A device and method for detecting the degree of polymerization of paraformaldehyde

By designing a paraformaldehyde polymerization degree detection device and combining a reasonable layout of the loading and processing components, convenient detection of paraformaldehyde polymerization degree is achieved, solving the problems of low efficiency and insufficient safety in the existing detection process, and improving the convenience and accuracy of detection.

CN122361704APending Publication Date: 2026-07-10HEBEI JIZHOU YINHE CHEM CO LTD
View PDF 2 Cites 0 Cited by

Patent Information

Application Number
CN202610671143.8
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2026-05-15
Publication Date
2026-07-10

AI Technical Summary

Technical Problem

Existing paraformaldehyde polymerization degree detection devices have failed to effectively combine the optimization and innovation of detection equipment, resulting in low efficiency and unreliability of the detection process.

Method used

A device for detecting the degree of polymerization of paraformaldehyde was designed, including a main frame, a loading component, a processing component, and an operating component. By rationally arranging reagent bottles and raw material bottles, and utilizing permanent magnet positioning, spring structure, and control valves, convenient sample transfer and reaction control are achieved, and detection is performed using iodometric titration.

Benefits of technology

It improves the convenience and safety of the testing operation, ensures the smooth progress of the reaction, provides a stable container and storage space, and enhances the efficiency and accuracy of the testing process.

✦ Generated by Eureka AI based on patent content.

Smart Images

  • Figure CN122361704A_ABST
    Figure CN122361704A_ABST
Patent Text Reader

Abstract

The application relates to the technical field of detection devices, and discloses a detection device and method for the polymerization degree of paraformaldehyde, which are combined with a special paraformaldehyde polymerization degree detection device, are specially designed for the polymerization degree detection working condition of paraformaldehyde, can provide convenient conditions for the polymerization degree detection operation, and have higher overall practicability. The device comprises multiple reagent bottles, multiple raw material bottles, a main frame, a load component rotatably connected to the main frame, a processing component, and an operation component. The multiple reagent bottles are arranged in the processing component, and the multiple raw material bottles are arranged in the load component. The operation component comprises a mounting plate and two fixed pipes. The mounting plate is fixedly connected to the main frame, and the two fixed pipes are rotatably connected to the mounting plate. Lifting pipes are slidably connected in the two fixed pipes, sampling pipes are slidably connected in the two lifting pipes, primary springs are fixedly connected between the lifting pipes and the fixed pipes, and secondary springs are fixedly connected between the sampling pipes and the lifting pipes.
Need to check novelty before this filing date? Find Prior Art

Description

Technical Field

[0001] This invention relates to the field of detection device technology, and specifically to a device and method for detecting the degree of polymerization of paraformaldehyde. Background Technology

[0002] As is well known, existing paraformaldehyde polymerization degree detection devices mainly consist of an analytical balance, reagent bottles, a constant temperature water bath, a burette, a volumetric flask, a light-proof standing container, and matching glassware. They can be used with a Karl Fischer moisture analyzer to detect free moisture. The sample dissolution, depolymerization, chemical reaction, and titration are completed by iodometric titration or sodium sulfite titration. Combined with formaldehyde content and moisture detection data, the average degree of polymerization of paraformaldehyde can be indirectly calculated.

[0003] A search revealed that Chinese patent application CN201910243791.3 discloses a method for detecting the degree of polymerization of paraformaldehyde. The main steps are as follows: Methanol (solvent and dispersant) is added to a reaction tank, paraformaldehyde is added, and the mixture is stirred thoroughly to obtain a mixed solution. The moisture content of mixed solution 1 is measured using a micro-moisture analyzer and recorded as h1. An additive is added to the mixed solution, and the mixture is stirred to obtain mixed solution 2. The moisture content of mixed solution 2 is measured using a micro-moisture analyzer and recorded as h2. The degree of polymerization of paraformaldehyde is then determined. The degree of polymerization value can be obtained. Chinese patent application number CN201910989633.2 discloses a method for detecting the degree of polymerization of sodium alginate oligosaccharides. It is roughly described as including the following steps: (1) preparing DNS (3,5-dinitrosalicylic acid) reagent, (2) preparing a series of oligosaccharide solutions of specific concentrations and the solution required for the standard curve, (3) preparing a series of oligosaccharide solutions, (4) taking the sodium alginate oligosaccharide solution from step (3), adding the DNS reagent, heating at 100°C for 5-10 min, and measuring its absorbance value at 540 nm, (5) obtaining the degree of polymerization of the sodium alginate oligosaccharide to be tested by the relationship curve between the percentage of reducing sugar content and the degree of polymerization.

[0004] While the aforementioned existing technical solutions can all be matched with their respective detection targets to form polymerization degree detection, this content only covers the relevant detection methods and does not specifically involve the detection equipment. Therefore, on the basis of ensuring the accuracy of paraformaldehyde polymerization degree detection, how to optimize and innovate the detection device is the core key to improving the efficiency of the detection process and ensuring the safety and reliability of the detection process. Summary of the Invention

[0005] To address the shortcomings of existing technologies, this invention provides a device and method for detecting the degree of polymerization of paraformaldehyde, which is used in conjunction with a dedicated paraformaldehyde degree of polymerization detection device. This detection device is specifically designed to adapt to the working conditions of paraformaldehyde degree of polymerization detection, providing convenient conditions for polymerization degree detection operations and enhancing overall practicality.

[0006] To achieve the above objectives, the present invention provides the following technical solution: a device for detecting the degree of polymerization of paraformaldehyde, comprising multiple reagent bottles and multiple raw material bottles, and a main frame. A loading component, a processing component, and an operating component are rotatably connected to the main frame. The multiple reagent bottles are disposed within the processing component, and the multiple raw material bottles are disposed within the loading component. The operating component includes a mounting plate and two fixing tubes. The mounting plate is fixedly connected to the main frame, and the two fixing tubes are rotatably connected to the mounting plate. A lifting tube is slidably connected within each of the two fixing tubes, and a sampling tube is slidably connected within each of the two lifting tubes. A primary spring is fixedly connected between the lifting tube and the fixing tube, and a secondary spring is fixedly connected between the sampling tube and the lifting tube. An absorption air bag and an injection quick-connect tube are respectively fixedly connected to the top ends of the two sampling tubes.

[0007] Preferably, the processing assembly includes a fixed tray and a rotating frame. The fixed tray is fixedly connected to the main frame, and the rotating frame is rotatably engaged with the main frame. The rotating frame is rotatably engaged between the fixed tray and the mounting plate. The rotating frame is provided with multiple fan-shaped processing stations, and processing frames are detachably installed in each of the multiple fan-shaped processing stations. Each of the multiple processing frames has an installation port, and a lifting cylinder adapted to the reagent bottle is slidably connected to each of the multiple installation ports. Conical springs are fixedly connected to the outside of each of the multiple lifting cylinders, and the multiple conical springs are respectively fixedly connected to the multiple processing frames. A passage is opened at the bottom end of the fixed tray, and a water bath is fixedly connected to the bottom end of the fixed tray. The water bath communicates with the passage. A downward limiting structure is installed in the main frame. The downward limiting structure is used to limit the downward push of the lifting cylinder into the water bath.

[0008] Preferably, the downward limiting structure includes a central operating column. The main frame has a guide opening, an extension bar opening, and a track bar opening. The central operating column is slidably fitted in the guide opening. The central operating column is fixedly connected to a drive plate and a limiting column. A transmission ring matching the drive plate is fixedly connected to the outside of each of the multiple lifting cylinders. The drive plate extends out of the main frame through the extension bar opening. The limiting column extends out of the main frame through the track bar opening. The limiting column is rotatably connected to a lifting frame. The lifting frame is fixedly connected to a limiting spring. The limiting spring is fixedly connected to a positioning frame. The positioning frame is rotatably connected to the main frame.

[0009] Preferably, the loading assembly includes a loading rotating frame, which is rotatably connected to the main frame. Multiple loading racks are detachably mounted inside the loading rotating frame. Each of the multiple loading racks has a guide insertion rack fixedly connected to it. Each of the multiple guide insertion racks has a limiting cylinder slidably connected to it. The bottom end of each of the multiple limiting cylinders is fixedly connected to a limiting spring. The multiple limiting springs are respectively fixedly connected to the multiple guide insertion racks. Multiple raw material bottles are respectively placed inside the multiple limiting cylinders. Each of the multiple loading racks has a positioning port, which is matched with the constricted neck section of the multiple raw material bottles. Each of the multiple loading racks is equipped with a cooperating valve, which is matched with the multiple lifting tubes.

[0010] Preferably, each of the plurality of cooperating valve components includes an outer frame, which is fixedly connected to the plurality of carrying racks. A first sealing cover and a second sealing cover are rotatably connected within each of the plurality of outer frames. An opening push block is slidably connected within each of the plurality of outer frames. A pointed block is fixedly connected to the lower end of each of the plurality of opening push blocks. A first sealing cover is provided with a first slope, and a second sealing cover is provided with a second slope. The first slope matches the pointed blocks, and the second slope matches the pointed blocks. A first return spring is fixedly connected to each of the plurality of first sealing covers, and the first return springs are fixedly connected within the plurality of outer frames. A second return spring is fixedly connected to each of the plurality of second sealing covers, and the second return springs are also fixedly connected within the plurality of outer frames.

[0011] Preferably, the top ends of both sampling tubes are fixedly connected to a holding auxiliary frame, and a stepped storage port is opened on the right-hand holding auxiliary frame. The absorption air bag is located in the storage port, and a pressure frame is provided on the absorption air bag. The quick-connect tube is equipped with a control valve, and the control valve is equipped with a press switch.

[0012] Preferably, the control valve includes an external inlet pipe, which is fixedly connected to the quick-connect inlet pipe. A transmission rod is fixedly connected to the bottom end of the push-button switch. A sliding seal is provided between the transmission rod and the external inlet pipe. A sealing disc is fixedly connected to the bottom end of the transmission rod. The sealing disc is slidably disposed inside the quick-connect inlet pipe. A liquid passage hole is provided on the sealing disc. An ejector spring is fixedly connected to the external inlet pipe. The ejector spring is fixedly connected to the push-button switch.

[0013] Preferably, both the rotating frame and the carrying frame are fixedly connected to multiple permanent magnets, and both the multiple processing frames and the multiple carrying frames are fixedly connected to iron blocks that can be magnetically attracted by the permanent magnets.

[0014] Preferably, all of the processing racks and the multiple carrying racks are provided with auxiliary operation slots.

[0015] A method for operating a paraformaldehyde polymerization degree detection device includes the following steps: S1. Inspect the entire device, place the reagent bottle containing the corresponding reagent into the processing component, and place the clean raw material bottle into the carrying component and adjust it to a position that is easy to operate. S2. Align the raw material bottle with the corresponding sampling tube, press the sampling tube and squeeze the absorption air bag to extract the sample. After releasing, the sampling tube will return to its original position, which can ensure that the extracted sample is stably stored in the sampling tube. S3. By rotating the processing component, the sampling tube is aligned with the reagent bottle, and the absorption air bag is squeezed to release the sample in the sampling tube, thus completing the transfer. S4. Adjust the reagent bottle to a stable reaction position, control the reaction temperature, humidity and time to ensure that the sample and reagent are fully mixed and reacted, repeat the above steps to complete the detection work of the entire detection process, and record the amount of liquid added in each step. S5. After the reaction is completed, the reaction reagents in the reagent bottle will be tested, and the corresponding data will be recorded in combination with the amount added at each step. The operation will be repeated with different samples to complete at least 3 sets of parallel tests. After each test, the relevant sampling components will be cleaned and the data will be recorded.

[0016] Compared with the prior art, the present invention provides a device and method for detecting the degree of polymerization of paraformaldehyde, which has the following beneficial effects: (1). In this invention, the supporting components provide basic storage space for multiple raw material bottles, which facilitates the storage of raw materials for testing.

[0017] (2). In this invention, through the coordinated cooperation of the processing components, a basic storage space is provided for multiple reagent bottles, while a stable container is provided for the detection reaction, ensuring the smooth progress of the reaction.

[0018] (3). In this invention, through the reasonable design of the operating components, not only can auxiliary reagents such as distilled water be added to the reagent bottle, but it is also convenient to add the detection raw materials in the raw material bottle to the reagent bottle, thereby improving the ease of operation. Attached Figure Description

[0019] Figure 1 This is a three-dimensional structural diagram of the entire invention; Figure 2 For the present invention Figure 1 A magnified schematic diagram of the partial structure at point A in the middle; Figure 3 This is a three-dimensional structural diagram of the cooperation between the carrier, the outer frame, and the first closing cover of the present invention; Figure 4 This is a partial cross-sectional three-dimensional structural schematic diagram of the cooperation of the carrier, the outer frame, and the first closing cover of the present invention; Figure 5 For the present invention Figure 4 A magnified schematic diagram of the local structure at point B; Figure 6 This is a partial cross-sectional three-dimensional structural schematic diagram of the cooperation of the carrier, guide insertion frame and limiting spring of the present invention; Figure 7 This is a three-dimensional structural diagram of the limiting cylinder of the present invention; Figure 8 This is a three-dimensional structural diagram of the reagent bottle, processing rack, and lifting cylinder of the present invention. Figure 9 This is a three-dimensional structural diagram of the cooperation between the lifting cylinder and the cone spring of the present invention; Figure 10 This is a three-dimensional structural schematic diagram showing a partial cross-section of the main frame, mounting plate, and gripping auxiliary frame of the present invention. Figure 11 For the present invention Figure 10 A magnified schematic diagram of the local structure at point C; Figure 12 This is a three-dimensional structural diagram of the invention viewed from below. Figure 13 For the present invention Figure 12 A magnified schematic diagram of the local structure at point D; Figure 14 This is a bottom-view three-dimensional structural diagram showing the cooperation of the main frame, mounting plate, and rotating frame of the present invention. Figure 15 This is a bottom-view three-dimensional structural diagram showing the cooperation of the main frame, mounting plate, and fixing pipe of the present invention; Figure 16 This is a three-dimensional structural diagram of the cooperation between the central operating column, drive plate, and limiting column of the present invention; Figure 17 This is a three-dimensional structural diagram of the processing frame, cone spring, and transmission ring of the present invention, viewed from below. Figure 18 This is a three-dimensional structural diagram of the relative interaction of the first sealing cover, the second sealing cover, and the opening push block of the present invention; Figure 19 This is a three-dimensional structural diagram of the main frame of the present invention.

[0020] In the diagram: 1. Reagent bottle; 2. Raw material bottle; 3. Main frame; 4. Mounting plate; 5. Fixing tube; 6. Lifting tube; 7. Sampling tube; 8. Primary spring; 9. Secondary spring; 10. Absorption air bag; 11. Quick-connect tube; 12. Fixing tray; 13. Rotating frame; 14. Processing frame; 15. Lifting cylinder; 16. Conical spring; 17. Central operating column; 18. Drive plate; 19. Limiting column; 20. Transmission ring; 21. Lifting rotating frame; 22. Limiting sleeve spring; 23. Positioning rotating frame; 24. Loading rotating frame; 25. Loading... 26. Shelf; 27. Guide insertion frame; 28. Limiting cylinder; 29. ​​Limiting spring; 30. Positioning port; 31. Outer frame; 32. First sealing cover; 33. Second sealing cover; 34. Opening push block; 35. Pointed block; 36. First slope; 37. Second slope; 38. First return spring; 39. Second return spring; 40. Pressing frame; 41. Grip auxiliary frame; 42. Press switch; 43. Outer guide tube; 44. Transmission rod; 45. Sealing plate; 46. Permanent magnet; 47. Iron block; 48. Auxiliary operation slot. Detailed Implementation

[0021] The technical solutions of the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings. Obviously, the described embodiments are only some embodiments of the present invention, and not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by those skilled in the art without creative effort are within the scope of protection of the present invention.

[0022] For examples, please refer to Figures 1-19A device for detecting the degree of polymerization of paraformaldehyde includes multiple reagent bottles 1 and multiple raw material bottles 2, and a main frame 3. A carrying component, a processing component, and an operating component are rotatably connected to the main frame 3. The multiple reagent bottles 1 are disposed within the processing component, and the multiple raw material bottles 2 are disposed within the carrying component. The operating component includes a mounting plate 4 and two fixing tubes 5. The mounting plate 4 is fixedly connected to the main frame 3, and the two fixing tubes 5 are rotatably connected to the mounting plate 4. A lifting tube 6 is slidably connected within each of the two fixing tubes 5, and a sampling tube 7 is slidably connected within each of the two lifting tubes 6. A primary spring 8 is fixedly connected between the lifting tube 6 and the fixing tube 5. The sampling tube 7 is connected to the lifting tube 6. A secondary spring 9 is fixedly connected between tubes 6. The top ends of the two sampling tubes 7 are respectively fixedly connected to an absorption air bag 10 and an addition quick-connect tube 11. Through the reasonable design of the operating components, not only can auxiliary reagents such as distilled water be added to reagent bottle 1, but it is also convenient to add the detection raw material in raw material bottle 2 to reagent bottle 1, improving the ease of operation. The processing component includes a fixed support plate 12 and a rotating frame 13. The fixed support plate 12 is fixedly connected to the main frame 3. The rotating frame 13 is rotatably engaged with the main frame 3, and the rotating frame 13 is rotatably engaged between the fixed support plate 12 and the mounting plate 4. The rotating frame 13 is provided with multiple fan-shaped processing stations, and processing frames 14 can be detachably installed in each of the multiple fan-shaped processing stations. Each of the processing racks 14 has an installation port, and a lifting cylinder 15 adapted to the reagent bottle 1 is slidably connected to each of the installation ports. Conical springs 16 are fixedly connected to the outside of each of the lifting cylinders 15, and each of the conical springs 16 is fixedly connected to the processing racks 14. A passage opening is provided at the bottom end of the fixed support plate 12, and a water bath is fixedly connected to the bottom end of the fixed support plate 12. The water bath communicates with the passage opening. A downward limiting structure is installed inside the main frame 3. The downward limiting structure includes a central operating column 17. The main frame 3 has a guide opening, an extension strip opening, and a track strip opening. The central operating column 17 is slidably fitted within the guide opening and is fixedly connected to a drive plate 18 and... The limiting post 19 and the multiple lifting cylinders 15 are all fixedly connected to a transmission ring 20 that matches the drive plate 18. The drive plate 18 extends to the outside of the main frame 3 through the extension strip opening. The limiting post 19 extends to the outside of the main frame 3 through the track strip opening. The limiting post 19 is rotatably connected to the lifting frame 21. The lifting frame 21 is fixedly connected to the limiting sleeve spring 22. The limiting sleeve spring 22 is fixedly connected to the positioning frame 23. The positioning frame 23 is rotatably connected to the main frame 3. The downward limiting structure is used to limit the downward movement of the lifting cylinder 15 into the water bath. Through the coordinated cooperation of the processing components, a basic storage space is provided for multiple reagent bottles 1. At the same time, it can provide a stable container for the detection reaction and ensure the smooth progress of the reaction.

[0023] It should be further explained that the loading assembly includes a loading rotating frame 24, which is rotatably connected to the main frame 3. Multiple loading racks 25 are detachably installed within the loading rotating frame 24. Each of the multiple loading racks 25 has a guide insertion rack 26 fixedly connected to it. Each of the multiple guide insertion racks 26 has a slidably connected limit cylinder 27. The bottom end of each of the multiple limit cylinders 27 is fixedly connected to a limit spring 28. The multiple limit springs 28 are respectively fixedly connected within the multiple guide insertion racks 26. Multiple raw material bottles 2 are respectively placed within the multiple limit cylinders 27. Each of the multiple loading racks 25 has a positioning port 29, which matches the constricted neck section of each of the multiple raw material bottles 2. Each of the multiple loading racks 25 has... Each of the multiple coordinating valves is equipped with a coordinating valve component, which is respectively matched with a plurality of lifting pipes 6. Each of the multiple coordinating valve components includes an outer frame 30, which is respectively fixedly connected to a plurality of carrying racks 25. A first sealing cover 31 and a second sealing cover 32 are rotatably connected within each of the multiple outer frame 30. An opening push block 33 is slidably connected within each of the multiple outer frame 30. A pointed block 34 is fixedly connected to the lower end of each of the multiple opening push blocks 33. Each of the multiple first sealing covers 31 is provided with a first slope 35, and each of the multiple second sealing covers 32 is provided with a second slope 36. Each of the multiple first slopes 35 is matched with a plurality of pointed blocks 34, and each of the multiple second slopes 36 is also matched with a plurality of pointed blocks 34. Each of the 31 components is fixedly connected to a first return spring 37. Multiple first return springs 37 are respectively fixedly connected to multiple outer mounting frames 30. Multiple second sealing caps 32 are fixedly connected to second return springs 38, which are also respectively fixedly connected to multiple outer mounting frames 30. Through the matching of the carrying components, basic storage space is provided for multiple raw material bottles 2, facilitating the storage of raw materials for testing. The tops of both sampling tubes 7 are fixedly connected to a holding auxiliary frame 40. One of the holding auxiliary frames 40 on the right side has a stepped storage opening. The absorption airbag 10 is located inside the storage opening. The absorption airbag 10 is equipped with a pressing frame 39. The quick-connect fitting 11 is equipped with a control valve, which is equipped with a push-button switch 41. The control valve includes an external inlet pipe 42, which is fixedly connected to the quick-connect inlet pipe 11. A transmission rod 43 is fixedly connected to the bottom end of the push-button switch 41. A sliding seal is provided between the transmission rod 43 and the external inlet pipe 42. A sealing disc 44 is fixedly connected to the bottom end of the transmission rod 43. The sealing disc 44 is slidably disposed within the quick-connect inlet pipe 11 and has a liquid passage hole. A push-out spring is fixedly connected to the external inlet pipe 42 and is fixedly connected to the push-button switch 41. During operation, the palm of one hand, using the four fingers excluding the thumb, assists in gripping the holding bracket 40, and the thumb is used to press the pressing bracket 39 or the push-button switch 41 to compress the absorption airbag 10 or adjust the control valve.Both the rotating frame 13 and the carrying frame 24 are fixedly connected to multiple permanent magnets 45. Each of the multiple processing frames 14 and multiple carrying frames 25 is fixedly connected to an iron block 46 that can be magnetically attracted by the permanent magnets 45. Through the magnetic attraction between the permanent magnets 45 and the iron blocks 46, the processing frame 14 can be easily positioned magnetically relative to the rotating frame 13, and the carrying frame 25 can also be easily positioned magnetically relative to the carrying frame 24. Each of the multiple processing frames 14 and multiple carrying frames 25 is provided with an auxiliary operation slot 47 for assisting in gripping and applying force during installation.

[0024] A method for operating a paraformaldehyde polymerization degree detection device includes the following steps: First, inspect the entire device. Place the reagent bottle 1, pre-filled with the corresponding reagent, into the processing component. Place the clean raw material bottle 2 into the carrying component and adjust it to a convenient operating position. Then, align the raw material bottle 2 with the corresponding sampling tube 7, press the sampling tube 7 and squeeze the absorption bladder 10 to extract the sample. After releasing, the sampling tube 7 returns to its original position, ensuring that the extracted sample is stably stored in the sampling tube 7. Then, by rotating the processing component, align the sampling tube 7 with the reagent bottle 1 and squeeze the absorption bladder 10 to release the sample in the sampling tube 7, completing the transfer. Next, adjust the reagent bottle 1 to a stable reaction position, control the reaction temperature, humidity, and time to ensure that the sample and reagent are fully mixed and reacted. Repeat the aforementioned steps to complete the detection operation of the entire detection process. Record the amount added in each step. After the reaction is completed, test the reaction reagent in the reagent bottle 1 and record the corresponding data in conjunction with the amount added in each step. Repeat the operation with a different sample to complete at least three sets of parallel tests. After each test, clean the sampling-related components and record the data.

[0025] In summary, this method for detecting the degree of polymerization of paraformaldehyde is based on the iodometric titration method for determining formaldehyde content. The entire process is completed using the paraformaldehyde degree of polymerization detection device of this invention. The core principle is that paraformaldehyde depolymerizes into formaldehyde monomers under specific conditions, reacts with excess iodine in an alkaline environment, and the remaining iodine is acidified and titrated with a sodium thiosulfate standard solution. The formaldehyde mass fraction is calculated by the difference between the blank control test results. The average degree of polymerization of paraformaldehyde is then calculated by combining the sample free water content (measured by Karl Fischer method). Before testing, a quick-connect fitting 11 is added to connect to an external distilled water guide tube. Distilled water is introduced into the distilled water guide tube. The device is checked and reagents are prepared. Reagent preparation must strictly adhere to standard concentration requirements, specifically including iodine standard solution (…). 0.1 mol / L), sodium thiosulfate standard solution ( =0.1mol / L), sodium hydroxide solution (2mol / L), sulfuric acid solution (1+8 volume ratio), and 1% starch indicator (must be prepared and used immediately to avoid expiration). After all reagents are prepared, they should be properly stored in multiple raw material bottles 2. Place the raw material bottles 2 into the rotating rack 24. During the placement process, press the limiting cylinder 27 to elastically compress the limiting spring 28, so that there is enough height space between the limiting cylinder 27 and the rack 25 to allow the raw material bottles 2 to be inserted. After placing the raw material bottles 2 into the limiting cylinder 27, release it. The downward pressure applied to the limiting cylinder 27, under the elastic reset action of the limiting spring 28, pushes the raw material bottle 2 upward, eventually causing the bottle mouth of the raw material bottle 2 to enter the positioning port 29. The positioning of the raw material bottle 2 is achieved through the limiting spring 28 and the positioning port 29, and the reagent bottle 1 is installed into the lifting cylinder 15. After the reagent bottle 1 and the raw material bottle 2 are installed, the relative positioning between the processing rack 14 and the rotating rack 13 is achieved through the magnetic attraction between the permanent magnet 45 and the iron block 46, and the relative positioning between the carrying rack 25 and the carrying rotating rack 24 is also achieved.

[0026] Furthermore, using an analytical balance, accurately weigh 0.15–0.20 g of paraformaldehyde sample (accurate to 0.0001 g), remove reagent bottle 1 from the lifting cylinder 15, place the weighed sample into reagent bottle 1, and then place reagent bottle 1 back into the removed lifting cylinder 15. Reposition the processing rack 14 relative to the rotating rack 13. Add 50 mL of distilled water to reagent bottle 1 through the sampling tube 7 connected to the quick-connect fitting 11. During the addition process, press the pressure switch 41 to drive the sealing plate 44 down, connecting the liquid passage to the quick-connect fitting 11, adding distilled water to reagent bottle 1. Then, rotate the rotating rack 13 to align the lifting cylinder 15 with the passage above the water bath, and push down the central operating column 17. The process of the central operating column 17 falling... The drive plate 18 pushes the transmission ring 20, causing the lifting cylinder 15 to slide down along the mounting port of the processing rack 14 with the reagent bottle 1 until the reagent bottle 1 is partially immersed in the water bath. During the adjustment process, the lifting frame 21 rotates accordingly. The limiting sleeve spring 22 and the positioning frame 23 are used to achieve the auxiliary limiting of the fixed limiting column 19, thereby achieving the downward limit of the lifting cylinder 15. During the heating process, the temperature of the water bath should be controlled ≤60℃ to avoid excessive temperature leading to formaldehyde volatilization loss and to improve the safety of the test. After depolymerization is completed, the central operating column 17 is pulled up to reset the lifting cylinder 15 under the action of the cone spring 16. After the lifting cylinder 15 has completed the reset, the rotating frame 13 is rotated to align the through hole on the rotating frame 13 that matches the sampling tube 7 with the sampling tube on the right side. 7. Rotate and adjust the loading rack 24 so that the corresponding raw material bottle 2 inside the loading rack 24 rotates to directly below the sampling tube 7, so that the sampling tube 7 can take samples subsequently. After adjustment, hold the gripping auxiliary frame 40 corresponding to the sampling tube 7 on the right. By adjusting the height of the gripping auxiliary frame 40, the lifting tube 6 and the sampling tube 7 are driven downward. The corresponding primary spring 8 and secondary spring 9 will be compressed synchronously. Since the elastic force of the primary spring 8 is greater than that of the secondary spring 9, the lifting tube 6 will first move downward relative to the fixed tube 5. During this process, although the sampling tube 7 will partially fall relative to the lifting tube 6, the sampling tube 7 will not protrude from the lower end of the lifting tube 6 when the lifting tube 6 falls. When the lifting tube 6 is inserted into the corresponding outer frame 30, it will... The opening pusher 33 is pressed down, and as it falls, the pointed block 34 at its bottom falls simultaneously. With the cooperation of the pointed block 34, the first and second slopes 35 and 36, the first and second sealing caps 31 and 32 rotate and open synchronously, providing a passage for the sampling tube 7. After the first and second sealing caps 31 and 32 are fully open, the lifting tube 6 is inserted to its limit relative to the outer frame 30. Then, the gripping auxiliary frame 40 is pressed down further, and the lifting tube 6 stops falling. The sampling tube 7 then protrudes from the bottom of the lifting tube 6 and enters the corresponding reagent bottle 1. After the sampling tube 7 enters the reagent bottle 1, the thumb is bent to press down on the actuating frame 39, squeezing the absorption airbag 10.Appropriately squeeze the absorption airbag 10 to draw out the solution to be added. After drawing, release the downward pressure acting on the gripping auxiliary frame 40, allowing the sampling tube 7 to be drawn out of the reagent bottle 1. Simultaneously, the lifting tube 6 returns to its original position relative to the fixed tube 5. When the lifting tube 6 rises relative to the outer frame 30, the downward pushing force acting on the opening push block 33 becomes ineffective, and the first sealing cap 31 and the second sealing cap 32 will rotate relative to each other and close, thus reducing the evaporation loss of the reagent in the reagent bottle 1 and improving operational safety.

[0027] Repeat the above steps. First, extract 25.00 mL of 0.1 mol / L iodine solution and store it in sampling tube 7. Then, rotate and adjust the rotating frame 13 so that sampling tube 7 is aligned with the mouth of reagent bottle 1. Next, squeeze the absorption bladder 10 to slowly release the iodine solution into reagent bottle 1, completing the iodine addition. Then, extract 10 mL of 2 mol / L sodium hydroxide solution and add it. After the addition is complete, place reagent bottle 1 back into the water bath, strictly control the reaction temperature and keep it at a constant temperature for 10 minutes. Strictly control the reaction time to avoid detection errors caused by time deviation. After the reaction is complete, extract 15 mL of 1+8 sulfuric acid solution through sampling tube 7 on the right and add it to reagent bottle 1 for acidification. After acidification, extract 0.1 mol / L thiocyanate solution. Add sodium thiosulfate standard solution slowly to reagent bottle 1 until the solution turns pale yellow, then stop titrating. Add 2-3 mL of 1% starch indicator through sampling tube 7 on the right, and continue titrating until the blue color just fades, which is the titration endpoint. Record the volume V1 of sodium thiosulfate standard solution consumed at this point. Simultaneously, perform a blank test, following the same procedure as the sample test, except without adding paraformaldehyde sample. All other reagent volumes and reaction conditions remain the same. Record the volume V0 of sodium thiosulfate standard solution consumed in the blank test. After titration, further process the reaction reagents in reagent bottle 1. After recording the test data, calculate the formaldehyde mass fraction and the degree of polymerization of paraformaldehyde according to the corresponding formulas. The formula for calculating the formaldehyde mass fraction w is: In the formula, c is the concentration of sodium thiosulfate standard solution (mol / L), V0 is the volume of sodium thiosulfate standard solution consumed in the blank test (mL), V1 is the volume of sodium thiosulfate standard solution consumed in the sample titration (mL), m is the weight of the paraformaldehyde sample (g), 0.03003 is the formaldehyde molar mass conversion factor, and the formula for calculating the degree of polymerization n of paraformaldehyde is: In the formula The free water content of the sample was measured using a Karl Fischer moisture analyzer. If a moisture analyzer is unavailable, a rough calculation can be performed, approximating the free water content. In this case, the formula for calculating the degree of polymerization can be simplified to: Throughout the testing process, key precautions must be strictly followed. Because iodine is volatile and decomposes in light, reagent bottle 1 is stored on the processing rack 14. Enclosed by the mounting plate 4, rotating frame 13, and fixed support plate 12, it is relatively isolated from the external space, improving the safety of the testing operation. The water bath temperature is always controlled below 60℃ to avoid formaldehyde volatilization affecting the test results. The reaction time after adding alkali is strictly controlled to 10 minutes; too long or too short a time will lead to significant errors. The starch indicator must be added near the titration endpoint, not at the beginning, to prevent starch from adsorbing iodine and affecting titration accuracy. To ensure the reliability of the test results, two parallel tests are required, and the test results are only valid if the parallel deviation is ≤0.3%. Repeat all the above operations when changing samples, completing at least three sets of parallel tests. After each test, the relevant sampling components must be thoroughly cleaned, and all test data must be recorded in detail to ensure data integrity and traceability. After the test, reagent bottle 1 and raw material bottle 2 are removed from the device, cleaned, and properly stored. The relevant power is turned off, and the testing device is tidied up to complete the entire paraformaldehyde polymerization degree test. To ensure the creation of a good reaction environment, the mounting plate 4, fixed support plate 12, rotating frame 13, and processing frame 14 are all made of opaque material. In order to observe the test operation process, a camera can be added inside the processing frame 14, and a display screen is provided for the camera. The camera's imaging area is matched with the reagent bottle 1 inside the processing frame 14. Through the display screen, the real-time status of the target substance inside the reagent bottle 1 captured by the camera can be observed in real time, so as to facilitate real-time observation of the test operation process.

[0028] Although embodiments of the invention have been shown and described, it will be understood by those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the invention, the scope of which is defined by the appended claims and their equivalents.

Claims

1. A device for detecting the degree of polymerization of paraformaldehyde, comprising multiple reagent bottles (1) and multiple raw material bottles (2), characterized in that, It also includes a main frame (3), on which a loading component, a processing component and an operating component are rotatably connected. Multiple reagent bottles (1) are disposed in the processing component, and multiple raw material bottles (2) are disposed in the loading component. The operating component includes a mounting plate (4) and two fixing tubes (5). The mounting plate (4) is fixedly connected to the main frame (3), and the two fixing tubes (5) are rotatably connected to the mounting plate (4). A lifting tube (6) is slidably connected inside each of the two fixing tubes (5), and a sampling tube (7) is slidably connected inside each of the two lifting tubes (6). A primary spring (8) is fixedly connected between the lifting tube (6) and the fixing tube (5), and a secondary spring (9) is fixedly connected between the sampling tube (7) and the lifting tube (6). An absorption air bag (10) and an addition quick-connect tube (11) are fixedly connected to the top of each of the two sampling tubes (7).

2. The device for detecting the degree of polymerization of paraformaldehyde according to claim 1, characterized in that, The processing assembly includes a fixed tray (12) and a rotating frame (13). The fixed tray (12) is fixedly connected to the main frame (3), and the rotating frame (13) is rotatably engaged with the main frame (3). The rotating frame (13) is rotatably engaged between the fixed tray (12) and the mounting plate (4). The rotating frame (13) is provided with multiple fan-shaped processing stations. Each of the multiple fan-shaped processing stations can be detachably equipped with a processing frame (14). Each of the multiple processing frames (14) has an installation port. Each of the multiple lifting cylinders (15) is slidably connected to a lifting cylinder (1), and each of the multiple lifting cylinders (15) is fixedly connected to a conical spring (16). The multiple conical springs (16) are respectively fixedly connected to the multiple processing racks (14). The bottom end of the fixed tray (12) is provided with a passage opening. The bottom end of the fixed tray (12) is fixedly connected to a water bath. The water bath is connected to the passage opening. The main frame (3) is equipped with a downward limiting structure. The downward limiting structure is used to limit the downward movement of the lifting cylinder (15) into the water bath.

3. The device for detecting the degree of polymerization of paraformaldehyde according to claim 2, characterized in that, The downward limiting structure includes a central operating column (17). The main frame (3) is provided with a guide port, an extension bar port and a track bar port. The central operating column (17) is slidably fitted in the guide port. The central operating column (17) is fixedly connected to a drive plate (18) and a limiting column (19). A transmission ring (20) matching the drive plate (18) is fixedly connected to the outside of the multiple lifting cylinders (15). The drive plate (18) extends out of the main frame (3) through the extension bar port. The limiting column (19) extends out of the main frame (3) through the track bar port. The limiting column (19) is rotatably connected to a lifting frame (21). The lifting frame (21) is fixedly connected to a limiting sleeve spring (22). The limiting sleeve spring (22) is fixedly connected to a positioning frame (23). The positioning frame (23) is rotatably connected to the main frame (3).

4. The device for detecting the degree of polymerization of paraformaldehyde according to claim 3, characterized in that, The loading assembly includes a loading frame (24), which is rotatably connected to the main frame (3). Multiple loading frames (25) are detachably installed inside the loading frame (24). Each of the multiple loading frames (25) is fixedly connected to a guide insertion frame (26). Each of the multiple guide insertion frames (26) is slidably connected to a limit cylinder (27). The bottom end of each of the multiple limit cylinders (27) is fixedly connected to a limit spring (28). Each of the multiple limit springs (28) is fixedly connected to the multiple guide insertion frames (26). Multiple raw material bottles (2) are placed inside the multiple limit cylinders (27). Each of the multiple loading frames (25) has a positioning port (29). Each of the multiple positioning ports (29) matches the necked section of the bottle mouth of each of the multiple raw material bottles (2). Each of the multiple loading frames (25) is equipped with a cooperating valve. Each of the multiple cooperating valves matches the multiple lifting pipes (6).

5. The device for detecting the degree of polymerization of paraformaldehyde according to claim 4, characterized in that, Each of the aforementioned coordinating valve components includes an outer frame (30), which is fixedly connected to a plurality of the aforementioned shelves (25). A first sealing cover (31) and a second sealing cover (32) are rotatably connected within each of the outer frames (30). An opening push block (33) is slidably connected within each of the outer frames (30). A pointed block (34) is fixedly connected to the lower end of each of the multiple opening push blocks (33). Each of the multiple first sealing covers (31) is provided with a first slope (35), and each of the multiple second sealing covers (32) is provided with a second slope (35). The slope (36), the multiple first slopes (35) are respectively matched with the multiple pointed blocks (34), the multiple second slopes (36) are also respectively matched with the multiple pointed blocks (34), the multiple first closed covers (31) are all fixedly connected with the first return springs (37), the multiple first return springs (37) are respectively fixedly connected in the multiple outer frames (30), the multiple second closed covers (32) are fixedly connected with the second return springs (38), the multiple second return springs (38) are also respectively fixedly connected in the multiple outer frames (30).

6. The device for detecting the degree of polymerization of paraformaldehyde according to claim 5, characterized in that, The top ends of both sampling tubes (7) are fixedly connected to a gripping auxiliary frame (40). A stepped storage port is opened on one of the gripping auxiliary frames (40) on the right side. The absorption air bag (10) is located in the storage port. The absorption air bag (10) is equipped with a pressing frame (39). The quick-connect pipe (11) is equipped with a control valve. The control valve is equipped with a press switch (41).

7. The device for detecting the degree of polymerization of paraformaldehyde according to claim 6, characterized in that, The control valve includes an external inlet pipe (42), which is fixedly connected to the quick-connect pipe (11). A transmission rod (43) is fixedly connected to the bottom end of the push switch (41). A sliding seal is provided between the transmission rod (43) and the external inlet pipe (42). A sealing disc (44) is fixedly connected to the bottom end of the transmission rod (43). The sealing disc (44) is slidably disposed in the quick-connect pipe (11). A liquid passage hole is provided on the sealing disc (44). A push-out spring is fixedly connected to the external inlet pipe (42). The push-out spring is fixedly connected to the push switch (41).

8. The device for detecting the degree of polymerization of paraformaldehyde according to claim 7, characterized in that, The rotating frame (13) and the carrying frame (24) are each fixedly connected to a plurality of permanent magnets (45), and the plurality of processing frames (14) and the plurality of carrying frames (25) are each fixedly connected to an iron block (46) that can be magnetically attracted by the permanent magnets (45).

9. The device for detecting the degree of polymerization of paraformaldehyde according to claim 8, characterized in that, Each of the processing racks (14) and the multiple storage racks (25) is provided with an auxiliary operation slot (47).

10. A method for operating a device for detecting the degree of polymerization of paraformaldehyde, characterized in that, The method for detecting the degree of polymerization of paraformaldehyde according to any one of claims 1-9 includes the following steps: S1. Inspect the entire device, put the reagent bottle (1) containing the corresponding reagent into the processing component, put the clean raw material bottle (2) into the carrying component and adjust it to a position that is easy to operate. S2. Align the raw material bottle (2) with the corresponding sampling tube (7), press the sampling tube (7) and squeeze the absorption air bag (10) to extract the sample. After releasing, the sampling tube (7) will reset, which can ensure that the extracted sample is stably stored in the sampling tube (7). S3. By rotating the processing component, the sampling tube (7) is aligned with the reagent bottle (1), and the absorption air bag (10) is squeezed to release the sample in the sampling tube (7) to complete the transfer. S4. Adjust the reagent bottle (1) to a stable reaction position, control the reaction temperature, humidity and time, ensure that the sample and reagent are fully mixed and reacted, repeat the above steps to complete the detection operation of the entire detection process, and record the amount of drops added in each step; S5. After the reaction is completed, the reaction reagent in the reagent bottle (1) will be tested, and the corresponding data will be recorded in combination with the amount added in each step. The sample will be replaced and the operation will be repeated to complete at least 3 sets of parallel tests. After each test, the relevant parts of the sample will be cleaned and the data will be recorded.

Citation Information

Patent Citations

  • Method for detecting polymerization degree of paraformaldehyde

    CN109884245A

  • Method for detecting polymerization degree of sodium alginate oligosaccharide

    CN112683888A