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Method for preparing high-water-solubility cydiodine with low cost

A cedidin and water-soluble technology, applied in the field of low-cost preparation of high water-soluble cedidin, can solve the problems of decreased coating rate, unreachable higher concentration, high product cost, improved iodine recovery rate, The effect of reducing the loss of iodine and reducing the product cost

Inactive Publication Date: 2013-11-20
何元龙
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] 1. The coating rate is low, iodine crystallizes in the coating, and part of the iodine is wasted
[0005] Because high-concentration iodine solution is used during coating, and the temperature of iodine solution and cyclodextrin temperature are not strictly controlled, if the temperature of iodine solution is higher than the temperature of cyclodextrin solution, iodine will crystallize due to the drop in temperature during coating. Crystallization is difficult to be coated, so sublimation occurs when cedi iodine is dried, resulting in a waste of iodine
In addition, if a saturated solution is used for cyclodextrin, when iodine solution is added to the cyclodextrin solution, because the solubility of cyclodextrin in ethanol solution is much lower than that in water, cyclodextrin is also easy to precipitate and crystallize, resulting in a decrease in the coating rate
[0006] 2. Part of β-cyclodextrin is destroyed by iodine
[0007] Since the coating process uses saturated β-cyclodextrin solution and high-concentration iodine solution, and usually reacts at high temperature, high-concentration iodine is easy to destroy the molecular structure of β-cyclodextrin, making the cyclodextrin after coating Yield reduction
[0008] 3. Iodine loss caused by coating drying and dehydration process
[0009] About 1% to 3% of iodine will sublime when the coated cediodine is dried above room temperature and below 60°C, resulting in iodine loss.
[0010] 4. The high temperature treatment process of the coating results in the loss of iodine
[0012] 5. Part of the coating after high temperature treatment is unstable and the product quality is poor
[0013] After high temperature treatment, the water solubility of the product increases, but the stability of the product decreases. After 180 days at room temperature, the iodine content in the product decreases by about 2% to 5% before it can maintain long-term stability. Difference
[0014] 6. Water solubility is still low
[0015] The solubility of the highly water-soluble cedi iodine produced by the above patent is: Dissolve 0.1g in 100ml of water at 20°C (i.e. the iodine concentration after dissolution is about 160mg / L), and the higher concentration cannot reach
[0016] 7. High product cost
[0017] The above problems directly lead to a low total yield of the highly water-soluble product finally prepared by the above patent, about 85% to 90%, the recovery rate of iodine is 90%, and the yield of available iodine after 180 days is about 80%, resulting in the waste of part of the iodine , the water solubility of the product is not high, and the production cost of the product is relatively high

Method used

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Examples

Experimental program
Comparison scheme
Effect test

example 1

[0037] Weigh 150g of β-cyclodextrin, add it into a glass reactor with 1000ml of water, stir and heat to 78°C and dissolve completely, then keep the temperature for later use. Weigh 33.5g of iodine and 5g of potassium iodide, add them to 260ml of 90% ethanol solution, and heat to 75°C to dissolve them all. Then, under stirring, the iodine solution was slowly added to the β-cyclodextrin solution, and the reaction kettle was naturally cooled to room temperature under constant stirring. The reaction solution is separated by a continuous high-speed centrifuge with a rotation speed of 5000rps to separate the cedi iodine, and then the precipitate is placed in an enamel plate and dried naturally at room temperature until it is powdered. Put the cedi iodine powder in a vacuum desiccator, connect the desiccator’s exhaust port to the bottom of the vacuum bottle, and put the cyclodextrin or povidone iodine solution in the bottle to recover the iodine vapor, vacuumize and raise the tempera...

example 2

[0039] Weigh 100kg of β-cyclodextrin, add it into an enamel reaction kettle with 1200kg of water, stir and heat to 70°C and dissolve completely, then keep the temperature for later use. Weigh 22.4kg of iodine and 4kg of potassium iodide, add them to 300L of 95% ethanol solution, and heat to 70°C to dissolve them all. Slowly add the iodine solution to the β-cyclodextrin solution under stirring, and let the reaction kettle cool down to room temperature naturally under constant stirring. Then pour the reaction solution into a stainless steel liquid storage tank and store it at room temperature for 24 hours to allow the cedi iodine to precipitate naturally, then remove the supernatant; put the precipitate into a suitable container and dry it naturally to powder at room temperature. Put the Sidi iodine powder into the rake-type vacuum dryer, connect the air suction port to the iodine vapor recovery device, evacuate and heat to 130°C and maintain for 40 minutes.

example 3

[0041]Weigh 360g of β-cyclodextrin, add it into a glass reactor with 2500ml of water, stir and heat to 80°C and dissolve completely, then keep the temperature for later use. Weigh 80.5g of iodine and 10g of potassium iodide, add them to 600ml of 85% ethanol solution, and heat to 80°C to dissolve them all. Slowly add the iodine solution to the saturated β-cyclodextrin solution under stirring, and let the reaction kettle cool down to room temperature naturally under continuous stirring; the reaction liquid is naturally precipitated and then the supernatant is removed. The precipitate was vacuum-dried to powder at low temperature in a freeze-vacuum dryer. Put the cedi iodine powder in a vacuum desiccator, connect the air outlet of the desiccator to the iodine vapor recovery device, evacuate and raise the temperature to 120°C and maintain it for 60 minutes to obtain highly water-soluble cedi iodine.

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PUM

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Abstract

The invention discloses a method for preparing high-water-solubility cydiodine with a low cost. The method comprises the following steps of: preparing beta-cyclodextrin into an unsaturated solution; dissolving iodine and potassium iodide into an ethanol solution to obtain an iodine solution, wherein the temperature of the iodine solution is not higher than the temperature of the beta-cyclodextrin solution, and the volume of the ethanol solution is not greater than the 30% of the volume of the beta-cyclodextrin solution; slowly adding the iodine solution into the beta-cyclodextrin solution under stirring condition, and naturally cooling to the room temperature under continuous stirring condition; carrying out natural precipitation or centrifugation on the cooled peridium suspension so as to obtain a coating; drying the peridium to be powder at the room temperature or under a low-temperature condition; then putting the cydiodine into a vacuum dry container, and vacuuming, drying and uniformly mixing at 100-200 DEG C so as to obtain the high-water-solubility cydiodine; and at the same time recycling iodine steam. The effective iodine content of the cydiodine prepared by using the method is greater than 16%, the solubility of the cydiodine in 100ml of water at 20 DEG C is greater than 0.2g, the product yield is greater than 95%, and the iodine recycling rate is greater than 99%.

Description

technical field [0001] The invention relates to a low-cost preparation method of highly water-soluble cedi iodine, which belongs to the technical field of pharmacy. Background technique [0002] As a low-cost coating preparation of iodine, cediiodine has the characteristics of high iodine content, good stability and low cost, and has been developed in clinical medicine for more than 20 years. At the same time, iodine disinfectant is one of the species with the greatest consumption and unique disinfection effect. It is the dream of many scientific researchers whether to develop low-cost cedi iodine into disinfectant products. However, cediodine itself is a poorly water-soluble substance, so the product has not been successfully developed into a disinfectant for many years. [0003] There are many patents about cediodine at home and abroad, but the prepared cediodine is all non-water-soluble products. Only the invention patent "Preparation Method of Highly Water-Soluble Cedi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): A61K33/18A61K47/40A61P31/04A61P31/10A61P31/12
Inventor 何元龙
Owner 何元龙
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