A high-stability povidone-iodine preparation and preparation method thereof

By optimizing the reaction process and equipment design of povidone iodine preparations, the problems of high energy consumption, poor stability and low manual detection efficiency in the prior art are solved, and the povidone iodine with high stability, low energy consumption and high efficiency detection are achieved Preparation production.

CN118634188BActive Publication Date: 2025-02-11SHANGHAI CONSON BIOLOGICAL TECH +1
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Patent Information

Application Number
CN202410767613.1
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2024-06-14
Publication Date
2025-02-11
Estimated Expiration
2044-06-14

AI Technical Summary

Technical Problem

The existing povidone iodine preparations have problems such as high energy consumption, long reaction temperature and time, poor stability and low manual screening efficiency during the production process. The chemical bottles are prone to damage during the filling process and low manual detection efficiency.

Method used

High stability povidone iodine preparation using polyvinylpyrrolidone K30, essence iodine, ethanol, potassium iodide, organic acids and surfactants, through the optimization of reaction process and equipment design, including the use of the first and second reaction tanks , stirring and cooling systems, and filling and testing units to realize automated filling and testing.

Benefits of technology

The stability and iodine conversion rate of povidone iodine preparations are improved, energy consumption and reaction time are reduced, production efficiency and product quality are improved, and the filling and detection efficiency is greatly improved through automated filling and testing systems.

✦ Generated by Eureka AI based on patent content.

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Abstract

The invention discloses a high-stability povidone-iodine preparation, including polyvinylpyrrolidone K30 15.0%-25.0%, refined iodine 10.0%-12.0%, ethanol 20.0%-30.0%, potassium iodide 2.0-4.0%, organic acid 0.1-1.0%, organic acid salt 0.1-2.0%, surfactant 1.0%-3.0%, stabilizer 1.0%-5.0%, and the rest is water. Compared with the prior art, the invention has the beneficial effects that the povidone-iodine preparation obtained by the invention has good stability, low reaction temperature during the reaction, short total reaction time (only 4h-6h), high iodine yield (low degradation rate), can improve production efficiency, and reduce production energy consumption.
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Description

Technical Field

[0001] The invention relates to the technical field of disinfectants, and in particular to a high-stability povidone-iodine preparation and a preparation method thereof. Background Art

[0002] Povidone-iodine is a complex of polyvinylpyrrolidone and iodine. It is a non-ionic iodine tincture with active iodine as the main bactericidal ingredient. It has a strong killing effect on bacteria, viruses, fungi, molds and spores. It is currently the most widely used and safest antibacterial disinfectant. It has the characteristics of high efficiency, broad spectrum, low irritation, no toxic side effects, no residue and no drug resistance. It is included in major pharmacopoeias in the world and has been included in the 1990 edition of the Chinese Pharmacopoeia.

[0003] The bactericidal mechanism of povidone-iodine is as follows: the polymer carrier povidone has an affinity for the cell membrane and adsorbs on the cell membrane. At the same time, it transports the complexed iodine to the cell membrane and releases free iodine, destroying the protein structure of the cell membrane, causing the cell membrane permeability to increase. The free iodine enters the cell and directly oxidizes the active groups in the bacterial protoplasmic protein, destroying the internal structure of the cell, inhibiting the activity of respiratory enzymes, and causing obstacles to bacterial energy metabolism. At the same time, it also causes abnormal activity of various enzymes required for bacterial metabolism and proliferation, such as lactate dehydrogenase and RNA transcriptase in the bacteria, leading to DNA replication and transcription disorders, and ultimately killing the bacteria. When the free iodine is consumed, it can be continuously replenished from the complexed povidone-iodine.

[0004] Polyvinylpyrrolidone, referred to as PVP, is a non-ionic polymer compound and the most distinctive raw material among N-vinylamide polymers. PVP is divided into four grades according to its average molecular weight, which is usually expressed by K value. Different K values ​​represent the corresponding average molecular weight range of PVP. K value is actually a characteristic value related to the relative viscosity of PVP aqueous solution, and viscosity is a physical quantity related to the molecular weight of polymer. Therefore, K value can be used to characterize the average molecular weight of PVP. Generally, the larger the K value, the greater the viscosity and the stronger the adhesion.

[0005] Existing povidone-iodine preparations are often prepared using polyvinyl pyrrolidone K30 and iodine as raw materials. The mixture of polyvinyl pyrrolidone K30 and iodine is maintained at a temperature of 60-80°C for 14-18 hours under stirring for reaction. There are problems such as high reaction temperature, long reaction time, and high energy consumption. At the same time, the prepared povidone-iodine solution has obvious batch differences (pH, effective iodine content, stability) and the like.

[0006] At the same time, during the production process of vinfoam iodine preparations, the medicine needs to be injected into the medicine bottle through a filling mechanism. During the injection process, the medicine bottle may be impacted, causing damage to the medicine bottle. After the medicine is injected, a stopper will be inserted into the bottle mouth to seal it. The stopper may not be pressed into place. Therefore, subsequent manual inspection is required to remove defective products. The manual screening efficiency in the existing technology is low and cannot meet the needs of large-scale mass production. Summary of the invention

[0007] In order to solve the problems mentioned in the above background technology, the present invention provides a high-stability povidone-iodine preparation and a preparation method thereof.

[0008] In order to achieve the above object, the present invention adopts the following technical solutions:

[0009] A high-stability povidone-iodine preparation comprises, calculated by mass percentage, 15.0%-25.0% of polyvinyl pyrrolidone K30, 10.0%-12.0% of refined iodine, 20.0%-30.0% of ethanol, 2.0%-4.0% of potassium iodide, 0.1%-1.0% of organic acid, 0.1%-2.0% of organic acid salt, 1.0%-3.0% of surfactant, 1.0%-5.0% of stabilizer, and the rest is water.

[0010] A method for preparing a high-stability povidone-iodine preparation comprises the following steps:

[0011] S1. Add water and organic acid to the first reaction tank, start stirring at a stirring speed of 10-20rpm, add polyvinyl pyrrolidone K30 while heating, disperse evenly and heat to 35-45°C;

[0012] S2. The surfactant and stabilizer are added to the first reaction tank, stirred for 20-30min, and after complete dispersion, the first reaction solution is obtained and allowed to stand for use;

[0013] S3. Add ethanol, refined iodine and potassium iodide to the second reaction tank, start stirring at a stirring speed of 10-20rpm until all the solids are completely dissolved, let stand, and filter to obtain a second reaction solution;

[0014] S4. The second reaction liquid is transferred to the first reaction tank, mixed with the first reaction liquid, stirred at a speed of 15-25rpm, stirred at 35-45°C for 20-30min, and cooled to 28-30°C with cooling water;

[0015] S5. Pre-dissolve the organic acid salt with an appropriate amount of water, then add it to the first reaction tank, adjust the pH to 4.5-5.5, stir for 10-20 minutes, filter out the material, and fill it with a filling mechanism to obtain a high-stability povidone-iodine preparation.

[0016] Preferably, the organic acid is selected from any one or more of acetic acid, oxalic acid, citric acid, lactic acid and ascorbic acid.

[0017] Preferably, the organic acid salt is selected from any one or more of sodium acetate, sodium oxalate, sodium citrate, sodium lactate and sodium ascorbate.

[0018] Preferably, the surfactant is selected from any one or more of Tween 20, Span 60, cocamidopropyl betaine, sodium dodecylbenzene sulfonate, sodium lauryl sulfate, and diisooctyl sodium sulfosuccinate.

[0019] Preferably, the stabilizer is selected from any one or more of glycerol, polyethylene glycol 400, butylene glycol and propylene glycol.

[0020] Preferably, the equipment used in the above preparation method includes a first reaction tank, a second reaction tank and a filling mechanism, the filling mechanism includes a filling detection unit, the filling detection unit includes a filling conveyor belt, a filling machine, a defective conveyor belt and a good conveyor belt, characterized in that: a plurality of medicine bottle clamps are evenly distributed on the filling conveyor belt, a plurality of mounting holes are provided on the medicine bottle clamp, a medicine bottle fixing seat is installed in the mounting hole, a mounting groove is provided on the top of the medicine bottle fixing seat, and a detection fill light is provided in the mounting groove;

[0021] A detection mechanism is provided at the bottom end of the filling conveyor belt, and the detection mechanism comprises a first cylinder, a horizontal driving box is fixed to the top end of the first cylinder, a bracket is connected to the output end of the horizontal driving box, and a photo detector is fixed on the bracket.

[0022] Preferably, a plurality of support frames are fixed in the installation holes, a lifting guide rod is vertically slidably installed on the support frame, the top end of the lifting guide rod is fixed to the medicine bottle fixing seat, and a return spring is provided on the outer side of the lifting guide rod.

[0023] Preferably, a horizontal push pin is movably installed on the medicine bottle clamp, one end of the horizontal push pin extends to the outside of the mounting hole, the other end of the horizontal push pin extends to the inside of the mounting hole and is fixed with a wedge block, and an inclined plate that slides with the wedge block is fixed on the medicine bottle fixing seat.

[0024] Preferably, a notch is provided at the top of the medicine bottle fixing seat, and a locking pressure plate is rotatably installed in the notch. There are multiple notches, and the multiple notches are distributed in a ring array.

[0025] Preferably, a vertically arranged spur rack is fixed on the inner wall of the mounting hole at a position corresponding to the locking pressure plate, and an arc-shaped rack is fixed on the locking pressure plate, and the spur rack is meshed with the arc-shaped rack.

[0026] Preferably, a rubber pad is fixed to the bottom end of the locking pressure plate, and raised particles are provided on the rubber pad.

[0027] Preferably, a horizontal slider is slidably installed inside the horizontal driving box, a lead screw is rotatably installed inside the horizontal driving box, the horizontal slider is threadedly installed on the outside of the lead screw, and the lead screw is driven by a rotating motor.

[0028] Preferably, a connecting rod is fixed on the horizontal slider, and the connecting rod extends to the outside of the horizontal drive box through the sliding opening and is fixed to the bracket. A second cylinder is also fixed on the bracket, and the output shaft of the second cylinder is fixed with a first push plate corresponding to the horizontal push pin, and the second cylinder and the photo detector have a spacing in the extension direction of the medicine bottle clamp, and the spacing is exactly equal to the spacing between the two mounting holes.

[0029] Preferably, the defective product conveyor belt is located close to the first cylinder, the good product conveyor belt is close to one end of the filling conveyor belt, a third cylinder is fixed to the bottom end of the filling conveyor belt close to the good product conveyor belt, a fourth cylinder is fixed to the output shaft of the third cylinder, a second push plate is fixed to the output shaft of the fourth cylinder, a fifth cylinder is also fixed to the defective product conveyor belt through a fixing frame, and a third push plate is fixed to the output shaft of the fifth cylinder.

[0030] Compared with the prior art, the present invention has the following beneficial effects:

[0031] 1. The povidone-iodine preparation obtained by the present invention has good stability, low reaction temperature during the reaction process, short total reaction time (only 4h-6h), high iodine yield (low degradation rate), and can improve production efficiency and reduce production energy consumption.

[0032] 2. The pH of the reaction solution is adjusted with an organic acid before the complex reaction, so that the degradation rate of iodine during the complex reaction is reduced and the conversion rate of complex iodine is improved: the usual conversion rate of effective iodine is about 85%, while the conversion rate of the present invention is about 95%.

[0033] 3. The addition of potassium iodide can help dissolve refined iodine, while improving the stability of iodine in povidone-iodine solution, preventing the recrystallization of iodine in the system, and also help drug absorption and improve the efficacy of sterilization and disinfection.

[0034] 4. The reaction process of povidone-iodine preparation is optimized. Refined iodine is easily soluble in ethanol, and the molecular chain of polyvinylpyrrolidone K30 polymer is in a state of free expansion in aqueous solution. Compared with the traditional complexing method, refined iodine is directly added to the polyvinylpyrrolidone K30 solution with higher consistency. The dissolution and diffusion of refined iodine are inhibited by the consistency of the solution. In order to obtain better uniformity, the reaction temperature (60-80°C) is increased and the reaction time (14-18 hours) is extended. However, this will significantly increase the degradation rate of iodine (iodine is greatly affected by temperature and is easy to sublimate), and the final iodine conversion rate is not high. The refined iodine of the present invention is pre-dissolved in ethanol in advance, which is a homogeneous reaction. The temperature required for the reaction is relatively low (35-45°C), and the reaction time is very short (0.5-1 hour), which saves time and energy consumption while improving the conversion rate of iodine.

[0035] 5. The povidone-iodine preparation obtained by the present invention is suitable for use in a variety of occasions. In the medical field, the povidone-iodine concentrated solution can be used for disinfection of human skin and mucous membranes, helping to prevent the occurrence of infection and ensuring the safety of surgery and medical operations. In the field of veterinary medicine, especially before and after milking of dairy cows, it can effectively kill bacteria, ensure the sanitary quality of dairy products, and also protect dairy cows from bacterial infection; for animal living places such as pens, its application can help eliminate pathogenic microorganisms, improve the sanitary level of the animal growth environment, and prevent the spread of diseases; its multifunctional application makes it a widely applicable disinfectant, providing strong support for health protection in multiple fields.

[0036] 6. The medicine bottles to be tested can be installed in groups of multiple medicine bottles in the medicine bottle testing fixture. Multiple groups of medicine bottles can be transported to the filling machine and the testing mechanism in sequence through the testing conveyor belt for filling and subsequent testing. Compared with the existing technology, the filling and testing efficiency is greatly improved.

[0037] 7. Due to the design of the medicine bottle detection fixture, when the medicine bottle mounting seat is not subjected to thrust, the locking pressure plate is in a horizontal state, so that the medicine bottle can be clamped in the mounting groove, and the thrust of the return spring can stably confine the medicine bottle in the mounting groove. Even if the mounting groove faces downward, the medicine bottle will not fall out. When the horizontal push pin is subjected to thrust, the return spring will be compressed, and the medicine bottle mounting seat will move upward. Due to the engagement of the straight rack and the arc rack, the locking pressure plate can be driven to flip upward and open. At this time, the staff can install the medicine bottle on the medicine bottle mounting seat. When the mounting groove faces downward, the medicine bottle will automatically fall, and the medicine bottle can be installed and poured out more efficiently.

[0038] 8. The detector can be driven horizontally by the horizontal drive box to move to each medicine bottle position in sequence. When the detector detects a medicine bottle and moves to the next medicine bottle position, the second cylinder can move to the position of the previous medicine bottle. If the medicine bottle fails the inspection, the second cylinder can push the horizontal push pin at that position. Since the installation groove is facing downward at this time, the medicine bottle that fails the inspection will automatically fall onto the defective product conveyor belt and be transported away.

[0039] 9. The first push plate has a smaller area and can only push one horizontal push pusher at a time, so that a defective product can be unlocked individually and dropped onto the defective product conveyor belt. The second and third push plates have larger areas and can push a whole row of horizontal push push pushers at a time, so that when loading medicine bottles, a row of locking pressure plates can be opened at one time, so that they can be installed without obstacles. After the inspection is completed, the remaining qualified products can be dropped onto the good product conveyor belt at one time for transportation, and the defective products can be automatically separated from the good products, further improving the efficiency of inspection. BRIEF DESCRIPTION OF THE DRAWINGS

[0040] Figure 1 The process of the present invention Figure 1 ;

[0041] Figure 2 The process of the present invention Figure 2 ;

[0042] Figure 3 This is a front view of the filling conveyor belt of the present invention;

[0043] Figure 4 This is a position distribution diagram of the medicine bottle clamp of the present invention on the filling conveyor belt;

[0044] Figure 5 It is a top view of the relative position of the filling conveyor belt, the defective product conveyor belt and the good product conveyor belt of the present invention;

[0045] Figure 6 This is an enlarged detail view of the medicine bottle clamp of the present invention from a top view;

[0046] Figure 7 for Figure 6 A zoomed-in detail of position A in the middle;

[0047] Figure 8 This is an enlarged detail view of the medicine bottle clamp of the present invention from an upward angle;

[0048] Fig. 9 This is an internal cross-sectional view of the installation hole of the present invention;

[0049] Fig.10 This is an enlarged detail view of the position of the medicine bottle fixing seat of the present invention;

[0050] Fig.11It is a schematic diagram of the relative positions of the arc-shaped rack and the spur rack when the locking pressure plate of the present invention is in a clamping state;

[0051] Fig.12 It is a schematic diagram of the relative positions of the arc-shaped rack and the spur rack when the locking pressure plate of the present invention is in the open state;

[0052] Fig.13 This is an enlarged detail view of the locking pressure plate position of the present invention;

[0053] Fig.14 This is a detailed view of the interior of the horizontal drive box of the present invention;

[0054] Fig.15 This is an enlarged detail view of the horizontal drive box of the present invention from the first viewing angle;

[0055] Fig.16 This is an enlarged detail view of the horizontal drive box of the present invention from a second viewing angle;

[0056] Fig.17 It is a schematic diagram of the structure of the medicine bottle of the present invention.

[0057] In the figure: 1 filling conveyor belt, 2 medicine bottle fixture, 201 installation hole, 202 power interface, 3 defective conveyor belt, 4 medicine bottle fixing seat, 401 installation groove, 4011 detection fill light, 4012 notch, 4013 locking pressure plate, 4014 arc rack, 4015 rubber pad, 402 lifting guide rod, 4021 return spring, 403 support frame, 404 straight rack, 405 horizontal push pin, 4051 wedge block, 406 inclined plate, 5 first cylinder, 501 horizontal drive box, 502 rotating motor, 503 screw rod, 504 horizontal slider, 505 connecting rod, 506 bracket, 507 second cylinder, 508 photo detector, 6 third cylinder, 601 fourth cylinder, 602 second push plate, 7 fixed frame, 701 fifth cylinder, 702 third push plate, 8 good product conveyor belt, 9 first reaction tank, 10 second reaction tank, 11 medicine bottle, 1101 annular protrusion, 12 filling mechanism. DETAILED DESCRIPTION

[0058] Unless otherwise specified, the raw materials and reagents used in the present invention are commercially available or can be prepared by known methods.

[0059] Example 1

[0060] A high-stability povidone-iodine preparation comprises, by weight percentage, 20.0% polyvinylpyrrolidone K30, 11.0% refined iodine, 25.0% ethanol, 3.0% potassium iodide, 0.25% citric acid, an appropriate amount of sodium citrate, 2.0% Tween 20, 3.0% polyethylene glycol 400, and the remainder water;

[0061] The preparation method of the high-stability povidone-iodine preparation comprises the following steps:

[0062] S1. Add water and citric acid to the first reaction tank, start stirring at a stirring speed of 15 rpm, add polyvinyl pyrrolidone K30 while heating, disperse evenly and heat to 40 ° C;

[0063] S2. Tween 20 and polyethylene glycol 400 were added to the first reaction tank and stirred for 25 min. After being completely dispersed, the first reaction solution was obtained and allowed to stand for use;

[0064] S3. Add ethanol, refined iodine and potassium iodide to the second reaction tank, start stirring at a stirring speed of 15 rpm until all the solids are completely dissolved, let stand, and filter to obtain a second reaction solution;

[0065] S4. The second reaction solution was transferred to the first reaction tank, stirred and mixed with the first reaction solution at a stirring speed of 20 rpm, stirred at 40 ° C for 25 min, and cooled to 29 ° C with cooling water;

[0066] S5. Pre-dissolve an appropriate amount of sodium citrate in water, then add it to the first reaction tank, adjust the pH to 5.0, stir for 15 minutes and filter the material, then fill it with a filling mechanism to obtain a highly stable povidone-iodine preparation.

[0067] Example 2

[0068] A high-stability povidone-iodine preparation, calculated by mass percentage, comprising: the same as in Example 1;

[0069] The difference between the preparation method and Example 1 is: S5. Pre-dissolve an appropriate amount of sodium citrate in water, then add it to the first reaction tank, and adjust the pH to 4.5; the rest is exactly the same as Example 1.

[0070] Example 3

[0071] A high-stability povidone-iodine preparation, calculated by mass percentage, comprising: the same as in Example 1;

[0072] The difference between the preparation method and Example 1 is as follows: S5. Pre-dissolve an appropriate amount of sodium citrate in water, then add it to the first reaction tank, and adjust the pH to 4.0;

[0073] The rest is exactly the same as in Example 1.

[0074] Example 4

[0075] A high-stability povidone-iodine preparation, calculated by mass percentage, comprising: the same as in Example 1;

[0076] The difference between the preparation method and Example 1 is as follows: S5. Pre-dissolve an appropriate amount of sodium citrate in water, then add it to the first reaction tank, and adjust the pH to 5.5;

[0077] The rest is exactly the same as in Example 1.

[0078] Example 5

[0079] A high-stability povidone-iodine preparation comprises, by weight percentage, 15.0% polyvinyl pyrrolidone K30, 10.0% refined iodine, 20.0% ethanol, 2.0% potassium iodide, 0.25% acetic acid, an appropriate amount of sodium acetate, 1.0% Span 60, 1.0% propylene glycol, and the remainder being water.

[0080] The preparation method of the high-stability povidone-iodine preparation comprises the following steps:

[0081] S1. Add water and acetic acid to the first reaction tank, start stirring at a stirring speed of 15 rpm, add polyvinyl pyrrolidone K30 while heating, disperse evenly and heat to 40 ° C;

[0082] S2. Span 60 and propylene glycol were added to the first reaction tank and stirred for 25 min. After complete dispersion, the first reaction solution was obtained and allowed to stand for use;

[0083] S3. Add ethanol, refined iodine and potassium iodide to the second reaction tank, start stirring at a stirring speed of 15 rpm until all the solids are completely dissolved, let stand, and filter to obtain a second reaction solution;

[0084] S4. The second reaction solution was transferred to the first reaction tank, stirred and mixed with the first reaction solution at a stirring speed of 20 rpm, stirred at 40 ° C for 25 min, and cooled to 29 ° C with cooling water;

[0085] S5. Pre-dissolve an appropriate amount of sodium acetate in water, then add it into the first reaction tank, adjust the pH to 5.0, stir for 15 minutes, filter out the material, and fill it with a filling mechanism to obtain a high-stability povidone-iodine preparation.

[0086] Example 6

[0087] A high-stability povidone-iodine preparation comprises, by weight percentage, 25.0% polyvinyl pyrrolidone K30, 12.0% refined iodine, 30.0% ethanol, 4.0% potassium iodide, 0.25% lactic acid, an appropriate amount of sodium lactate, 3.0% sodium lauryl sulfate, 5.0% glycerol, and the remainder is water.

[0088] The preparation method of the high-stability povidone-iodine preparation comprises the following steps:

[0089] S1. Add water and lactic acid to the first reaction tank, start stirring at a stirring speed of 15 rpm, add polyvinyl pyrrolidone K30 while heating, disperse evenly and heat to 40 ° C;

[0090] S2. Sodium lauryl sulfate and glycerol were added to the first reaction tank and stirred for 25 min. After complete dispersion, the first reaction solution was obtained and allowed to stand for use;

[0091] S3. Add ethanol, refined iodine and potassium iodide to the second reaction tank, start stirring at a stirring speed of 15 rpm until all the solids are completely dissolved, let stand, and filter to obtain a second reaction solution;

[0092] S4. The second reaction solution was transferred to the first reaction tank, stirred and mixed with the first reaction solution at a stirring speed of 20 rpm, stirred at 40 ° C for 25 min, and cooled to 29 ° C with cooling water;

[0093] S5. Pre-dissolve an appropriate amount of sodium lactate in water, then add it into the first reaction tank, adjust the pH to 5.0, stir for 15 minutes, filter out the material, and fill it with a filling mechanism to obtain a high-stability povidone-iodine preparation.

[0094] The initial effective iodine content in the povidone-iodine preparations of Examples 1-6 was detected. According to the accelerated test method (disinfection technical specifications, 54° C., 14D), the effective iodine content after the experiment was detected. The results are shown in Table 1.

[0095] Table 1

[0096]

[0097] As can be seen from the table, the available iodine data in the povidone-iodine concentrated preparations all showed a downward trend, but the samples prepared with an initial pH of around 5.0 had a higher stability, which was significantly higher than other samples.

[0098] Example 7

[0099] A high-stability povidone-iodine preparation, calculated by mass percentage, comprises: the difference from Example 1 is: 0% citric acid; the rest is exactly the same as Example 1;

[0100] The difference between the preparation method and Example 1 is that an appropriate amount of citric acid (sodium) is pre-dissolved in water and then added to the first reaction tank, and the pH is adjusted to 5.0. The rest is exactly the same as Example 1.

[0101] Example 8

[0102] A high-stability povidone-iodine preparation, calculated by mass percentage, comprises: the difference from Example 1 is: 0.5% citric acid; the rest is exactly the same as Example 1;

[0103] The preparation method is exactly the same as that in Example 1.

[0104] Example 9

[0105] A high-stability povidone-iodine preparation, calculated by mass percentage, comprises: the difference from Example 1 is: 0.8% citric acid; the rest is exactly the same as Example 1;

[0106] The preparation method is exactly the same as that in Example 1.

[0107] The initial effective iodine content in the povidone-iodine preparations of Examples 1, 7, 8, and 9 was detected. The effective iodine content after the experiment was detected according to the accelerated test method (disinfection technical specifications, 54° C., 14D). The results are shown in Table 2.

[0108] Table 2

[0109]

[0110] Organic acids dissolve in water and can ionize H + , which increases the acidity of the solution, thereby inhibiting the hydrolysis of iodine molecules to generate iodine anions (the degradation of iodine molecules into iodine anions will increase the acidity of the solution), inhibiting the degradation of iodine in the solution, thereby increasing the content of effective iodine and reducing the loss rate of effective iodine; however, when H + When a certain concentration is reached, it will affect the combination of iodine and PVP to form PVP-I. Organic acids and their salts can make iodine ions react with iodine molecules to form I 3- Then it combines with PVP to form PVP-I. As the concentration of organic acid increases, H + The increase in solubility inhibits the concentration of iodine anions and reduces the forward reaction. At the same time, too much organic acid is added, and more organic acid salts are needed to adjust the pH in the last step of pH adjustment, which will significantly increase the ionic strength in the solution and affect the solubility of PVP, etc. The applicant unexpectedly found that the addition of citric acid at 0.25% and the pH adjustment of 5 are more suitable.

[0111] Example 10

[0112] Reference Figure 1-17A method for preparing a high-stability povidone-iodine preparation, wherein the equipment used in the above-mentioned preparation method includes a first reaction tank 9, a second reaction tank 10 and a filling mechanism 12, wherein the filling mechanism 12 includes a filling detection unit, wherein the filling detection unit includes a filling conveyor belt 1, a filling machine, a defective conveyor belt 3 and a good conveyor belt 8, wherein a plurality of medicine bottle clamps 2 are evenly distributed on the filling conveyor belt 1, wherein a plurality of mounting holes 201 are provided on the medicine bottle clamp 2, wherein a medicine bottle fixing seat 4 is installed in the mounting hole 201, wherein a mounting groove 401 is provided at the top of the medicine bottle fixing seat 4, wherein a detection fill light 4011 is provided in the mounting groove 401;

[0113] After preparation and filtration, the medicine is transported to the filling machine to wait for filling. The empty medicine bottle is transported to the filling machine position through the filling conveyor belt 1, and then the medicine is filled into the filling machine and then sealed with a bottle stopper.

[0114] A detection mechanism is provided at the bottom end of the filling conveyor belt 1, and the detection mechanism includes a first cylinder 5, a horizontal driving box 501 is fixed to the top of the first cylinder 5, and the output end of the horizontal driving box 501 is connected to a bracket 506, and a photo detector 508 is fixed on the bracket 506. The detection mechanism takes a photo of the medicine bottle after filling through the photo detector 508, and then compares it through a computer to detect whether there are cracks on the mouth and body of the medicine bottle, and detect whether the bottle plug of the medicine bottle is pressed in place. When the medicine bottle clamp 2 moves to the position of the detection mechanism, the power plug can be inserted into the power interface 202 through the push rod motor to power the detection fill light 4011, thereby increasing the brightness during the detection process and improving the detection success rate.

[0115] Embodiment 11

[0116] Reference Figure 1-17 The difference between this embodiment and embodiment 10 is that a plurality of support frames 403 are fixed in the mounting hole 201, and a lifting guide rod 402 is vertically slidably mounted on the support frame 403. The top of the lifting guide rod 402 is fixed to the medicine bottle fixing seat 4, and a return spring 4021 is sleeved on the outer side of the lifting guide rod 402. When the medicine bottle fixing seat 4 is subjected to an upward thrust, the return spring 4021 will be compressed. When the thrust applied to the medicine bottle fixing seat 4 is released, the return spring 4021 will push the medicine bottle fixing seat 4 to return to its original position.

[0117] Among them, a horizontal push pin 405 is movably installed on the medicine bottle clamp 2, one end of the horizontal push pin 405 extends to the outside of the mounting hole 201, the other end of the horizontal push pin 405 extends to the inside of the mounting hole 201 and is fixed with a wedge block 4051, and an inclined plate 406 that slides with the wedge block 4051 is fixed on the medicine bottle fixing seat 4. When the horizontal push pin 405 is subjected to a horizontal thrust, the cooperation between the wedge block 4051 and the inclined plate 406 can push the medicine bottle fixing seat 4 to move upward, and when the thrust applied to the horizontal push pin 405 is cancelled, the reset spring 4021 will push the medicine bottle fixing seat 4 to reset.

[0118] Among them, a notch 4012 is opened at the top of the medicine bottle fixing seat 4, and a locking pressure plate 4013 is rotatably installed in the notch 4012. There are multiple notches 4012, and the multiple notches 4012 are distributed in a ring array. A vertically arranged spur rack 404 is fixed at a position corresponding to the locking pressure plate 4013 on the inner wall of the installation hole 201, and an arc-shaped rack 4014 is fixed on the locking pressure plate 4013, and the spur rack 404 is meshed with the arc-shaped rack 4014;

[0119] The bottom end of the medicine bottle 11 is provided with an annular protrusion 1101. When the medicine bottle fixing seat 4 is not subjected to thrust, the locking pressure plate 4013 is in a horizontal state, so that the medicine bottle 11 can be clamped in the installation groove 401. The locking pressure plate 4013 clamps the medicine bottle 11 from all sides. The locking pressure plate 4013 is just stuck on the top of the annular protrusion 1101. The thrust of the return spring 4021 can stably confine the medicine bottle 11 in the installation groove 401. When the mounting groove 401 faces downward, the medicine bottle 11 will not fall out. When the horizontal push pin 405 is pushed, the return spring 4021 will be compressed and the medicine bottle holder 4 will move upward. Since the straight rack 404 is meshed with the arc rack 4014, the locking pressure plate 4013 can be driven to flip upward and open. At this time, the staff can put an empty medicine bottle 11 into the medicine bottle holder 4. When the mounting groove 401 faces downward, the medicine bottle 11 will automatically fall out.

[0120] Among them, a rubber pad 4015 is fixed to the bottom end of the locking pressure plate 4013, and the rubber pad 4015 is provided with raised particles. The rubber pad 4015 can increase the friction and buffer, so that the medicine bottle 11 is clamped more stably.

[0121] Example 12

[0122] Reference Figure 1-17 The difference between this embodiment and embodiment 10 is that a horizontal slider 504 is slidably installed inside the horizontal driving box 501, a screw rod 503 is rotatably installed inside the horizontal driving box 501, the horizontal slider 504 is threadedly installed on the outside of the screw rod 503, and the screw rod 503 is driven by a rotating motor 502;

[0123] When the screw rod 503 is driven to rotate by the rotary motor 502 , the horizontal slider 504 can be driven to move horizontally.

[0124] Among them, a connecting rod 505 is fixed on the horizontal slider 504, and the connecting rod 505 extends to the outside of the horizontal driving box 501 through the sliding opening and is fixed to the bracket 506. The bracket 506 is also fixed with a second cylinder 507, and the output shaft of the second cylinder 507 is fixed with a first push plate corresponding to the horizontal push pin 405, and the second cylinder 507 and the photo detector 508 have a spacing in the extension direction of the medicine bottle clamp 2, and the spacing is exactly equal to the spacing between the two mounting holes 201;

[0125] The horizontal driving box 501 drives the photo detector 508 to move horizontally and move to the positions of each medicine bottle 11 in sequence. When the photo detector 508 detects one medicine bottle 11 and moves to the position of the next medicine bottle 11, the second cylinder 507 can just move to the position of the previous medicine bottle 11. If the medicine bottle 11 fails the inspection, the second cylinder 507 can push the horizontal push pin 405 at that position. Since the installation groove 401 is facing downward at this time, the medicine bottle 11 that fails the inspection will automatically fall onto the defective product conveyor belt 3 and be transported away.

[0126] The defective conveyor belt 3 is located near the first cylinder 5, the good conveyor belt 8 is close to one end of the filling conveyor belt 1, and the bottom end of the filling conveyor belt 1 is fixed with a third cylinder 6 near the good conveyor belt 8, the output shaft of the third cylinder 6 is fixed with a fourth cylinder 601, and the output shaft of the fourth cylinder 601 is fixed with a second push plate 602;

[0127] The first push plate has a smaller area and can only push one horizontal push pin 405 at a time, so that a defective product can be unlocked and dropped onto the defective product conveyor belt 3. The second push plate 602 and the third push plate 702 have larger areas and can push the entire row of horizontal push pins 405 at a time, so that when loading the medicine bottles 11, a row of locking plates 4013 can be opened at one time, so that the installation can be unobstructed, and the remaining qualified products can be dropped onto the qualified product conveyor belt 8 at one time after the inspection is completed and transported away;

[0128] A fifth cylinder 701 is also fixed on the defective product conveyor belt 3 via a fixing frame 7, and a third push plate 702 is fixed on the output shaft of the fifth cylinder 701;

[0129] The first cylinder 5 and the third cylinder 6 can drive the horizontal driving box 501 and the fourth cylinder 601 to move vertically, so that when the filling conveyor belt 1 is running, the horizontal driving box 501 and the fourth cylinder 601 can move downward without blocking the medicine bottle clamp 2.

[0130] Working principle:

[0131] The first step is to control the fifth cylinder 701 to extend, drive the third push plate 702 to push the horizontal push pin 405 on the medicine bottle clamp 2 on the leftmost side of the top of the filling conveyor belt 1, and the horizontal push pin 405 can push the wedge block 4051 to move horizontally, thereby pushing the medicine bottle fixing seat 4 to move upward. During the upward movement of the medicine bottle fixing seat 4, the straight rack 404 is engaged with the arc rack 4014, thereby driving the locking pressure plate 4013 to flip upward and open. At this time, the staff puts the medicine bottle 11 into the installation groove 401. When the fifth cylinder 701 is shortened, the reset spring 4021 will automatically push the medicine bottle fixing seat 4 to move downward and reset, thereby driving the locking pressure plate 4013 to rotate and reset, and press the medicine bottle 11 from the top of the annular protrusion 1101 of the medicine bottle 11, so that the medicine bottle 11 will not fall off;

[0132] In the second step, after installing a row of medicine bottles 11, the medicine bottles 11 are transported to the filling machine position through the filling conveyor belt 1, and the medicine is poured into the medicine bottles 11 by the filling machine, and then the sealing type is inserted into the bottle mouth, and then it is further transported to the detection mechanism position. At this time, the installation groove 401 is downward, because of the existence of the locking pressure plate 4013, the medicine bottle 11 will not fall. Only when the horizontal push pusher 405 is pushed, the locking pressure plate 4013 will be opened, and the medicine bottle 11 will automatically fall.

[0133] In the third step, the horizontal driving box 501 drives the photo detector 508 to move horizontally to the positions of the medicine bottles 11 in sequence, and detects the medicine bottles 11. If an unqualified medicine bottle 11 is detected, the second cylinder 507 pushes the horizontal push pin 405 at the corresponding position, and the unqualified medicine bottle 11 will automatically fall to the defective conveyor belt 3, and the qualified medicine bottle 11 will continue to be conveyed to the top of the good conveyor belt 8, and then the fourth cylinder 601 pushes all the horizontal push pins 405, and the remaining qualified medicine bottles 11 will automatically fall to the top of the good conveyor belt 8;

[0134] In the fourth step, the empty medicine bottle fixture 2 finally moves to the initial position following the filling conveyor belt 1, and the empty medicine bottle 11 can be placed therein.

[0135] The control method of the present invention is automatic control through a controller. The control circuit of the controller can be implemented by simple programming by technicians in this field. The provision of power is also common knowledge in this field. The present invention is mainly used to protect mechanical devices, so the present invention will no longer explain the control method and circuit connection in detail.

[0136] The above description is only a preferred specific implementation manner of the present invention, but the protection scope of the present invention is not limited thereto. Any technician familiar with the technical field can make equivalent replacements or changes according to the technical scheme and inventive concept of the present invention within the technical scope disclosed by the present invention, which should be covered by the protection scope of the present invention.

Claims

1. A method for preparing a high-stability povidone-iodine preparation, the povidone-iodine preparation comprising, calculated by mass percentage, the following: Polyvinylpyrrolidone K30 15.0%-25.0%, refined iodine 10.0%-12.0%, ethanol 20.0%-30.0%, potassium iodide 2.0-4.0%, organic acid 0.1-1.0%, organic acid salt 0.1-2.0%, surfactant 1.0%-3.0%, stabilizer 1.0%-5.0%, and the rest is water, characterized in that it comprises the following steps: S1. Add water and organic acid to the first reaction tank, start stirring at a stirring speed of 10-20rpm, add polyvinyl pyrrolidone K30 while heating, disperse evenly and heat to 35-45°C; S2. The surfactant and stabilizer are added to the first reaction tank, stirred for 20-30min, and after complete dispersion, the first reaction solution is obtained and allowed to stand for use; S3. Add ethanol, refined iodine and potassium iodide to the second reaction tank, start stirring at a stirring speed of 10-20rpm until all the solids are completely dissolved, let stand, and filter to obtain a second reaction solution; S4. The second reaction liquid is transferred to the first reaction tank, mixed with the first reaction liquid, stirred at a speed of 15-25rpm, stirred at 35-45°C for 20-30min, and cooled to 28-30°C with cooling water; S5. The organic acid salt is pre-dissolved with an appropriate amount of water, and then added to the first reaction tank, the pH is adjusted to 4.5-5.5, and the material is filtered after stirring for 10-20min, and the filling mechanism is filled to obtain a highly stable povidone iodine preparation; The filling mechanism comprises a filling detection unit, the filling detection unit comprises a filling conveyor belt (1), a filling machine, a defective product conveyor belt (3) and a good product conveyor belt (8), a plurality of medicine bottle clamps (2) are evenly distributed on the filling conveyor belt (1), a plurality of mounting holes (201) are provided on the medicine bottle clamps (2), a medicine bottle fixing seat (4) is installed in the mounting holes (201), a mounting groove (401) is provided at the top of the medicine bottle fixing seat (4), and a detection fill light (4011) is provided in the mounting groove (401); A detection mechanism is provided at the bottom end of the filling conveyor belt (1), the detection mechanism comprising a first cylinder (5), a horizontal drive box (501) being fixed to the top end of the first cylinder (5), a bracket (506) being connected to the output end of the horizontal drive box (501), and a photo detector (508) being fixed to the bracket (506).

2. The method for preparing a high-stability povidone-iodine preparation according to claim 1, characterized in that: A plurality of support frames (403) are fixed in the installation holes (201), and a lifting guide rod (402) is vertically slidably installed on the support frame (403). The top of the lifting guide rod (402) is fixed to the medicine bottle fixing seat (4), and a return spring (4021) is sleeved on the outer side of the lifting guide rod (402); A horizontal push pin (405) is movably mounted on the medicine bottle clamp (2), one end of the horizontal push pin (405) extends to the outside of the mounting hole (201), the other end of the horizontal push pin (405) extends to the inside of the mounting hole (201) and is fixed with a wedge block (4051), and an inclined plate (406) that slidably cooperates with the wedge block (4051) is fixed on the medicine bottle fixing seat (4).

3. The method for preparing a high-stability povidone-iodine preparation according to claim 1, characterized in that: The organic acid is selected from any one or more of acetic acid, oxalic acid, citric acid, lactic acid and ascorbic acid.

4. The method for preparing a high-stability povidone-iodine preparation according to claim 1, characterized in that: The organic acid salt is selected from any one or more of sodium acetate, sodium oxalate, sodium citrate, sodium lactate and sodium ascorbate.

5. The method for preparing a high-stability povidone-iodine preparation according to claim 1, characterized in that: The surfactant is selected from any one or more of Tween 20, Span 60, cocamidopropyl betaine, sodium dodecylbenzene sulfonate, sodium lauryl sulfate, and sodium diisooctyl sulfosuccinate.

6. The method for preparing a high-stability povidone-iodine preparation according to claim 1, characterized in that: The stabilizer is selected from any one or more of glycerol, polyethylene glycol 400, butylene glycol, and propylene glycol.

7. The method for preparing a high-stability povidone-iodine preparation according to claim 1, characterized in that: A notch (4012) is provided at the top of the medicine bottle fixing seat (4), and a locking pressure plate (4013) is rotatably mounted in the notch (4012). There are a plurality of notches (4012), and the plurality of notches (4012) are distributed in a ring array.

Citation Information

Patent Citations

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