Intermittent pretreatment device and method for high-purity reagent acetonitrile

Abstract

The invention discloses a high-purity reagent acetonitrile intermittent pretreatment device and method, and relates to the technical field of pretreatment, the high-purity reagent acetonitrile intermittent pretreatment device comprises a reaction container, the outer wall of the reaction container is fixedly provided with a support frame, the top of the reaction container is fixedly provided with a feed pipe, and the bottom of the reaction container is fixedly provided with a discharge pipe; a monitoring tank is fixedly mounted at the bottom of the discharging pipe; the pretreatment device is arranged in the reaction container, the pretreatment device comprises a motor, a fixed rod, a filter frame, an elastic telescopic rod, a molecular sieve plate, a reciprocating threaded groove, a threaded plate, a fixed column and a circular sieve plate, the elastic telescopic rod is driven to rotate through rotation of the filter frame, and the molecular sieve plate is driven to rotate through rotation of the elastic telescopic rod; the motor is fixedly installed at the top of the reaction container, gas or liquid molecules are adsorbed through rotation of the molecular sieve plate, water in acetonitrile is adsorbed, the adsorption effect is improved, and the water is prevented from affecting the concentration of acetonitrile.

Description

Technical Field

[0001] The invention relates to the technical field of pretreatment, and in particular to an intermittent pretreatment device and method for high-purity reagent acetonitrile. Background Art

[0002] High-purity reagent acetonitrile batch pretreatment device is usually used in chemical experiments, production or industrial processes, especially when high-purity reagents need to be treated, separated or purified.

[0003] The patent with patent announcement number CN206089511U relates to an intermittent pretreatment device for high-purity reagent acetonitrile, which is composed of an acetonitrile raw material receiving tank, an acetonitrile pretreatment receiving tank, and an exhaust gas destroyer. The acetonitrile raw material receiving tank is connected to the material inlet at the top of the acetonitrile pretreatment receiving tank, and the gaseous oxidant enters the acetonitrile pretreatment receiving tank from the gas disperser at the bottom of the acetonitrile pretreatment receiving tank. The exhaust valve at the top of the acetonitrile pretreatment receiving tank is connected to the exhaust gas destroyer. Two "cross-shaped" gas dispersers are installed at the bottom of the acetonitrile pretreatment tank. The installation angle of the two gas dispersers is 90°. The gas dispersers are made of stainless steel pipes. Numerous microholes are punched on the stainless steel pipes by laser. The pore diameter is 0.1mm and the hole spacing is 0.5mm. The gas oxidant enters the acetonitrile pretreatment tank from the gas disperser at the bottom of the acetonitrile pretreatment tank. The acetonitrile material is injected from the feed port at the top of the acetonitrile pretreatment tank. There are two material baffles and an exhaust valve on the top of the acetonitrile pretreatment tank. A magnetic flap level gauge is installed on the side of the acetonitrile pretreatment tank.

[0004] In the above patent, acetonitrile material is injected from the feed port at the top of the acetonitrile pretreatment tank. There are two material baffles and one exhaust valve on the top of the acetonitrile pretreatment tank. A magnetic flap level gauge is installed on the side of the acetonitrile pretreatment tank. However, acetonitrile impurities may adhere to the inner wall of the filter, causing the filter holes to be blocked, affecting the separation effect. Summary of the invention

[0005] In view of the deficiencies in the prior art, the present invention provides an intermittent pretreatment device and method for a high-purity reagent acetonitrile, which solves the problems raised in the above-mentioned background technology.

[0006] To achieve the above objectives, the present invention is implemented through the following technical solutions: an intermittent pretreatment device for high-purity reagent acetonitrile, comprising: a reaction container, a support frame is fixedly installed on the outer wall of the reaction container, a feed pipe is fixedly installed on the top of the reaction container, a discharge pipe is fixedly installed on the bottom of the reaction container, and a monitoring tank is fixedly installed on the bottom of the discharge pipe; a pretreatment device, the pretreatment device is arranged inside the reaction container, the pretreatment device includes a motor, a fixed rod, a filter frame, an elastic telescopic rod, a molecular sieve plate, a reciprocating threaded groove, a threaded plate, a fixed column and a circular sieve plate, the rotation of the filter frame will drive the elastic telescopic rod to rotate, and the rotation of the elastic telescopic rod will drive the molecular sieve plate to rotate, the motor is fixedly installed on the top of the reaction container, The fixed rod is fixedly installed at the output end of the motor, the filter frame is fixedly installed at the bottom of the fixed rod, the elastic telescopic rod is fixedly installed at the bottom of the filter frame, the molecular sieve plate is fixedly installed at the free end of the elastic telescopic rod, the reciprocating thread groove is opened on the circumferential surface of the fixed rod, the threaded plate is threadedly installed on the circumferential surface of the fixed rod, the fixed column is fixedly installed on the top of the inner wall of the reaction container, the fixed column penetrates the surface of the threaded plate, and the circular sieve plate is fixedly installed on the circumferential surface of the threaded plate. The rotation of the fixed rod will drive the reciprocating thread groove to rotate, the rotation of the reciprocating thread groove will drive the threaded plate to reciprocate up and down, the up and down reciprocating motion of the threaded plate will drive the circular sieve plate to reciprocate up and down, and the up and down reciprocating motion of the circular sieve plate will scrape off the particles attached to the inner wall of the filter frame.

[0007] According to the above technical solution, the circular sieve plate contacts the inner wall of the filter frame, and the inner wall of the filter frame is scraped by moving the circular sieve plate up and down. The molecular sieve plate is arranged at the bottom of the filter frame, and the moisture in acetonitrile is removed by the molecular sieve plate.

[0008] According to the above technical scheme, the fixed column is provided with an anti-adhesion device for preventing the solution from adhering to the inner wall of the reaction container, and the anti-adhesion device is provided with an anti-blocking device. The anti-adhesion device includes a hollow column, a sliding plate, a connecting rod, a circular ring plate and a short rod. The threaded plate moves upward to drive the hollow column to move upward, and the upward movement of the hollow column will push the sliding plate to move upward, and the upward movement of the sliding plate will drive the connecting rod to move upward, and the upward movement of the connecting rod will drive the circular ring plate to move upward. The hollow column is fixedly installed on the top of the threaded plate, and the hollow column is slidably installed on the surface of the fixed column. A sliding groove is opened on the surface of the fixed column, and the sliding plate is slidably installed on the inner wall of the sliding groove. The connecting rod is fixedly installed on the top of the sliding plate, and the circular ring plate is fixedly installed on the bottom of the connecting rod, and the short rod is fixedly installed on the bottom of the circular ring plate.

[0009] According to the above technical solution, a U-shaped rod is fixedly installed on the surface of the sliding plate, a sealing ring is fixedly installed on the inner wall of the feed pipe, a sliding rod is slidably installed on the surface of the sealing ring, a sealing plate is fixedly installed on the top of the sliding rod, and a long rod is fixedly installed on the bottom of the sealing plate. The upward movement of the sliding plate will drive the U-shaped rod to move upward, the upward movement of the U-shaped rod will drive the long rod to move upward, the upward movement of the long rod will drive the sealing plate to move upward, and the upward movement of the sealing plate will break away from the contact with the sealing ring, allowing acetonitrile to flow into the filter frame.

[0010] According to the above technical solution, the hollow column is arranged below the sliding plate, a No. 1 spring is arranged between the sliding plate and the sliding groove, and the sliding plate is reset by the No. 1 spring, and a No. 2 spring is arranged between the sealing ring and the sliding rod, and the sliding rod is reset by the No. 2 spring.

[0011] According to the above technical scheme, the anti-clogging device includes a fixed frame, a connecting frame, a rotating plate, a sliding seat, a convex rod and a convex block. The upward movement of the circular ring plate will drive the fixed frame to move upward, the upward movement of the fixed frame will drive the rotating plate to move upward, and the upward movement of the rotating plate will pull the sliding seat to move toward the inner wall of the reaction vessel. The fixed frame is fixedly installed on the bottom of the circular ring plate, the connecting frame is fixedly installed on the inner wall of the reaction vessel, the sliding seat is slidably installed on the inner wall of the connecting frame, one end of the rotating plate is rotatably installed on the inner wall of the fixed frame, and the other end of the rotating plate is rotatably installed on the surface of the sliding seat, the convex rod is fixedly installed on the side of the sliding seat away from the reaction vessel, and the convex block is fixedly installed on the circumferential surface of the filter frame.

[0012] According to the above technical solution, a fixed connecting rod is fixedly installed at the bottom of the sliding seat, a triangular block is fixedly installed at the bottom of the fixed connecting rod, and a dome column is fixedly installed on the top of the molecular sieve plate. When the molecular sieve plate rotates, the dome column will be driven to rotate, and the rotation of the dome column will contact the triangular block. The triangular block will push the dome column to move downward, and the downward movement of the dome column will drive the molecular sieve plate to move up and down.

[0013] According to the above technical solution, a No. 3 spring is arranged between the sliding seat and the connecting frame, and the No. 3 spring drives the sliding seat to reset, and the protruding rod contacts the surface of the protruding block.

[0014] A method for using a high-purity reagent acetonitrile intermittent pretreatment device comprises the following steps: Step 1: inject acetonitrile into the filter frame through the feed pipe, start the motor, the motor rotates to drive the fixed rod to rotate, the fixed rod rotates to drive the filter frame to rotate, and the solid particles, impurities and insolubles in the acetonitrile are separated from the acetonitrile by the centrifugal force generated by the rotation of the filter frame, so as to prevent the solid particles, impurities and insolubles from affecting the purity of the acetonitrile; Step 2: The rotation of the filter frame drives the elastic telescopic rod to rotate, and the rotation of the elastic telescopic rod drives the molecular sieve plate to rotate. The molecular sieve plate rotates to adsorb gas or liquid molecules, and absorbs the moisture in acetonitrile to prevent the moisture from affecting the acetonitrile concentration. At the same time, the rotation can significantly increase the contact area between the adsorbent and the target molecules, thereby improving the adsorption effect; Step 3: Improve the treatment effect. At the same time, the rotation of the fixed rod drives the reciprocating thread groove to rotate. The rotation of the reciprocating thread groove drives the thread plate to reciprocate up and down. The up and down reciprocating movement of the thread plate drives the circular screen plate to reciprocate up and down. The particles attached to the inner wall of the filter frame are scraped off by the up and down reciprocating movement of the circular screen plate to prevent the particles from clogging the filter frame and affecting the filtering and separation effect of the filter frame. Step 4: The treated acetonitrile will enter the monitoring tank through the discharge pipe. By detecting the moisture content of acetonitrile, the adsorption effect of the molecular sieve plate can be judged. If the moisture content in acetonitrile is still high after treatment, it means that the molecular sieve plate has lost its adsorption capacity and may need to be replaced or regenerated.

[0015] The present invention provides a high-purity reagent acetonitrile intermittent pretreatment device and method, which has the following beneficial effects: (1) The invention separates solid particles, impurities and insolubles in acetonitrile from acetonitrile through the centrifugal force generated by the rotation of the filter frame, thereby preventing the solid particles, impurities and insolubles from affecting the purity of the acetonitrile. At the same time, the rotation of the filter frame will drive the elastic telescopic rod to rotate, and the rotation of the elastic telescopic rod will drive the molecular sieve plate to rotate. The rotation of the molecular sieve plate adsorbs gas or liquid molecules, and absorbs the moisture in the acetonitrile, thereby improving the adsorption effect and preventing the moisture from affecting the acetonitrile concentration. At the same time, the rotation can significantly increase the contact area between the adsorbent and the target molecules, thereby improving the treatment effect. The up and down reciprocating motion of the circular sieve plate will scrape off the particles attached to the inner wall, thereby preventing the particles from clogging the filter frame. The adsorption effect of the molecular sieve plate can be judged by detecting the moisture content of the acetonitrile. If the moisture content in the acetonitrile is still high after treatment, it means that the molecular sieve has lost its adsorption capacity and may need to be replaced or regenerated.

[0016] (2) The invention drives the hollow column upward by moving the threaded plate upward, which in turn drives the sliding plate upward, which in turn drives the connecting rod upward. The acetonitrile adhering to the inner wall of the reaction vessel is pushed downward onto the molecular sieve plate by the up-and-down reciprocating motion of the circular ring plate, thereby improving the adsorption effect. At the same time, the sealing plate moves upward to break away from the contact with the sealing ring, allowing the acetonitrile to flow into the filter frame, and is processed by intermittently feeding acetonitrile to prevent too much acetonitrile from entering at one time, resulting in the inability of the molecular sieve plate of the filter frame to effectively process the acetonitrile, thereby affecting the purity of the acetonitrile.

[0017] (3) In the present invention, the movement of the sliding seat toward the inner wall of the reaction container drives the protruding rod to move toward the inner wall of the reaction container. The movement of the protruding rod toward the inner wall of the reaction container causes the protruding rod to break away from the contact with the protrusion, thereby preventing the protruding rod from continuously contacting the protrusion when the filter frame drives the protrusion to rotate, thereby reducing the service life of the filter frame. By moving the molecular sieve plate up and down, the contact time and contact area between the molecular sieve plate and acetonitrile can be increased, thereby extending the contact time between the water molecules in the acetonitrile and the molecular sieve, increasing the adsorption opportunities of the molecular sieve plate, and facilitating more efficient water removal. BRIEF DESCRIPTION OF THE DRAWINGS

[0018] Figure 1 It is a schematic diagram of the overall structure of the present invention; Figure 2 It is a schematic diagram of the overall cross-sectional structure of the present invention; Figure 3 This is a schematic diagram of the cross-sectional structure of the filter frame of the present invention; Figure 4 This is a schematic diagram of the structure of the elastic telescopic rod and the molecular sieve plate of the present invention; Figure 5 It is a schematic diagram of the structure of the sliding plate and the U-shaped plate of the present invention; Figure 6 This is a schematic diagram of the cross-sectional structure of the feed pipe of the present invention; Figure 7 It is a schematic structural diagram of the anti-clogging device of the present invention.

[0019] In the figure: 1, reaction vessel; 2, support frame; 3, feed pipe; 4, discharge pipe; 5, monitoring tank; 6, motor; 7, fixed rod; 8, filter frame; 9, elastic telescopic rod; 10, molecular sieve plate; 11, reciprocating thread groove; 12, threaded plate; 13, fixed column; 14, circular sieve plate; 151, hollow column; 152, sliding plate; 153, connecting rod; 154, circular ring plate; 155, short rod; 156, U-shaped rod; 157, sealing ring; 158, sliding rod; 159, sealing plate; 1510, long rod; 161, fixed frame; 162, connecting frame; 163, rotating plate; 164, sliding seat; 165, convex rod; 166, convex block; 167, fixed connecting rod; 168, triangular block; 169, dome column. DETAILED DESCRIPTION

[0020] The following will be combined with the drawings in the embodiments of the present invention to clearly and completely describe the technical solutions in the embodiments of the present invention. Obviously, the described embodiments are only part of the embodiments of the present invention, not all of the embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field without creative work are within the scope of protection of the present invention.

[0021] See also Figure 1-Figure 3One embodiment of the present invention is: an intermittent pretreatment device for high-purity reagent acetonitrile, comprising: a reaction vessel 1, a support frame 2 is fixedly installed on the outer wall of the reaction vessel 1, a feed pipe 3 is fixedly installed on the top of the reaction vessel 1, a discharge pipe 4 is fixedly installed on the bottom of the reaction vessel 1, and a monitoring tank 5 is fixedly installed on the bottom of the discharge pipe 4; a pretreatment device, the pretreatment device is arranged inside the reaction vessel 1, the pretreatment device comprises a motor 6, a fixed rod 7, a filter frame 8, an elastic telescopic rod 9, a molecular sieve plate 10, a reciprocating thread groove 11, a threaded plate 12, a fixed column 13 and a circular sieve plate 14, the molecular sieve plate 10 rotates to adsorb gas or liquid molecules, and the moisture in the acetonitrile is adsorbed to provide High adsorption effect, prevent moisture from affecting acetonitrile concentration, motor 6 is fixedly installed on the top of reaction container 1, fixed rod 7 is fixedly installed on the output end of motor 6, filter frame 8 is fixedly installed on the bottom of fixed rod 7, elastic telescopic rod 9 is fixedly installed on the bottom of filter frame 8, molecular sieve plate 10 is fixedly installed on the free end of elastic telescopic rod 9, reciprocating thread groove 11 is opened on the circumferential surface of fixed rod 7, threaded plate 12 is threadedly installed on the circumferential surface of fixed rod 7, fixed column 13 is fixedly installed on the top of the inner wall of reaction container 1, fixed column 13 passes through the surface of threaded plate 12, circular sieve plate 14 is fixedly installed on the circumferential surface of threaded plate 12, prevent particulate matter from clogging filter frame 8 and affecting the filtering and separation effect of filter frame 8.

[0022] The circular sieve plate 14 contacts the inner wall of the filter frame 8 and is moved up and down to scrape the inner wall of the filter frame 8 . The molecular sieve plate 10 is arranged at the bottom of the filter frame 8 and is used to remove moisture from the acetonitrile.

[0023] When the present embodiment is working, acetonitrile is injected into the filter frame 8 through the feed pipe 3, and the motor 6 is started. The rotation of the motor 6 drives the fixed rod 7 to rotate, and the rotation of the fixed rod 7 drives the filter frame 8 to rotate. The solid particles, impurities and insolubles in the acetonitrile are separated from the acetonitrile by the centrifugal force generated by the rotation of the filter frame 8, so as to prevent the solid particles, impurities and insolubles from affecting the purity of the acetonitrile. At the same time, the rotation of the filter frame 8 drives the elastic telescopic rod 9 to rotate, and the rotation of the elastic telescopic rod 9 drives the molecular sieve plate 10 to rotate. The molecular sieve plate 10 rotates to adsorb gas or liquid molecules, and absorbs the moisture in the acetonitrile, thereby improving the adsorption effect and preventing the moisture from affecting the acetonitrile concentration. At the same time, the rotation can significantly increase the contact surface between the adsorbent and the target molecule. The treatment effect is improved, and the rotation of the fixed rod 7 will drive the reciprocating thread groove 11 to rotate, and the rotation of the reciprocating thread groove 11 will drive the thread plate 12 to reciprocate up and down, and the up and down reciprocating movement of the thread plate 12 will drive the circular sieve plate 14 to reciprocate up and down, and the up and down reciprocating movement of the circular sieve plate 14 will scrape off the particles attached to the inner wall of the filter frame 8 to prevent the particles from clogging the filter frame 8 and affecting the filtering and separation effect of the filter frame 8. The acetonitrile after the treatment will enter the monitoring tank 5 through the discharge pipe 4. By detecting the water content of acetonitrile, the adsorption effect of the molecular sieve plate 10 can be judged. If the water content in the acetonitrile is still high after treatment, it means that the molecular sieve has lost its adsorption capacity and may need to be replaced or regenerated.

[0024] See also Figure 1-Figure 7 On the basis of the above embodiment, in another embodiment of the present invention, an anti-adhesion device for preventing the solution from adhering to the inner wall of the reaction container 1 is provided on the fixed column 13, and an anti-blocking device is provided on the anti-adhesion device. The anti-adhesion device includes a hollow column 151, a sliding plate 152, a connecting rod 153, a circular ring plate 154 and a short rod 155. The hollow column 151 is fixedly mounted on the top of the threaded plate 12, and the hollow column 151 is slidably mounted on the surface of the fixed column 13. A slide groove is provided on the surface of the fixed column 13, and the sliding plate 152 is slidably mounted on the inner wall of the slide groove. The connecting rod 153 is fixedly mounted on the top of the sliding plate 152, and the circular ring plate 154 is fixedly mounted on the bottom of the connecting rod 153. The short rod 155 is fixedly mounted on the bottom of the circular ring plate 154. The acetonitrile adhering to the inner wall of the reaction container 1 is pushed down to the molecular sieve plate 10 through the up and down reciprocating motion of the circular ring plate 154, thereby improving the adsorption effect.

[0025] A U-shaped rod 156 is fixedly installed on the surface of the sliding plate 152, a sealing ring 157 is fixedly installed on the inner wall of the feed pipe 3, a sliding rod 158 is slidably installed on the surface of the sealing ring 157, a sealing plate 159 is fixedly installed on the top of the sliding rod 158, and a long rod 1510 is fixedly installed on the bottom of the sealing plate 159. Acetonitrile is intermittently fed for treatment to prevent excessive entry at one time, which causes the filter frame 8 molecular sieve plate 10 to be unable to effectively treat the acetonitrile, affecting the purity of the acetonitrile.

[0026] The hollow column 151 is arranged below the sliding plate 152. A No. 1 spring is arranged between the sliding plate 152 and the slide groove, and the sliding plate 152 is reset by the No. 1 spring. A No. 2 spring is arranged between the sealing ring 157 and the sliding rod 158, and the sliding rod 158 is reset by the No. 2 spring.

[0027] The anti-clogging device includes a fixed frame 161, a connecting frame 162, a rotating plate 163, a sliding seat 164, a protruding rod 165 and a protruding block 166. The fixed frame 161 is fixedly installed at the bottom of the circular ring plate 154, the connecting frame 162 is fixedly installed on the inner wall of the reaction vessel 1, the sliding seat 164 is slidably installed on the inner wall of the connecting frame 162, one end of the rotating plate 163 is rotatably installed on the inner wall of the fixed frame 161, and the other end of the rotating plate 163 is rotatably installed on the surface of the sliding seat 164, the protruding rod 165 is fixedly installed on the side of the sliding seat 164 away from the reaction vessel 1, and the protruding block 166 is fixedly installed on the circumferential surface of the filter frame 8. The vibration generated when the protruding block 166 contacts the protruding rod 165 will shake off the particles attached to the inside of the filter frame 8, thereby preventing the particles from clogging the filter frame 8 and affecting the separation effect.

[0028] A fixed connecting rod 167 is fixedly installed at the bottom of the sliding seat 164, a triangular block 168 is fixedly installed at the bottom of the fixed connecting rod 167, and a dome column 169 is fixedly installed on the top of the molecular sieve plate 10, which can enhance the contact time and contact area between the molecular sieve plate 10 and acetonitrile, prolong the contact time between the water molecules in the acetonitrile and the molecular sieve, increase the adsorption opportunity of the molecular sieve plate 10, and facilitate more efficient removal of moisture.

[0029] A No. 3 spring is provided between the sliding seat 164 and the connecting frame 162 , and the No. 3 spring drives the sliding seat 164 to return to its original position, so that the protruding rod 165 contacts the surface of the protruding block 166 .

[0030] A method for using a high-purity reagent acetonitrile intermittent pretreatment device comprises the following steps: Step 1: inject acetonitrile into the filter frame 8 through the feed pipe 3, start the motor 6, the motor 6 rotates to drive the fixed rod 7 to rotate, the fixed rod 7 rotates to drive the filter frame 8 to rotate, and the solid particles, impurities and insolubles in the acetonitrile are separated from the acetonitrile by the centrifugal force generated by the rotation of the filter frame 8, so as to prevent the solid particles, impurities and insolubles from affecting the purity of the acetonitrile; Step 2: The filter frame 8 rotates to drive the elastic telescopic rod 9 to rotate, and the elastic telescopic rod 9 rotates to drive the molecular sieve plate 10 to rotate. The molecular sieve plate 10 rotates to adsorb gas or liquid molecules, and absorbs moisture in acetonitrile to prevent moisture from affecting the concentration of acetonitrile. At the same time, the rotation can significantly increase the contact area between the adsorbent and the target molecules, thereby improving the adsorption effect; Step 3: Improve the treatment effect. At the same time, the fixed rod 7 rotates to drive the reciprocating thread groove 11 to rotate. The reciprocating thread groove 11 rotates to drive the thread plate 12 to reciprocate up and down. The up and down reciprocating movement of the thread plate 12 drives the circular screen plate 14 to reciprocate up and down. The up and down reciprocating movement of the circular screen plate 14 scrapes off the particles attached to the inner wall of the filter frame 8 to prevent the particles from clogging the filter frame 8 and affecting the filtering and separation effect of the filter frame 8. Step 4: The treated acetonitrile will enter the monitoring tank 5 through the discharge pipe 4. By detecting the water content of the acetonitrile, the adsorption effect of the molecular sieve plate 10 can be determined. If the water content in the acetonitrile is still high after treatment, it means that the molecular sieve plate 10 has lost its adsorption capacity and may need to be replaced or regenerated.

[0031] When the present embodiment is working, the threaded plate 12 moves upward to drive the hollow column 151 to move upward, the hollow column 151 moves upward to push the sliding plate 152 to move upward, the sliding plate 152 moves upward to drive the connecting rod 153 to move upward, the connecting rod 153 moves upward to drive the circular ring plate 154 to move upward, when the threaded plate 12 moves downward, the sliding plate 152 loses the push of the hollow column 151 and will reset under the action of the first spring, the sliding plate 152 moves downward to drive the connecting rod 153 and the circular ring plate 154 to move downward, and the circular ring plate 154 will reciprocate up and down to push the connecting rod 153 and the circular ring plate 154 to move downward. The acetonitrile on the inner wall of the container 1 is pushed downward onto the molecular sieve plate 10 to improve the adsorption effect. At the same time, the upward movement of the sliding plate 152 will drive the U-shaped rod 156 to move upward, and the upward movement of the U-shaped rod 156 will drive the long rod 1510 to move upward. The upward movement of the long rod 1510 will drive the sealing plate 159 to move upward. The upward movement of the sealing plate 159 will break away from the contact with the sealing ring 157, allowing the acetonitrile to flow into the filter frame 8, and be processed by intermittently feeding acetonitrile to prevent too much entering at one time, resulting in the inability of the molecular sieve plate 10 of the filter frame 8 to effectively process the acetonitrile, affecting the purity of the acetonitrile.

[0032] The upward movement of the annular plate 154 will drive the fixing frame 161 to move upward, the upward movement of the fixing frame 161 will drive the rotating plate 163 to move upward, the upward movement of the rotating plate 163 will pull the sliding seat 164 to move in the direction close to the inner wall of the reaction vessel 1, the movement of the sliding seat 164 in the direction close to the inner wall of the reaction vessel 1 will drive the protruding rod 165 to move in the direction close to the inner wall of the reaction vessel 1, the movement of the protruding rod 165 in the direction close to the inner wall of the reaction vessel 1 will break away from the contact with the protruding block 166, so as to prevent the protruding rod 165 from continuously contacting the protruding block 166 when the filter frame 8 drives the protruding block 166 to rotate, resulting in a reduction in the service life of the filter frame 8, and at the same time, the vibration generated when the protruding block 166 contacts the protruding rod 165 will shake off the particles attached to the inside of the filter frame 8, so as to prevent the particles from clogging the filter frame 8 and affecting the separation effect, and at the same time, the sliding seat 164 moves closer to the reaction vessel 1 will drive the fixed connecting rod 167 to move toward the inner wall of the reaction container 1, and the fixed connecting rod 167 to move toward the inner wall of the reaction container 1 will drive the triangular block 168 to move toward the inner wall of the reaction container 1, and the triangular block 168 to move toward the inner wall of the reaction container 1 is at the bottom of the dome column 169, and when the molecular sieve plate 10 rotates, the dome column 169 will be driven to rotate, and the rotation of the dome column 169 will contact the triangular block 168, and the triangular block 168 will push the dome column 169 to move downward, and the downward movement of the dome column 169 will drive the molecular sieve plate 10. By moving the molecular sieve plate 10 up and down, the contact time and contact area of ​​the molecular sieve plate 10 and acetonitrile can be enhanced, so that the contact time between the water molecules in the acetonitrile and the molecular sieve is prolonged, and the adsorption opportunity of the molecular sieve plate 10 is increased, which is conducive to more efficient removal of moisture.

[0033] Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and variations may be made to the embodiments without departing from the principles and spirit of the present invention, and that the scope of the present invention is defined by the appended claims and their equivalents.

Claims

1. A high-purity reagent acetonitrile intermittent pretreatment device, characterized in that, include: A reaction container (1), wherein a support frame (2) is fixedly mounted on the outer wall of the reaction container (1), a feed pipe (3) is fixedly mounted on the top of the reaction container (1), a discharge pipe (4) is fixedly mounted on the bottom of the reaction container (1), and a monitoring tank (5) is fixedly mounted on the bottom of the discharge pipe (4); A pretreatment device, the pretreatment device being arranged inside a reaction container (1), the pretreatment device comprising a motor (6), a fixing rod (7), a filter frame (8), an elastic telescopic rod (9), a molecular sieve plate (10), a reciprocating thread groove (11), a threaded plate (12), a fixing column (13) and a circular sieve plate (14), the motor (6) being fixedly mounted on the top of the reaction container (1), the fixing rod (7) being fixedly mounted on the output end of the motor (6), and the filter frame (8) being fixedly mounted on the bottom of the fixing rod (7). The elastic telescopic rod (9) is fixedly mounted on the bottom of the filter frame (8), the molecular sieve plate (10) is fixedly mounted on the free end of the elastic telescopic rod (9), the reciprocating thread groove (11) is formed on the circumferential surface of the fixed rod (7), the threaded plate (12) is threadedly mounted on the circumferential surface of the fixed rod (7), the fixed column (13) is fixedly mounted on the top of the inner wall of the reaction container (1), the fixed column (13) passes through the surface of the threaded plate (12), and the circular sieve plate (14) is fixedly mounted on the circumferential surface of the threaded plate (12); Wherein, the fixed column (13) is provided with an anti-adhesion device for preventing the solution from adhering to the inner wall of the reaction container (1), and the anti-adhesion device is provided with an anti-blocking device.

2. A high-purity reagent acetonitrile intermittent pretreatment device according to claim 1, characterized in that: The circular sieve plate (14) is in contact with the inner wall of the filter frame (8), and the molecular sieve plate (10) is arranged at the bottom of the filter frame (8).

3. A high-purity reagent acetonitrile intermittent pretreatment device according to claim 2, characterized in that: The anti-adhesion device comprises a hollow column (151), a sliding plate (152), a connecting rod (153), a circular ring plate (154) and a short rod (155), wherein the hollow column (151) is fixedly mounted on the top of the threaded plate (12), the hollow column (151) is slidably mounted on the surface of the fixed column (13), the surface of the fixed column (13) is provided with a sliding groove, the sliding plate (152) is slidably mounted on the inner wall of the sliding groove, the connecting rod (153) is fixedly mounted on the top of the sliding plate (152), the circular ring plate (154) is fixedly mounted on the bottom of the connecting rod (153), and the short rod (155) is fixedly mounted on the bottom of the circular ring plate (154).

4. A high-purity reagent acetonitrile intermittent pretreatment device according to claim 3, characterized in that: A U-shaped rod (156) is fixedly mounted on the surface of the sliding plate (152), a sealing ring (157) is fixedly mounted on the inner wall of the feed pipe (3), a sliding rod (158) is slidably mounted on the surface of the sealing ring (157), a sealing plate (159) is fixedly mounted on the top of the sliding rod (158), and a long rod (1510) is fixedly mounted on the bottom of the sealing plate (159).

5. A high-purity reagent acetonitrile intermittent pretreatment device according to claim 4, characterized in that: The hollow column (151) is arranged below the sliding plate (152), a No. 1 spring is arranged between the sliding plate (152) and the sliding groove, and a No. 2 spring is arranged between the sealing ring (157) and the sliding rod (158).

6. A high-purity reagent acetonitrile intermittent pretreatment device according to claim 5, characterized in that: The anti-clogging device comprises a fixed frame (161), a connecting frame (162), a rotating plate (163), a sliding seat (164), a convex rod (165) and a convex block (166); the fixed frame (161) is fixedly mounted on the bottom of the circular ring plate (154); the connecting frame (162) is fixedly mounted on the inner wall of the reaction container (1); the sliding seat (164) is slidably mounted on the inner wall of the connecting frame (162); one end of the rotating plate (163) is rotatably mounted on the inner wall of the fixed frame (161); the other end of the rotating plate (163) is rotatably mounted on the surface of the sliding seat (164); the convex rod (165) is fixedly mounted on a side of the sliding seat (164) away from the reaction container (1); and the convex block (166) is fixedly mounted on the circumferential surface of the filter frame (8).

7. A high-purity reagent acetonitrile intermittent pretreatment device according to claim 6, characterized in that: A fixed connecting rod (167) is fixedly mounted on the bottom of the sliding seat (164), a triangular block (168) is fixedly mounted on the bottom of the fixed connecting rod (167), and a dome column (169) is fixedly mounted on the top of the molecular sieve plate (10).

8. A high-purity reagent acetonitrile intermittent pretreatment device according to claim 7, characterized in that: A No. 3 spring is provided between the sliding seat (164) and the connecting frame (162), and the protruding rod (165) is in surface contact with the protruding block (166).

9. A method for using a high-purity reagent acetonitrile intermittent pretreatment device, using the high-purity reagent acetonitrile intermittent pretreatment device according to claim 8, characterized in that: The following steps are involved: Step 1: injecting acetonitrile into the filter frame (8) through the feed pipe (3), starting the motor (6), the motor (6) rotates to drive the fixed rod (7) to rotate, the fixed rod (7) rotates to drive the filter frame (8) to rotate, and the solid particles, impurities and insolubles in the acetonitrile are separated from the acetonitrile by the centrifugal force generated by the rotation of the filter frame (8), so as to prevent the solid particles, impurities and insolubles from affecting the purity of the acetonitrile; Step 2: The filter frame (8) rotates to drive the elastic telescopic rod (9) to rotate, and the rotation of the elastic telescopic rod (9) drives the molecular sieve plate (10) to rotate. The molecular sieve plate (10) rotates to adsorb gas or liquid molecules, thereby adsorbing water in acetonitrile to prevent the water from affecting the concentration of acetonitrile. At the same time, the rotation can significantly increase the contact area between the adsorbent and the target molecules, thereby improving the adsorption effect; Step 3: To improve the treatment effect, the fixed rod (7) rotates to drive the reciprocating thread groove (11) to rotate, the reciprocating thread groove (11) rotates to drive the thread plate (12) to move up and down, the thread plate (12) moves up and down to drive the circular screen plate (14) to move up and down, and the circular screen plate (14) moves up and down to scrape off the particles attached to the inner wall of the filter frame (8) through the up and down reciprocating movement, so as to prevent the particles from clogging the filter frame (8) and affecting the filtering and separation effect of the filter frame (8); Step 4: The treated acetonitrile will enter the monitoring tank (5) through the discharge pipe (4). By detecting the water content of the acetonitrile, the adsorption effect of the molecular sieve plate (10) can be determined. If the water content of the acetonitrile is still high after treatment, it means that the molecular sieve plate (10) has lost its adsorption capacity and needs to be replaced or regenerated.

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