrally and accumulated at a fixed point, which makes it convenient for the solvent to soak the material. At the same time, the filter plate 46 rotates to accelerate the material to be fully dissolved in the solvent, ensuring that the components contained in the extracted liquid are relatively uniform, avoiding large errors in the test results when the sample liquid is tested, thereby reducing the detection accuracy; through the above coordination, the spiral mesh plate 49 is used to spirally stir the material precipitated at the bottom of the inner wall of the decomposition dish 43, so that the incompletely dissolved precipitated material is stirred by the spiral mesh plate 49 to reduce the viscosity with the bottom of the inner wall of the decomposition dish 43, which is convenient for it to be re-dissolved under the flushing of the solvent, and further ensures that the material can be fully dissolved in the solvent on the original basis, preventing material residue from remaining while avoiding the increase of detection accuracy error due to equipment reasons.

[0022] A plurality of filter plates 46 are evenly distributed on the outer wall of the electric rotating rod 45 , the outer wall of the friction ring 48 contacts the bottom of the inner wall of the decomposition dish 43 , and the spiral mesh plate 49 is located on the side of the friction ring 48 close to the axis of the filter plate 46 .

[0023] When in use, firstly, 2,4,5-trifluorotoluene is used as a raw material, and chlorine is used as a chlorinating agent to perform photocatalytic chloromethylation inside the reaction component 2 to synthesize 2,4,5-trifluorobenzyl chloride, then 2,4,5-trifluorobenzyl chloride is reacted with a cyanating agent inside the reaction component 2 to obtain 2,4,5-trifluorophenylacetonitrile, and finally 2,4,5-trifluorophenylacetonitrile is hydrolyzed inside the reaction component 2 to obtain 2,4,5-trifluorophenylacetic acid. During the reaction process, the reaction component 2 is a Corning microchannel reactor, and the catalytic lamps 23 in the center of the six reaction plates 22 inside the reaction component 2 are respectively 100 W for the first and fifth lamps, 250 W for the middle three lamps, and 100 W for the second and third lamps. w, then during feeding, chlorine is introduced into the first reaction plate 22 through the air intake assembly 21, and the amount of chlorine is manually controlled. After the finished product is manufactured, the finished product is transported to the inside of the extraction assembly 32 through the conveying assembly 3, and the solvent is injected into the inside of the extraction assembly 32 through the top pipeline of the extraction assembly 32 to dissolve the finished product. After that, the extraction assembly 32 drips the solution to be tested on the top of the detection assembly 31 through the bottom dropper for purity detection; Before the finished material enters the extraction component 32, the electric telescopic rod 41 is started. The telescopic end of the electric telescopic rod 41 drives the decomposition dish 43 to move reciprocatingly up and down. At the same time, the fixed end of the electric telescopic rod 41 limits the fine-pored mesh plate 42 to be stationary. During the reciprocating up and down movement of the decomposition dish 43, the finished material falling from the extraction component 32 is received. At the same time, the solvent is injected into the extraction component 32 and falls into the decomposition dish 43 to soak the finished material. At the same time, the electric rotating rod 45 is started. When the electric rotating rod 45 rotates, it drives the filter plate 46 to rotate and stirs the material and solvent in the decomposition dish 43. After the decomposition is completed, the staff remotely controls the electric door 44 to open through the electronic module. The electric door 44 flips downward with the hinge axis as the axis to cause the liquid in the decomposition dish 43 to fall, and the fine-pored mesh plate 42 blocks the material residue, and the detection liquid falls and is discharged. Through the above cooperation, during the vertical movement of the decomposition dish 43, the finished material is effectively prevented from being centered and accumulated at a fixed point, which is convenient for the solvent to enter the material When the filter plate 46 revolves, the round rod 47 is driven to revolve, and the round rod 47 drives the friction ring 48 to revolve and rub along the bottom of the inner wall of the decomposition dish 43 and generate a rotational force. When the friction ring 48 rotates, the round rod 47 is driven to rotate along the inner wall of the U-shaped groove of the filter plate 46, and the round rod 47 drives the spiral mesh plate 49 to rotate. Through the above cooperation, the spiral mesh plate 49 is used to spirally stir the material precipitated at the bottom of the inner wall of the decomposition dish 43, so that the precipitated material that is not completely dissolved is stirred by the stirring of the spiral mesh plate 49 to reduce the viscosity with the bottom of the inner wall of the decomposition dish 43, so that it is convenient to dissolve it again under the flushing of the solvent, and further ensure that the material can be fully dissolved in the solvent on the original basis, prevent the residual material residue from remaining, and avoid the increase of the detection accuracy error due to equipment reasons.

[0024] See also Figure 1-Figure 8 , based on the above embodiment, another embodiment of the present invention further includes an anti-curing device 5; The anti-curing device 5 includes a friction wheel 51, a reciprocating screw 52, ​​a transmission ring 53 and a U-shaped scraper 54. The bottom of the friction wheel 51 is rotatably installed on the top of one end of the filter plate 46 close to the inner wall of the decomposition dish 43, the bottom of the reciprocating screw 52 is rotatably installed at the center of the top of the friction wheel 51, the transmission ring 53 penetrates inside and is movably installed on the outer wall of the reciprocating screw 52, ​​and the U-shaped scraper 54 is fixedly installed on the outer wall of the transmission ring 53 away from the electric rotating rod 45. Through the above cooperation, the finished product powder remaining on the surface of the filter plate 46 is scraped off by the U-shaped scraper 54 to avoid the powder residue from filling the filter holes. Then, the filter plate 46 is covered with the help of the U-shaped scraper 54, so that no solvent passes through the filter holes of the filter plate 46, and the scouring force between the two is reduced, so that the bubbles generated during the revolution of the filter plate 46 gradually explode to avoid the finished product powder contained in the bubbles to reduce the purity of the solvent, and to avoid excessive accumulation of bubbles to produce foam.

[0025] The outer wall of the friction wheel 51 contacts the inner wall of the decomposition dish 43 , and the inner wall of the U-shaped scraper 54 is slidably connected to the outer wall of the filter plate 46 .

[0026] The anti-curing device 5 also includes a hollow plate 55, an arc plate 56, a vertical rod 57 and a bent plate 58. The end of the hollow plate 55 away from the inner wall of the decomposition dish 43 is hinged to the outer wall of the U-shaped scraper 54 through a torsion spring. The arc plate 56 is hinged to the end of the hollow plate 55 close to the inner wall of the decomposition dish 43 on the side close to the electric rotating rod 45. The outer wall of the arc plate 56 contacts the inner wall of the decomposition dish 43. Both ends of the vertical rod 57 are fixedly installed inside the hollow plate 55. The bent plate 58 penetrates inside and is fixedly installed on the outer wall of the vertical rod 57. Through the above cooperation, the arc plate 56 is used to scrape off the residue attached to the inner wall of the decomposition dish 43, so that the residue is discharged from the decomposition dish 43 in time after the reaction between the solvent and the finished product is completed and falls on the top of the fine-pore mesh plate 42, so as to avoid the solidification of the residue, prevent the chemical components in the residue from continuously corroding the decomposition dish 43 and affecting the next detection result, and rely on the curved surface of the bent plate 58 to guide the solvent and the finished product to be more fully in contact and mixed at the same rotation frequency.

[0027] When in use, the filter plate 46 drives the friction wheel 51 to rotate when it revolves, and the friction wheel 51 generates friction when it revolves along the inner wall of the decomposition dish 43. At this time, the friction wheel 51 starts to rotate along the top of the filter plate 46 due to the friction force. The friction wheel 51 drives the reciprocating screw rod 52 to rotate when it rotates. When the reciprocating screw rod 52 rotates, the reciprocating spiral groove on its outer wall restricts the built-in block of the transmission ring 53. The reciprocating spiral groove drives the transmission ring 53 to slide reciprocatingly downward along the outer wall of the reciprocating screw rod 52 and reset. The transmission ring 53 drives the U-shaped scraper 54 to slide downward along the outer wall of the filter plate 46 and reset. The movement resistance between the filter plate 46 and the solvent will be gradually increased during the process of the U-shaped scraper 54 gradually covering the outer wall of the filter plate 46. At the same time, the U-shaped scraper 54 scrapes the filter plate 46. Through the above cooperation, the finished product powder remaining on the surface of the filter plate 46 is scraped off by the U-shaped scraper 54 to prevent the residual powder from filling the filter holes. Then, the filter plate 46 is covered with the help of the U-shaped scraper 54, so that no solvent passes through the filter holes of the filter plate 46, and the scouring force between the two is reduced, so that the bubbles generated during the revolution of the filter plate 46 gradually explode to prevent the bubbles from containing finished product powder and reduce the purity of the solvent. And avoid excessive accumulation of bubbles to produce floating foam; when the U-shaped scraper 54 revolves and moves vertically up and down, it drives the hollow plate 55 to move synchronously, and the hollow plate 55 drives the arc plate 56 to move synchronously along the inner wall of the decomposition dish 43. The arc plate 56 is pushed by the hollow plate 55 to cause its own hinge axis to start rotating. At this time, the arc plate 56 rotates with the hinge axis as the axis and adjusts to a suitable sliding angle. Subsequently, the arc plate 56 removes the finished powder attached to the inner wall of the decomposition dish 43 due to the centrifugal force of the filter plate 46. At the same time, the hollow plate 55 drives the vertical rod 57 to move synchronously, and the vertical rod 57 drives The bending plate 58 moves synchronously, and the bending plate 58 expands the contact area between the solvent and the finished product through its own arc surface. Through the above cooperation, the residue attached to the inner wall of the decomposition dish 43 is scraped off with the help of the arc plate 56, so that the residue can be discharged from the decomposition dish 43 in time after the reaction between the solvent and the finished product is completed and fall on the top of the fine-pored mesh plate 42, avoiding the solidification of the residue, preventing the chemical components in the residue from continuously corroding the decomposition dish 43 and affecting the next detection result, and relying on the arc surface of the bending plate 58 to facilitate the solvent and the finished product to be more fully in contact and mixed at the same rotation frequency.

[0028] See also Figure 1-Figure 8 , based on the above embodiment, another embodiment of the present invention further includes an anti-delay device 6; The anti-delay device 6 includes a heating component 61, a pressure plate 62, a positioning plate 63, a transmission rod 64 and a plurality of heat-conducting plates 65. The back of the heating component 61 is fixedly mounted on the outer wall of the U-shaped scraper 54, the bottom of the pressure plate 62 close to the outer wall of the filter plate 46 is fixedly mounted on the top of the U-shaped scraper 54, the bottom of the positioning plate 63 close to the center of the decomposition dish 43 is fixedly mounted on the top edge of the electric rotating rod 45, and the top of the transmission rod 64 is fixedly mounted on the bottom edge of the positioning plate 63. Through the above coordination, the heat-conducting plate 65 is used to increase the frequency of the solvent moving toward the direction close to the heating component 61 within the same reaction time, so that the solvent can be heated evenly and quickly heated, thereby optimizing the plasma reaction of the material ion source and the solvent, improving the sensitivity and accuracy of the detection, and effectively shortening the waiting time for the precipitation to be detected.

[0029] The outer wall of the transmission rod 64 penetrates through and is threadedly connected to the inside of the pressure plate 62 . A plurality of heat conducting plates 65 are evenly distributed on the outer wall of the transmission rod 64 . A sliding groove begins to be formed on the outer wall of the heat conducting plates 65 .

[0030] The anti-delay device 6 also includes a sliding plate 66, a fixed block 67, a cross bar 68 and a friction roller 69. The outer wall of the sliding plate 66 is slidably installed in the slide groove of the heat conducting plate 65 by a longitudinal spring. The sliding plate 66 is located on the movement track at the bottom of the pressure plate 62. The back of the fixed block 67 is fixedly installed on the outer wall of the sliding plate 66. The cross bar 68 is rotatably installed on the right side of the fixed block 67 near one end of the transmission rod 64. The friction roller 69 passes through the inside and is fixedly installed on the outer wall of the cross bar 68. The outer wall of the friction roller 69 contacts the outer wall of the heat conducting plate 65. Through the above cooperation, the friction roller 69 rotates to brush away the powder residue attached to the outer wall of the heat conducting plate 65 to ensure the cleanliness of the outer wall of the heat conducting plate 65, avoid the outer wall of the heat conducting plate 65 being covered with powder residue, thereby reducing the thermal conductivity of the heat conducting plate 65, and avoid uneven temperature rise of the solvent inside the decomposition dish 43, resulting in the overall temperature difference of the solvent, thereby affecting the plasma reaction, causing the detection results to change frequently and making it difficult to obtain an accurate average value.

[0031] When in use, the U-shaped scraper 54 revolves and moves downward, driving the heating component 61 to move synchronously, thereby expanding the movement range of the heating component 61. At the same time, the heating component 61 drives the pressing plate 62 to move synchronously. When the pressing plate 62 moves downward, it will slide downward along the outer wall of the transmission rod 64. At this time, the positioning plate 63 limits the transmission rod 64. When the pressing plate 62 slides, it drives the spirally connected transmission rod 64 to generate a rotating force and start to rotate. When the transmission rod 64 rotates, it drives the heat conducting plate 65 to rotate. When the heat conducting plate 65 rotates, it disturbs the solvent around the heating component 61. Through the above cooperation, the frequency of the solvent moving toward the heating component 61 is increased within the same reaction time by relying on the heat conducting plate 65, so that the solvent can be heated evenly and quickly heated, thereby optimizing the plasma reaction of the material ion source and the solvent, improving the sensitivity and accuracy of the detection, and effectively shortening the waiting time for the precipitation to be detected; the heat conducting plate 65 drives the sliding plate 66 to move synchronously, and the top of the sliding plate 66 moves downward during the downward movement of the pressing plate 62. During the movement, the sliding plate 66 will be pressed by the bottom of the pressure plate 62. At this time, the sliding plate 66 slides downward along the inside of the slide groove of the heat conducting plate 65. When the pressure plate 62 is reset, the sliding plate 66 is automatically reset by the longitudinal spring, and this is repeated. At the same time, when the sliding plate 66 moves downward, it drives the fixed block 67 to move synchronously, and the fixed block 67 drives the cross bar 68 to move synchronously. The cross bar 68 drives the friction roller 69 to slide and rub downward along the outer wall of the heat conducting plate 65. The friction roller 69 generates a rotating force through friction and drives the cross bar 68 to rotate. The friction roller 69 moves downward along the outer wall of the heat conducting plate 65 and brushes the outer wall of the heat conducting plate 65. Through the above cooperation, the friction roller 69 rotates to brush away the powder residue attached to the outer wall of the heat conducting plate 65, so as to ensure the cleanliness of the outer wall of the heat conducting plate 65, avoid the outer wall of the heat conducting plate 65 being covered with powder residue, thereby reducing the thermal conductivity of the heat conducting plate 65, and avoid uneven temperature rise of the solvent inside the decomposition dish 43, resulting in the overall temperature difference of the solvent, thereby affecting the plasma reaction, causing the detection results to change frequently and making it difficult to obtain an accurate average value.

[0032] A sampling and detection method based on a sampling and detection device prepared by 2,4,5-trifluorophenylacetic acid, comprising the following steps: S1: firstly, 2,4,5-trifluorotoluene is used as a raw material, chlorine is used as a chlorinating agent, and photocatalytic chloromethylation is performed inside the reaction component 2 to synthesize 2,4,5-trifluorobenzyl chloride. Then, 2,4,5-trifluorobenzyl chloride is reacted with a cyanating agent inside the reaction component 2 to obtain 2,4,5-trifluorophenylacetonitrile. Finally, 2,4,5-trifluorophenylacetonitrile is hydrolyzed inside the reaction component 2 to obtain 2,4,5-trifluorophenylacetic acid. S2: During the reaction process, the reaction component 2 is a Corning microchannel reactor, and the catalytic lamps 23 in the center of the six reaction plates 22 inside it are the first and fifth 100 W lamps, and the three in the middle are 250 W. After that, when feeding, chlorine is introduced into the first reaction plate 22 through the air intake component 21, and the amount of chlorine is manually controlled. After the finished product is manufactured, the finished product is transported to the inside of the extraction component 32 through the conveying component 3, and the solvent is injected into the inside of the extraction component 32 through the top pipeline of the extraction component 32, and the finished product is dissolved. After that, the extraction component 32 drips the solution to be tested on the top of the detection component 31 through the bottom dropper for purity detection; S3: Before the finished material enters the extraction component 32, the electric telescopic rod 41 is started, and the telescopic end of the electric telescopic rod 41 drives the decomposition dish 43 to move up and down reciprocatingly. At the same time, the fixed end of the electric telescopic rod 41 limits the fine-mesh plate 42 to be stationary. During the reciprocating up and down movement of the decomposition dish 43, the finished material falling from the extraction component 32 is received; S4: At the same time, the solvent is injected into the extraction component 32 and then falls into the decomposition dish 43 and soaks the finished material. At the same time, the electric rotating rod 45 is started. When the electric rotating rod 45 rotates, it drives the filter plate 46 to rotate and stirs the material and solvent inside the decomposition dish 43. After the decomposition is completed, the staff remotely controls the electric door 44 to open through the electronic module. The electric door 44 flips downward with the hinge axis as the axis to cause the liquid inside the decomposition dish 43 to fall, and the fine-pored mesh plate 42 blocks the material residue, and the detection liquid falls and is discharged.

[0033] The above description is only a preferred specific implementation manner of the present invention, but the protection scope of the present invention is not limited thereto. Any technician familiar with the technical field can make equivalent replacements or changes according to the technical scheme and inventive concept of the present invention within the technical scope disclosed by the present invention, which should be covered by the protection scope of the present invention.

Claims

1. A sampling and detection device based on 2,4,5-trifluorophenylacetic acid, comprising a base (1), characterized in that: A reaction assembly (2) is arranged on the left side of the top of the base (1), an air intake assembly (21) is arranged on the top of the reaction assembly (2), six reaction plates (22) are arranged inside the reaction assembly (2), and catalytic lamps (23) are arranged inside the six reaction plates (22), a conveying assembly (3) is arranged on the right side of the reaction assembly (2), a detection assembly (31) is arranged on the right side of the top of the base (1), an extraction assembly (32) is arranged on the top of the detection assembly (31), and the left side of the extraction assembly (32) is connected to and fixedly mounted on the right side of the top of the conveying assembly (3); An anti-error device (4) is arranged inside the extraction component (32), an anti-solidification device (5) is arranged above the anti-error device (4), and an anti-delay device (6) is arranged inside the anti-solidification device (5); The error prevention device (4) comprises an electric telescopic rod (41), the bottom of the electric telescopic rod (41) being fixedly mounted at the bottom edge of the inner wall of the extraction component (32), a fine mesh plate (42) being fixedly mounted on the outer wall of the fixed end of the electric telescopic rod (41), a decomposition dish (43) being fixedly mounted on the top of the telescopic end of the electric telescopic rod (41), a plurality of electric doors (44) being hingedly connected to the bottom of the decomposition dish (43), an electric rotating rod (45) being rotatably mounted at the center of the bottom of the inner wall of the decomposition dish (43), a plurality of filter plates (46) being fixedly mounted on the outer wall of the electric rotating rod (45), a U-shaped groove being provided at the bottom of the filter plate (46), a round rod (47) being fixedly mounted on the inner wall of the U-shaped groove of the filter plate (46), friction rings (48) being fixedly mounted on the outer wall of both ends of the round rod (47) away from the axis of the filter plate (46), and a spiral mesh plate (49) being fixedly mounted on the outer wall of the round rod (47).

2. A sampling detection device prepared based on 2,4,5-trifluorophenylacetic acid according to claim 1, characterized in that: The plurality of filter plates (46) are equidistantly distributed on the outer wall of the electric rotating rod (45); the outer wall of the friction ring (48) contacts the bottom of the inner wall of the decomposition dish (43); and the spiral mesh plate (49) is located on the side of the friction ring (48) close to the axis of the filter plate (46).

3. A sampling detection device prepared based on 2,4,5-trifluorophenylacetic acid according to claim 2, characterized in that: The anti-curing device (5) comprises a friction wheel (51), a reciprocating screw rod (52), a transmission ring (53) and a U-shaped scraper (54); the bottom of the friction wheel (51) is rotatably mounted on the top of one end of the filter plate (46) close to the inner wall of the decomposition dish (43); the bottom of the reciprocating screw rod (52) is rotatably mounted at the center of the top of the friction wheel (51); the transmission ring (53) penetrates the inside and is movably mounted on the outer wall of the reciprocating screw rod (52); and the U-shaped scraper (54) is fixedly mounted on the outer wall of the transmission ring (53) on the side away from the electric rotating rod (45).

4. A sampling detection device prepared based on 2,4,5-trifluorophenylacetic acid according to claim 3, characterized in that: The outer wall of the friction wheel (51) contacts the inner wall of the decomposition dish (43), and the inner wall of the U-shaped scraper (54) is slidably connected to the outer wall of the filter plate (46).

5. A sampling detection device prepared based on 2,4,5-trifluorophenylacetic acid according to claim 4, characterized in that: The anti-solidification device (5) further comprises a hollow plate (55), an arc-shaped plate (56), a vertical rod (57) and a bent plate (58); an end of the hollow plate (55) away from the inner wall of the decomposition dish (43) is hinged to the outer wall of the U-shaped scraper (54) via a torsion spring; a side of the arc-shaped plate (56) close to the electric rotating rod (45) is hinged to an end of the hollow plate (55) close to the inner wall of the decomposition dish (43); the outer wall of the arc-shaped plate (56) contacts the inner wall of the decomposition dish (43); both ends of the vertical rod (57) are fixedly mounted inside the hollow plate (55); and the bent plate (58) penetrates inside and is fixedly mounted on the outer wall of the vertical rod (57).

6. A sampling detection device prepared based on 2,4,5-trifluorophenylacetic acid according to claim 5, characterized in that: The anti-delay device (6) comprises a heating component (61), a pressing plate (62), a positioning plate (63), a transmission rod (64) and a plurality of heat conducting plates (65). The back of the heating component (61) is fixedly mounted on the outer wall of the U-shaped scraper (54). The bottom of one end of the pressing plate (62) close to the outer wall of the filter plate (46) is fixedly mounted on the top of the U-shaped scraper (54). The bottom of one end of the positioning plate (63) close to the center of the decomposition dish (43) is fixedly mounted on the top edge of the electric rotating rod (45). The top of the transmission rod (64) is fixedly mounted on the bottom edge of the positioning plate (63). The plurality of heat conducting plates (65) are fixedly mounted on the outer wall of the transmission rod (64).

7. A sampling detection device prepared based on 2,4,5-trifluorophenylacetic acid according to claim 6, characterized in that: The outer wall of the transmission rod (64) penetrates through and is threadedly connected to the interior of the pressure plate (62); a plurality of the heat conducting plates (65) are equidistantly distributed on the outer wall of the transmission rod (64); and a slide groove is formed at the beginning of the outer wall of the heat conducting plate (65).

8. A sampling detection device prepared based on 2,4,5-trifluorophenylacetic acid according to claim 7, characterized in that: The anti-delay device (6) further comprises a sliding plate (66), a fixed block (67), a cross bar (68) and a friction roller (69); the outer wall of the sliding plate (66) is slidably mounted inside the slide groove of the heat conducting plate (65) via a longitudinal spring; the sliding plate (66) is located on the bottom movement track of the pressure plate (62); the back of the fixed block (67) is fixedly mounted on the outer wall of the sliding plate (66); one end of the cross bar (68) close to the transmission rod (64) is rotatably mounted on the right side of the fixed block (67); the friction roller (69) penetrates inside and is fixedly mounted on the outer wall of the cross bar (68); the outer wall of the friction roller (69) contacts the outer wall of the heat conducting plate (65).

9. A sampling and detection method based on the sampling and detection device prepared by 2,4,5-trifluorophenylacetic acid, using the sampling and detection device based on 2,4,5-trifluorophenylacetic acid according to claim 8, characterized in that: The following steps are involved: S1: firstly, 2,4,5-trifluorotoluene is used as a raw material and chlorine is used as a chlorinating agent to perform photocatalytic chloromethylation inside the reaction component (2) to synthesize 2,4,5-trifluorobenzyl chloride. Then, 2,4,5-trifluorobenzyl chloride is reacted with a cyanating agent inside the reaction component (2) to obtain 2,4,5-trifluorophenylacetonitrile. Finally, 2,4,5-trifluorophenylacetonitrile is hydrolyzed inside the reaction component (2) to obtain 2,4,5-trifluorophenylacetic acid. S2: During the reaction process, the reaction component (2) is a Corning microchannel reactor, and the catalytic lamps (23) in the center of the six reaction plates (22) inside the reactor are 100 W for the first and fifth lamps, and 250 W for the three middle lamps. When feeding, chlorine gas is introduced into the first reaction plate (22) through the air intake component (21), and the amount of chlorine gas is manually controlled. After the finished product is manufactured, the finished product is transported to the inside of the extraction component (32) through the conveying component (3), and the solvent is injected into the inside of the extraction component (32) through the top pipe of the extraction component (32) to dissolve the finished product. After that, the extraction component (32) drips the solution to be tested onto the top of the detection component (31) through the bottom dropper for purity detection; S3: before the finished material enters the extraction component (32), the electric telescopic rod (41) is started, and the telescopic end of the electric telescopic rod (41) drives the decomposition dish (43) to move up and down reciprocatingly, and at the same time, the fixed end of the electric telescopic rod (41) limits the fine-mesh plate (42) to be stationary, and the decomposition dish (43) receives the finished material falling from the extraction component (32) during the reciprocating up and down movement; S4: At the same time, the solvent is injected into the extraction component (32) and then falls into the decomposition dish (43) to soak the finished material. At the same time, the electric rotating rod (45) is started. When the electric rotating rod (45) rotates, it drives the filter plate (46) to rotate and stirs the material and the solvent inside the decomposition dish (43). After the decomposition is completed, the staff remotely controls the electric door (44) to open through the electronic module. The electric door (44) turns downward with the hinge axis as the axis to cause the liquid inside the decomposition dish (43) to fall, and the fine-pored mesh plate (42) blocks the material residue, and the detection liquid falls and is discharged.

Images