CN103766399B - A kind of iodine-containing disinfectant and preparation method thereof - Google Patents

A kind of iodine-containing disinfectant and preparation method thereof Download PDF

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CN103766399B
CN103766399B CN201210406246.XA CN201210406246A CN103766399B CN 103766399 B CN103766399 B CN 103766399B CN 201210406246 A CN201210406246 A CN 201210406246A CN 103766399 B CN103766399 B CN 103766399B
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disinfectant
quaternary ammonium
ammonium salt
iodine
double
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CN103766399A (en
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张许科
刘兴金
张晓会
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Luoyang Huizhong Animal Medicine Co Ltd
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Abstract

One iodine-containing disinfectant of the present invention and preparation method thereof, described iodine-containing disinfectant includes strand quaternary ammonium salt and/or double-chain quaternary ammonium salt, iodine, nonionic surfactant, acid and pharmaceutically acceptable carrier.Disinfectant prepared by the present invention is compared with existing iodine-containing disinfectant, and bactericidal action strengthens, and xanthochromia is low.Present invention also offers the preparation method of the composite disinfectant of a kind of quaternary ammonium salt and iodine, and the application in poultry house and environment disinfected.

Description

A kind of iodine-containing disinfectant and preparation method thereof
Technical field
The present invention relates to disinfectant field, be specifically related to a kind of iodine-containing disinfectant.
Background technology
Along with the development of modern intensive aquaculture, intensive cultivating condition makes poultry be caused The threat of sick microorganism is increasingly severe, although putting into substantial amounts of funds on vaccine and medicine, But still cannot avoid the disease harm to animal body, these diseases also threaten while existing The health of the mankind.Basic factor is exactly pathogenic microorganism, especially containing big in feces of livestock and poultry The mosquitos and flies that the pathogenic microorganism of amount, parasitic ovum and evil are raw, these all can make cause of disease in environment Kind increases, amount of bacteria increases, and causes spreading of people, animal infectious disease, especially infecting both domestic animals and human Disease, to the harm of bringing on a disaster property of people and animals.
Quaternary ammonium disinfectant was synthesized by American scholar one first as far back as 1915, was a class sun Ionic surface active agent, positively charged in water, it is possible to be adsorbed in forcefully various fungus, Antibacterial, virus surface, change fungus, antibacterial, the permeability of the thin spore of virion, in making thalline Lonely coenzyme and the effusion of Metabolic Intermediate product, hinder the breathing of mushroom and glycolytic cycle, and Make tropina degeneration, thus reach bactericidal action.
Quaternary ammonium disinfectant includes strand quaternary ammonium salt and double-chain quaternary ammonium salt two class.But quaternary ammonium salt Class disinfectant can not kill fungus, tubercule bacillus, hydrophilic viruses and bacterial spore, belongs to poor efficiency Disinfectant.But quaternary ammonium disinfectant Disinfection Effect when being used alone is bad, is usually vulnerable to The impact of the factors such as the kind of microorganism, pH value, temperature, concentration and Organic substance.And individually When using quaternary cationic surfactant, it is easy to produce owing to it belongs to low effect disinfectants Raw Resistant strain.
Iodine has the strongest sterilizing power and sterilization speed quickly under sour environment, and Operand becomes Disinfectant for a kind of function admirable.But the shortcoming of Operand is also apparent , as the least in the dissolubility in water, it is impossible to be configured to water formulation and use;Preparation is unstable, Iodine easily distils inefficacy;Iodine is stronger to the zest of skin;There is xanthochromia etc..
Iodine has the history of 150 years for body sterilization, but due to iodine dissolubility in water The least;The most easily distilling, content is unstable;To the mucocutaneous shortcoming such as irritant And limit its extensive application.At present, widely used povidone iodine class disinfectant is to have mostly Machine polymer or surfactant are carrier, by between carrier molecule formed network structure or Micelle, " fetters iodine " in wherein with the conformational effect in electronics and space, thus changes iodine one As free state in Operand so that it is stability and bactericidal action enhancing, zest and xanthochromia Property reduce.But this kind of product with surfactant as carrier is original micelle power after dilution Can be destroyed, make the stability of active iodine decline, thus affect its sterilization effect.But The general molecular weight of organic polymer relatively big (up to 70000-100000) is difficult to be biodegradable, Life-time service can be to environment.
In order to overcome the defect of single component, improve Disinfection Effect, make disinfectant wide spectrum, efficiently, Stable, easy to use, safe, anti-interference, moderate cost, compound recipe iodine-containing disinfectant has become Focus for current research.
Chinese patent CN1883273 provides a kind of preparation method containing iodine compound disinfectant, uses In the pathogenic microorganism and aquaculture of poultry susceptible virus, antibacterial and environment virus, The sterilization of antibacterial.It is equipped with other activity mainly with iodine and benzalkonium bromide as main active The factor forms, and its component and content is: benzalkonium bromide 5%-45%, Radix Sophorae Flavescentis extractive liquid 1%-2%, Ethanol 5%-10%, potassium iodide 0.1% one 1%, iodine 0.5%-3%, phosphatase 11 %-3%, water is complete Amount.Its shortcoming is: 1) prepare the antagonist that the potassium iodide added in prescription is benzalkonium bromide.2) Prescription adds Chinese medicine extract Radix Sophorae Flavescentis extractive liquid 1%-2%, uses after dilution and make without sterilization With.
Chinese patent CN 1238909A provides the preparation of a kind of quaternary ammonium salt chelated iodine disinfectant Method,
The method obtaining this complex disinfectant is: the compound that logical formula (I) is represented with Iodine is mixed together after stirring and react 1-2 hour and obtains product.This disinfectant has season by salt The double sterilization effect of compound and Operand, it is adaptable to culture fishery and livestock and poultry breeding industry Sterilizing.Its shortcoming is: 1) do not have ready-made raw material in preparation process, needs first to synthesize Intermediate leads to formula (I), then the synthesis of the agent raw material that carries out disinfection, and reactions steps is more, difficult quality Control.2) in preparation process, temperature is 70-80 DEG C of reaction 1h, and iodine easily distils.
Therefore, in the urgent need to a kind of wide spectrum, efficient, stable, use in livestock and poultry cultivation place Convenient, safe, anti-interference, the disinfectant of moderate cost.
Summary of the invention
It is an object of the invention to provide a kind of wide spectrum, efficient, stable iodine-containing disinfectant.? Quaternary ammonium salt iodine disinfectant technology of preparing adds potassium iodide and makes preparation stabilization, but add iodate Potassium has antagonism to the virus killing effect of quaternary ammonium salt, the preparation of quaternary ammonium salt iodine disinfectant in the present invention In eliminate potassium iodide, be simultaneously introduced nonionic surfactant and make preparation stabilization.Purport of the present invention Overcoming technology prejudice, it is provided that one has synergistic quaternary ammonium salt iodine disinfectant, the present invention The disinfectant of preparation is compared with existing iodine-containing disinfectant, and bactericidal action strengthens, and xanthochromia is low.
The invention provides a kind of iodine-containing disinfectant, additionally, present invention also offers described in one The preparation method of iodine-containing disinfectant, and the application in poultry house and environment disinfected.
The invention provides a kind of iodine-containing disinfectant, based on 100 mass parts, comprise following components:
Surplus is pharmaceutically acceptable carrier.
At least one in following compound of described strand quaternary ammonium salt: alkyl dimethyl benzyl ammonium Chloride (benzalkonium chloride), or for fragrance ring hydrogen is substituted by chlorine, methyl or ethyl And the replacement zephiran formed;It is preferably alkyl dimethyl benzyl ammonium chloride.
At least one in following compound of described double-chain quaternary ammonium salt: double octyl group quaternary ammonium salts, Double decyl quaternary ammonium salts, double dodecyl quaternary ammonium salt or octyl-decyl quaternary ammonium salt.
Preferably, at least one in following compound of described double-chain quaternary ammonium salt: double decyls Ditallowdimethyl ammonium bromide, double-track suspended self-propelled conveyor, dimethyl benzyl ammonium chloride, bromination double (ten Dialkyl dimethyl) ethylene diammonium, 2-(2-phenoxy group) ethyl-trimethyl salmiac, benzene Prick bromine ammonium or Benzalkonii Chloridum.
At least one in following compound of nonionic surfactant of the present invention: Fatty alcohol-polyoxyethylene ether (AEO), Polyethylene Glycol (PEG), alkylphenol polyoxyethylene (NP Or OP), poloxamer, lauric acid polyoxyethylene ester or castor oil polyoxyethylene ether.
At least one in hydrochloric acid, sulphuric acid or phosphoric acid of acid of the present invention.
Pharmaceutically acceptable carrier of the present invention is alcoholic solution, and preferred volume mark is The alcoholic solution of 50%.
At least one in following compound of described alcohol: glycerol, propylene glycol, ethanol Or ethylene glycol.
Of the present invention containing iodine composite disinfectant, its preparation method is as follows:
A) 5-40 mass parts quaternary ammonium salt is weighed;
B) weigh 10-30 mass parts nonionic surfactant, be subsequently adding described in pharmaceutically Acceptable carrier;
C) by above-mentioned steps a) and b) two kinds of solution mixing, the acid of 0.5-6.5 mass parts is added;
D) weigh the iodine of 0.3-3.0 mass parts, add solution prepared by step c), be heated to 50 DEG C, stirring, to being completely dissolved clarification, adds the described pharmaceutically acceptable carrier of surplus To 100 mass parts, mix homogeneously.
The described application containing iodine composite disinfectant in poultry house and environment disinfected.
Beneficial effects of the present invention:
1) present invention utilizes the combination of quaternary cationic surfactant and iodine, sends out Shoot powerful function of killing the virus, there is the double sterilization disinfection efficacy of benzalkonium bromide and iodine. Benzalkonium bromide and iodine play the effect of disinfection jointly, make sterilizing power be greatly enhanced. Such that it is able to effectively kill hydrophilic, lipophilic virus, antibacterial.It is suitably added doses Surfactant cetyl trimethylammonium bromide, under certain condition, can strengthen iodine and kill disease The effect of poison, improves efficiency about 3.6 times.There is the quick-acting effect of notable synergistic.Quaternary ammonium salt iodine is multiple Closing disinfectant is a kind of efficient, safety, bland disinfectant.
2) use liquor strength low, use after 3200 times of dilutions, can reach bactericidal action. Sterilization, bactericidal range extensively, use safe and nontoxic, environmentally safe, and stable in properties. Good product performance, low cost, easy to use, can wide popularization and application.
3) disinfectant of the present invention has certain broad spectrum activity, can effectively kill all kinds of danger The evil pathogenic bacteria of poultry, virus and the pathogenic bacteria made a variation because of ecological deterioration, virus, noxious bacteria bud Spore;Can also effectively kill and suppress the virus pathogenic bacterias such as bird flu, streptococcus that people poultry suffer from altogether. Solve the drawback using traditional disinfection liquid to expose in China's livestock-raising, slaughtering industry.
Detailed description of the invention
Below in conjunction with embodiment, the present invention is described in detail, but the present invention is not limited to following Embodiment.
As follows according to the embodiment that technical scheme is taked:
Embodiment 1
The disinfectant of the present embodiment comprises following component:
Its preparation method is as follows:
1) 10 mass parts benzalkonium bromides (after pure), the double decyl dimethyl of 10 mass parts are weighed Ammonium bromide (after pure), adds water or glycerol wiring solution-forming.
2) weigh 30 mass parts AEO-9, be subsequently adding 50%(volume fraction) glycerol.
3) by above-mentioned steps 1) and 2) two kinds of solution mixing, add 1.7 mass parts phosphoric acid.
4) weigh 0.9 mass parts iodine, add solution prepared by step 3), be heated to 50 DEG C, Stirring, to being completely dissolved clarification, is added 50% glycerol to 100 mass parts, mix homogeneously, is surveyed Determine pH value.
Embodiment 2
The disinfectant of the present embodiment comprises following component (see Table 1):
Preparation method is with embodiment 1.
Embodiment 3
The disinfectant of the present embodiment comprises following component (see Table 1):
Preparation method is with embodiment 1.
Embodiment 4
The disinfectant of the present embodiment comprises following component (see Table 1):
Preparation method is with embodiment 1.
Embodiment 5
The disinfectant of the present embodiment comprises following component (see Table 1):
Preparation method is with embodiment 1.
Embodiment 6
The disinfectant of the present embodiment comprises following component (see Table 1):
Preparation method is with embodiment 1.
Embodiment 7
The disinfectant of the present embodiment comprises following component (see Table 1):
Preparation method is with embodiment 1.
Embodiment 8
The disinfectant of the present embodiment comprises following component (see Table 1):
Preparation method is with embodiment 1.
Comparative example
The AEO-9 of 20% in embodiment 6 is replaced by the KI of 3.6%, the disinfectant of preparation For contrast disinfectant.
The disinfectant composition of table 1 embodiment 2-8
Embodiment 9: the disinfectant of the present invention and the Disinfection Effect comparative test contrasting disinfectant
1) test method
Test with reference to the Ministry of Agriculture's " disinfectant for animals qualification test technical specification " method, adopt Quantitative with bacterial suspension
2) test strain: include escherichia coli, staphylococcus aureus, Hemolytic streptococcus, purchase In China's veterinary medicament
3) test procedure:
1. the bacterium solution of preparation is carried out viable bacteria technology, then with the phosphate buffer of 0.03M It is diluted to containing bacterium 106The test bacterium solution of CFU/mL;
2. 0.5m1 bacterium solution is drawn in the disinfectant solution 4.5m1 of test concentrations;
3. effect 5min in 20 DEG C of water-baths is put;
Draw above-mentioned bacterium medicine mixed liquor 1.0ml the most immediately, add in 9.0ml neutralizer and mix;
5. replace disinfectant solution with 0.03M phosphate buffer, carry out above steps simultaneously. As a control group.
6. carry out count plate after neutralizing 10min, calculate sterilizing rate.
Disinfectant of the present invention is shown in Table 2 to the killing effect of different strains
Table 2 disinfectant of the present invention and comparative example's sterilizing rate to different strain
Ministry of Agriculture's disinfectant for animals qualification test technical specification regulation, tests its virus killing performance and then kills Bacterium rate arrive 99.9% with, then should improve when less than this standard disinfectant concentration or extend make Use the time.
Conclusion: from the experimental results, antibacterial is killed by the disinfectant of the present invention through 3200 times of dilutions The rate of going out remains to reach more than 99.9%, and comparative example is through 800 times of dilutions to bacterial inactivation rate More than 99.9% can be reached.Quaternary ammonium salt iodine disinfectant and comparative example's bactericidal effect in the present invention Compare, it is possible to significantly improve the bactericidal effect of compositions.
Embodiment 10: according to the acute eye irritation test of the compositions of embodiment 6 preparation
Experimental animal: healthy rabbits 3, body weight 2.0-2.5kg;
Test method: cancel the solution 0.1ml of toxic agent the highest application concentration 10 times, drips in rabbit In one branch hole conjunctival sac, another branch hole is using normal saline as normal control.After dripping tested material, Eye is passively closed 4s, with triumph normal saline washing after 30s.1h, 24h, 48h after eye drip, 72h, 7d, 14d and 21d, the damage of perusal rabbit eyes conjunctiva, iris and cornea is with extensive Multiple situation.If irritant reaction does not occurs in 72h, or 7d or 14d, eye irritation is anti- Should completely recover, termination test can be shifted to an earlier date.By SSICl/1 version " disinfection technology standard " Under middle 2.3.4 item, the regulation of acute eye irritation test carries out Eye irritation scoring and stimulus intensity classification.
Result of the test: 3 animal 24h, the average score of tri-time points of 48h, 72h is: cornea Infringement 0.6, iris 0., 3, conjunctival congestion 1.0, chemosis 0.5, corneal injury < 1, rainbow Film < 1, conjunctival congestion < 2, chemosis < 2, belong to nonirritant), it was demonstrated that this disinfectant is stingless Swash property.
Embodiment 11: according to the compositions toxicity test of embodiment 6 preparation
Experimental animal: healthy Kunming mouse 20, male and female half and half, body weight 18-22g.
Trial drug: 5000mg/kg body weight.
Test method: use disposable limitation administration by gavage to per os gastric infusion of mice, give Medicine volume 20m1/kg
Body weight, Continuous Observation 14d after administration, the poisoning manifestations of record mice and death condition.
Result of the test: statistical analysis, carries out toxicity grading, and result is with reference to disinfection technology standard " In evaluate regulation under 6, the results are shown in Table 3.
Table 3 disinfectant of the present invention is to chmice acute Oral toxicity result of the test
Conclusion: toxicity test result proves, the disinfectant of embodiment 6 preparation is the most nontoxic.
Embodiment 12: use disinfectant the answering in livestock and poultry farm is sterilized of embodiment 6 preparation With
The selection of test site
Select the colony house of 1 letting animals feed, rinse ground with tap water, just carrying out after 1 hour Formula is tested.
Test material
Cotton swab, martin's bouillon, Martin's agar, nertralizer
The preparation of disinfectant: take 1ml embodiment 1 preparation disinfectant add 1000ml without The solution (1:1000) of bacterium deionized water.
The method of sampling
Sterilization before and sterilization after 20,40,60 minutes, respectively on poultry colony house ground differently Side's sampling, after being soaked with nertralizer by cotton swab, is 5 × 5cm at area during sampling2Ground Firmly wiping 10 times, and constantly conversion swab wiping surface, cut swab Cotton Gossypii end into sample solution Middle forced oscillation 100 times, by bacterium eluting, washing liquid normal saline dilution, containing 10% blood Clear Martin's agar plate is cultivated and does count plate.
Interpretation of result
Viable count × 100% before sterilizing rate %=(viable count after viable count-sterilization before sterilization)/sterilization
On-site disinfection test result
On-site disinfection test the results are shown in Table 4.
Table 4 uses disinfectant on-the-spot disinfection experimental result prepared by embodiment 6
Time C1 C2 C3 C4
Sterilization 20min sterilizing rate 98.67% 97.55% 98.45% 94.12%
Sterilization 40min sterilizing rate 99.75% 99.67% 99.82% 99.75%
Sterilization 60min sterilizing rate 99.99% 99.92% 99.96% 99.98%
C1, C2, C3, C4 are the numbering of 4 sampled points.
Conclusion: the antibacterial in plant is had by disinfectant prepared by the present invention in production application There is killing effect well.
Embodiment 13: compositions, single preparations of ephedrine and the comparative example of embodiment 6 preparation kill Bacterium effect
The compositions (prescription 1) prepared according to embodiment 6 and single preparations of ephedrine benzalkonium bromide solution (prescription 2), single preparations of ephedrine iodine solution (prescription 3), by the AEO-9 of 20% in embodiment 6 KI (prescription 4) its Comparison of effect on sterilization being replaced by 3.6% is shown in Table 5.
Compositions, single preparations of ephedrine and comparative example's bactericidal effect of table 5 embodiment 6 preparation
Conclusion: compositions that quaternary ammonium salt and iodine are prepared by adding nonionic surfactant and list Square preparation is compared has synergy effect, and using nonionic surfactant to substitute potassium iodide can To significantly improve the bactericidal effect of compositions.
Embodiment 14: the compositions xanthochromia of embodiment 6 preparation
The compositions (prescription 1) prepared according to embodiment 6 and single preparations of ephedrine benzalkonium bromide solution (prescription 2), single preparations of ephedrine iodine solution (prescription 3) and comparative example compare its Huang to fabric Metachromia.
Using soaking disinfection, often group measures 10 (warp-wise and each 5 of broadwise), sterilization group 24h is soaked, then by disinfectant typical concentrations (100 times of dilutions) room temperature (20~25 DEG C) Rinsing is dried.Sterilization 10 times, 20 times, 30 times, 40 times, 50 times respectively.Matched group is adopted With the fabric of test group adjacent parts, disinfectant is replaced to disinfect equally with aqueous solvent.Disappear After poison, rinse and dry, be measured.The results are shown in Table 6.
Conclusion: the xanthochromia of the disinfectant prepared by the present invention and comparative example's phase comparison fabric Property is lower.
The compositions xanthochromia of table 6 embodiment 6 preparation

Claims (11)

1. an iodine-containing disinfectant, based on 100 mass parts, comprises following components:
Surplus is pharmaceutically acceptable carrier;
Wherein, at least one in following compound of described nonionic surfactant: fatty alcohol-polyoxyethylene ether, Polyethylene Glycol, alkylphenol polyoxyethylene, poloxamer, lauric acid polyoxyethylene ester or castor oil polyoxyethylene ether;
At least one in hydrochloric acid, sulphuric acid or phosphoric acid of described acid.
Disinfectant the most according to claim 1, it is characterised in that based on 100 mass parts, strand quaternary ammonium salt and/ Or double-chain quaternary ammonium salt is 10-20 mass parts.
Disinfectant the most according to claim 1, it is characterised in that described strand quaternary ammonium salt is in following compound At least one: alkyl dimethyl benzyl ammonium chloride or fragrance ring hydrogen is substituted by chlorine, methyl or ethyl and is formed Replace zephiran.
Disinfectant the most according to claim 3, it is characterised in that described strand quaternary ammonium salt is alkyl dimethyl Benzyl ammonium chloride.
Disinfectant the most according to claim 1, it is characterised in that described double-chain quaternary ammonium salt is in following compound At least one: double octyl group quaternary ammonium salts, double decyl quaternary ammonium salt, double dodecyl quaternary ammonium salt or octyl-decyl quaternary ammonium salt.
Disinfectant the most according to claim 5, it is characterised in that described double-chain quaternary ammonium salt is in following compound At least one: double decyl dimethyl ammonium bromide, double-track suspended self-propelled conveyor, dimethyl benzyl ammonium chloride, bromination double (ten Dialkyl dimethyl) ethylene diammonium or 2-(2-phenoxy group) ethyl-trimethyl salmiac.
7. according to the disinfectant described in claim 1,3 or 6, it is characterised in that described pharmaceutically acceptable Carrier is alcoholic solution.
8. want the disinfectant described in 7 according to right, it is characterised in that described pharmaceutically acceptable carrier is volume Mark is the alcoholic solution of 50%.
Disinfectant the most according to claim 7, it is characterised in that described alcoholic solution is in following compound At least one: glycerol, propylene glycol, ethanol or ethylene glycol.
10. according to the preparation method containing iodine composite disinfectant according to any one of claim 1-9, including walking as follows Rapid:
A) 5-45 mass parts quaternary ammonium salt is weighed;
B) weigh 10-30 mass parts nonionic surfactant, be subsequently adding described in pharmaceutically acceptable carrier;
C) by above-mentioned steps a) and b) two kinds of solution mixing, the acid of 0.5-6.5 mass parts is added;
D) weighing the iodine of 0.3-3.0 mass parts, add solution prepared by step c), be heated to 50 DEG C, stirring is to the most molten Solve clarification, add the described pharmaceutically acceptable carrier of surplus to 100 mass parts, mix homogeneously.
11. 1 kinds according to according to any one of claim 1-9 containing iodine composite disinfectant in poultry house and environment disinfected Application.
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CN105663158B (en) * 2016-03-15 2019-06-28 浙江海正动物保健品有限公司 A kind of high concentration iodic disinfecting liquid and preparation method thereof
CN106581051A (en) * 2016-11-08 2017-04-26 太原市诚诚科技有限公司 Nano microemulsion iodine and preparation method thereof
CN108566947A (en) * 2017-03-10 2018-09-25 洛阳惠中兽药有限公司 A kind of foam disinfectant auxiliary agent, preparation method and foamaseptic prepared therefrom
CN107258839A (en) * 2017-07-12 2017-10-20 合肥华盖生物科技有限公司 A kind of composite disinfectant and preparation method thereof
CN109042728B (en) * 2018-09-19 2021-01-01 青岛安特斯生物制药有限公司 Iodine disinfectant and preparation and use method thereof
CN109601535A (en) * 2018-12-30 2019-04-12 北京盛大康成医疗技术有限公司 Disinfectant, preparation method and sterilized articles therefrom
CN111328806A (en) * 2020-03-07 2020-06-26 郑州大学 Double-linear alkyl quaternary ammonium salt complex iodine bactericide
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CN1853480A (en) * 2005-04-20 2006-11-01 齐自同 Broad-spectrum antiseptics and production thereof
CN1883273A (en) * 2006-07-06 2006-12-27 王德昌 Active disinfectant germicide and method for preparing same
CN101084749A (en) * 2007-06-05 2007-12-12 孙保兴 Betaine-bound iodine disinfectant

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