CN107047649B - A kind of compound povidone iodine thimerosal for livestock-raising and preparation method thereof - Google Patents
A kind of compound povidone iodine thimerosal for livestock-raising and preparation method thereof Download PDFInfo
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- CN107047649B CN107047649B CN201710302589.4A CN201710302589A CN107047649B CN 107047649 B CN107047649 B CN 107047649B CN 201710302589 A CN201710302589 A CN 201710302589A CN 107047649 B CN107047649 B CN 107047649B
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- thimerosal
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Classifications
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N65/00—Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N37/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids
- A01N37/12—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing the group, wherein Cn means a carbon skeleton not containing a ring; Thio analogues thereof
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
- A01N59/12—Iodine, e.g. iodophors; Compounds thereof
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N65/00—Biocides, pest repellants or attractants, or plant growth regulators containing material from algae, lichens, bryophyta, multi-cellular fungi or plants, or extracts thereof
- A01N65/40—Liliopsida [monocotyledons]
- A01N65/42—Aloeaceae [Aloe family] or Liliaceae [Lily family], e.g. aloe, veratrum, onion, garlic or chives
Abstract
The present invention relates to thimerosal field, discloses a kind of compound povidone iodine thimerosal for livestock-raising and preparation method thereof.The compound povidone iodine thimerosal includes：8 12 parts of PVP-I, 13 parts of high-molecular copolymer antiseptic, 13 parts of extract solution from aloe, 0.5 1.5 parts of KI, 1.5 2.5 parts of Potassiumiodate, 0.5 1 parts of dispersant, 100 parts of water.The thimerosal of the present invention strengthens antibacterial sterilization ability using PVP-I as main disinfection composition, and simultaneously added with high-molecular copolymer antiseptic.And the thimerosal storage stability of the present invention is good, active iodine not easily runs off in thimerosal.
Description
Technical field
The present invention relates to thimerosal field, more particularly to a kind of compound povidone iodine thimerosal for livestock-raising and its
Preparation method.
Background technology
It is loose multiple that PVP-I (Povidone iodine) is that elemental iodine is mutually complexed with polymer support PVP
Compound, PVP play carrier and hydrotropy.It is yellowish-brown to brownish red amorphous powder under normal temperature.It is micro- smelly, it is soluble in water or
Ethanol, the aqueous solution is in acidity, insoluble in ether, chloroform, acetone, ethane and carbon tetrachloride.The PVP-I aqueous solution has sterilization
Effect, iodine can be immediately directed against on bacterial cell membrane, make protein, lipid that iodine oxidation occur, so as to kill bacterium and virus.
Therefore PVP-I is widely used in the sterilizing of livestock breeding industry.
But Povidone Iodine Disinfection Solution there is also it is obvious the shortcomings that, during prolonged preserve, PVP-I is stable
Property it is poor, even in being kept in dark place down, also easily degrade, cause active content of iodine in thimerosal to reduce, so as to influence it
Antivirus effect.
The content of the invention
In order to solve the above-mentioned technical problem, the invention provides a kind of compound povidone iodine thimerosal for livestock-raising
And preparation method thereof.The thimerosal of the present invention is using PVP-I as main disinfection composition, and simultaneously added with high-molecular copolymer
Antiseptic, strengthen antibacterial sterilization ability.And the thimerosal storage stability of the present invention is good, active iodine not easily runs off in thimerosal.
The present invention concrete technical scheme be：A kind of compound povidone iodine thimerosal for livestock-raising, including it is following
The component of parts by weight：
PVP-I 8-12 parts,
High-molecular copolymer antiseptic 1-3 parts,
Extract solution from aloe 1-3 parts,
KI 0.5-1.5 parts,
Potassiumiodate 1.5-2.5 parts,
Dispersant 0.5-1 parts,
100 parts of water.
First, in the sterilization formula of liquid of the present invention, high-molecular copolymer antiseptic, the high-molecular copolymer antibacterial are contained
Agent can aid in PVP-I to carry out antibiotic and sterilizing, and effect is more preferable after compounding.
Secondly, extract solution from aloe is also contained in thimerosal of the invention, extract solution from aloe is natural extract, has and disappears
Inflammation, antibacterial, the effect of wetting are good to skin mildness.In addition, the aqueous solution of extract solution from aloe also has certain viscosity,
The easy film forming on sprinkling object after sprinkling, contains the antimicrobial activity thing such as active iodine and high-molecular copolymer antiseptic in film layer
Matter, due to the good penetrability of extract solution from aloe, in process of osmosis, active iodine and high-molecular copolymer antiseptic can be thin
Bacterium.Virus adsorption, and then kill bacterium, virus.
Furthermore also contain KI and Potassiumiodate in the present invention, KI and Potassiumiodate can generate iodine under sour environment
Simple substance, it is possible to increase the content of available iodine in thimerosal, there is the active propiodal of abundance, improve the stability of thimerosal, i.e.,
Make after preserving for a long time, thimerosal also has good Disinfection Effect.
Preferably, the high-molecular copolymer antiseptic is PET and methacrylic acid, methyl-prop
The copolymer of olefin(e) acid -2- (dimethylamino) ethyl ester.
In above-mentioned copolymer, methacrylic acid -2- (dimethylamino) ethyl ester has antibacterial functions functional group, therefore has
The antibiotic property of color.The surface potential that copolymer is obtained after above-mentioned three kinds of monomer copolymerizations can be corresponding with the change of environment acid-base property
Change：Under sour environment, the center section segment that methacrylic acid is formed is in electroneutral, and outer layer segment is unfolded in protonation,
Whole copolymer shows as positive electricity, can upset the cell membrane of bacterium, so as to have antibiotic property.Under neutral environment, methyl-prop
The center section segment that olefin(e) acid is formed shows as negative electricity, is positive charge with outer layer segment, and middle segment occurs quiet with outer layer segment
Electro ultrafiltration, antibiotic property weaken or disappeared.It is advantageous in that with the function, during thimerosal preservation and after sprinkling, disappears
Venom has an outstanding antibiotic property in acidity, high-molecular copolymer antiseptic, and after sterilizing, with PVP-I decomposition and disappear
Iodine oxidation reaction occurs when malicious, thimerosal is acid gradually to be reduced, and now the antibiotic property of high-molecular copolymer antiseptic also disappears therewith
Lose.It is well known that high-molecular copolymer antiseptic has certain side effect and harmfulness in antibacterial to zooblast.Sprinkling
After thimerosal, if high-molecular copolymer antiseptic residues in animal skin surfaces, after bacterial virus is destroyed, macromolecule is common
Polymers antiseptic can continue to play antibacterial action, and animal health is impacted.And the high-molecular copolymer antiseptic of the present invention
After sterilization, its antibacterial activity disappears automatically, good to animal safety, reduces side effect as far as possible.
Preferably, the molecular weight of the high-molecular copolymer antiseptic is 5-15 ten thousand.
Antibacterial antiplaque agent effect of the high-molecular copolymer of above-mentioned molecular weight ranges when with antibiotic property is good.
Preferably, the particle diameter of the high-molecular copolymer antiseptic is 100-200 nanometers.
Good dispersion of the high-molecular copolymer antiseptic of above-mentioned particle size range in thimerosal, is easy to preserve.
Preferably, going back thimerosal also includes pH adjusting agent, thimerosal is kept in acidity.
Preferably, addition pH adjusting agent makes thimerosal pH value maintain 5.3-5.7.
Under above-mentioned pH value range, PVP-I is easier to preserve, and stability is good；Meanwhile high-molecular copolymer antiseptic
Stronger antibacterial activity can be shown,
Preferably, the dispersant is lignin or sodium carboxymethylcellulose.Above-mentioned substance has preferable dispersion effect.
A kind of preparation method of compound povidone iodine thimerosal for livestock-raising, comprises the following steps：
(1) PVP-I, KI, Potassiumiodate are added in water successively, until previous component fully dissolves during addition
Follow-up addition again afterwards, obtains solution A；
(2) high-molecular copolymer antiseptic, extract solution from aloe, dispersant are added in solution A successively, are uniformly dispersed,
Obtain solution B；
(3) pH value of solution B is adjusted to acidity with pH adjusting agent, compound povidone iodine thimerosal is made.
Preferably, the preparation method of the high-molecular copolymer antiseptic is：Will be poly- containing hydroxyl on 9-11 part end groups
PETP is dissolved in organic solvent, and 0.5-0.7 part bromos are added under the conditions of inert gas shielding, 1-5 DEG C
Isobutyl acylbromide is reacted, and reaction product is added in absolute ethyl alcohol after 10-20h and precipitated, and is obtained after separation modified poly-
PETP；Modified PET is dissolved in dimethyl sulfoxide (DMSO), adds 0.1-0.2 part brominations
It is cuprous, 5-7 part methacrylic acids are added under inert gas shielding, 14-16h is polymerize at 55-65 DEG C, then adds 25-35
Part methacrylic acid -2- (dimethylamino) ethyl ester, continue to polymerize 6-8h at 75-85 DEG C, reaction product is sunk after polymerization
Form sediment, filtering, obtain high-molecular copolymer antiseptic.
In above-mentioned polymerization process, three kinds of monomers polymerize successively, can obtain having function described previously after polymerization
High-molecular copolymer antiseptic.
It is compared with the prior art, the beneficial effects of the invention are as follows：The thimerosal of the present invention is using PVP-I as main sterilization
Composition, and simultaneously added with high-molecular copolymer antiseptic, strengthen antibacterial sterilization ability.And the thimerosal stable storing of the present invention
Property is good, and active iodine not easily runs off in thimerosal.
Embodiment
With reference to embodiment, the invention will be further described.
Embodiment 1
A kind of compound povidone iodine thimerosal for livestock-raising, include the component of following parts by weight：
10 parts of PVP-I,
2 parts of high-molecular copolymer antiseptic,
2 parts of extract solution from aloe,
1 part of KI,
2 parts of Potassiumiodate,
0.5 part of lignin,
Appropriate pH adjusting agent,
100 parts of water.
Wherein, the high-molecular copolymer antiseptic is PET and methacrylic acid, metering system
The copolymer of acid -2- (dimethylamino) ethyl ester, its molecular weight are 8-12 ten thousand, and particle diameter is 100-200 nanometers.
A kind of preparation method of compound povidone iodine thimerosal for livestock-raising, comprises the following steps：
(1) PVP-I, KI, Potassiumiodate are added in water successively, until previous component fully dissolves during addition
Follow-up addition again afterwards, obtains solution A；
(2) high-molecular copolymer antiseptic, extract solution from aloe, dispersant are added in solution A successively, are uniformly dispersed,
Obtain solution B；
(3) pH value of solution B is maintained 5.5 or so with pH adjusting agent, compound povidone iodine thimerosal is made.
Wherein, the preparation method of the high-molecular copolymer antiseptic is：Will be poly- to benzene containing hydroxyl on 10 parts of end groups
Dioctyl phthalate second diester is dissolved in organic solvent, and 0.6 part of bromo isobutyl acylbromide is added under the conditions of inert gas shielding, 3 DEG C and is entered
Row is reacted, and reaction product is added in absolute ethyl alcohol after 15h and precipitated, obtains being modified poly terephthalic acid second two after separation
Ester；Modified PET is dissolved in dimethyl sulfoxide (DMSO), adds 0.15 part of cuprous bromide, is protected in inert gas
Shield 6 parts of methacrylic acids of lower addition, 15h is polymerize at 60 DEG C, then adds 30 parts of methacrylic acid -2- (dimethylamino) second
Ester, continue polymerase 17 h at 80 DEG C, reaction product is precipitated after polymerization, filtered, obtains high-molecular copolymer antiseptic.
Embodiment 2
A kind of compound povidone iodine thimerosal for livestock-raising, include the component of following parts by weight：
8 parts of PVP-I,
3 parts of high-molecular copolymer antiseptic,
1 part of extract solution from aloe,
0.5 part of KI,
1.5 parts of Potassiumiodate,
0.5 part of sodium carboxymethylcellulose,
Appropriate pH adjusting agent,
100 parts of water.
Wherein, the high-molecular copolymer antiseptic is PET and methacrylic acid, metering system
The copolymer of acid -2- (dimethylamino) ethyl ester, its molecular weight are 5-7 ten thousand, and particle diameter is 100-200 nanometers.
A kind of preparation method of compound povidone iodine thimerosal for livestock-raising, comprises the following steps：
(1) PVP-I, KI, Potassiumiodate are added in water successively, until previous component fully dissolves during addition
Follow-up addition again afterwards, obtains solution A；
(2) high-molecular copolymer antiseptic, extract solution from aloe, dispersant are added in solution A successively, are uniformly dispersed,
Obtain solution B；
(3) pH value of solution B is maintained 5.3 or so with pH adjusting agent, compound povidone iodine thimerosal is made.
Wherein, the preparation method of the high-molecular copolymer antiseptic is：Will be poly- to benzene two containing hydroxyl on 9 parts of end groups
Formic acid second diester is dissolved in organic solvent, and 0.5 part of bromo isobutyl acylbromide is added under the conditions of inert gas shielding, 1 DEG C and is carried out
React, reaction product is added in absolute ethyl alcohol after 10h and precipitated, obtains being modified poly terephthalic acid second two after separation
Ester；Modified PET is dissolved in dimethyl sulfoxide (DMSO), adds 0.1 part of cuprous bromide, is protected in inert gas
Shield 5 parts of methacrylic acids of lower addition, 14h is polymerize at 55 DEG C, then adds 25 parts of methacrylic acid -2- (dimethylamino) second
Ester, continue to polymerize 6h at 75 DEG C, reaction product is precipitated after polymerization, filtered, obtains high-molecular copolymer antiseptic.
Embodiment 3
A kind of compound povidone iodine thimerosal for livestock-raising, include the component of following parts by weight：
12 parts of PVP-I,
1 part of high-molecular copolymer antiseptic,
3 parts of extract solution from aloe,
1.5 parts of KI,
2.5 parts of Potassiumiodate,
1 part of lignin,
Appropriate pH adjusting agent,
100 parts of water.
Wherein, the high-molecular copolymer antiseptic is PET and methacrylic acid, metering system
The copolymer of acid -2- (dimethylamino) ethyl ester, its molecular weight are 10-15 ten thousand, and particle diameter is 100-200 nanometers.
A kind of preparation method of compound povidone iodine thimerosal for livestock-raising, comprises the following steps：
(1) PVP-I, KI, Potassiumiodate are added in water successively, until previous component fully dissolves during addition
Follow-up addition again afterwards, obtains solution A；
(2) high-molecular copolymer antiseptic, extract solution from aloe, dispersant are added in solution A successively, are uniformly dispersed,
Obtain solution B；
(3) pH value of solution B is maintained 5.7 or so with pH adjusting agent, compound povidone iodine thimerosal is made.
Wherein, the preparation method of the high-molecular copolymer antiseptic is：Will be poly- to benzene containing hydroxyl on 11 parts of end groups
Dioctyl phthalate second diester is dissolved in organic solvent, and 0.7 part of bromo isobutyl acylbromide is added under the conditions of inert gas shielding, 5 DEG C and is entered
Row is reacted, and reaction product is added in absolute ethyl alcohol after 20h and precipitated, obtains being modified poly terephthalic acid second two after separation
Ester；Modified PET is dissolved in dimethyl sulfoxide (DMSO), adds 0.2 part of cuprous bromide, is protected in inert gas
Shield 7 parts of methacrylic acids of lower addition, 16h is polymerize at 65 DEG C, then adds 35 parts of methacrylic acid -2- (dimethylamino) second
Ester, continue to polymerize 8h at 85 DEG C, reaction product is precipitated after polymerization, filtered, obtains high-molecular copolymer antiseptic.
Storage stability test, test-strips are carried out to the thimerosal in embodiment and 10% Povidone Iodine Disinfection Solution purchased in market
Part is to take 100 milliliters of thimerosal, under the conditions of lucifuge, 20 DEG C preserve 30 days at room temperature after, using direct titrimetric method (thio sulphur
Sour sodium) active content of iodine in thimerosal is determined, data are as follows：
| Group | Initial activity content of iodine | Active content of iodine after 30 days |
| Embodiment 1 | 103.8mg | 101.7mg |
| 10% Povidone Iodine Disinfection Solution purchased in market | 99.5mg | 78.5mg |
The storage stability of thimerosal of the invention is more preferable as from the foregoing.
Raw materials used in the present invention, equipment, it is the conventional raw material, equipment of this area unless otherwise noted；In the present invention
Method therefor, it is the conventional method of this area unless otherwise noted.
It is described above, only it is presently preferred embodiments of the present invention, not the present invention is imposed any restrictions, it is every according to the present invention
Any simple modification, change and the equivalent transformation that technical spirit is made to above example, still fall within the technology of the present invention side
The protection domain of case.
Claims (7)
1. a kind of compound povidone iodine thimerosal for livestock-raising, it is characterised in that include the component of following parts by weight：
PVP-I 8-12 parts,
High-molecular copolymer antiseptic 1-3 parts,
Extract solution from aloe 1-3 parts,
KI 0.5-1.5 parts,
Potassiumiodate 1.5-2.5 parts,
Dispersant 0.5-1 parts,
100 parts of water；
The preparation method of the compound povidone iodine thimerosal for livestock-raising comprises the following steps：
（1）PVP-I, KI, Potassiumiodate are added in water successively, during addition until previous component fully dissolve after again
Follow-up addition, obtains solution A；
（2）High-molecular copolymer antiseptic, extract solution from aloe, dispersant are added in solution A successively, are uniformly dispersed, is obtained
Solution B；
（3）The pH value of solution B is adjusted to acidity with pH adjusting agent, compound povidone iodine thimerosal is made；
Wherein, the preparation method of the high-molecular copolymer antiseptic is：Will be poly- to benzene two containing hydroxyl on 9-11 part end groups
Formic acid second diester is dissolved in organic solvent, and 0.5-0.7 part bromo isobutyryls are added under the conditions of inert gas shielding, 1-5 DEG C
Bromine is reacted, and reaction product is added in absolute ethyl alcohol after 10-20h and precipitated, and is obtained after separation modified poly- to benzene two
Formic acid second diester；Modified PET is dissolved in dimethyl sulfoxide (DMSO), adds 0.1-0.2 part cuprous bromides,
5-7 part methacrylic acids are added under inert gas shielding, 14-16h is polymerize at 55-65 DEG C, then add 25-35 part methyl
Acrylic acid -2-（Dimethylamino）Ethyl ester, continue to polymerize 6-8h at 75-85 DEG C, reaction product is precipitated after polymerization, mistake
Filter, obtains high-molecular copolymer antiseptic.
A kind of 2. compound povidone iodine thimerosal for livestock-raising as claimed in claim 1, it is characterised in that the height
Molecule copolymer antiseptic is PET and methacrylic acid, methacrylic acid -2-（Dimethylamino）Ethyl ester
Copolymer.
A kind of 3. compound povidone iodine thimerosal for livestock-raising as claimed in claim 2, it is characterised in that the height
The molecular weight of molecule copolymer antiseptic is 5-15 ten thousand.
A kind of 4. compound povidone iodine thimerosal for livestock-raising as claimed in claim 1, it is characterised in that the height
The particle diameter of molecule copolymer antiseptic is 100-200 nanometers.
5. a kind of compound povidone iodine thimerosal for livestock-raising as claimed in claim 2, it is characterised in that also include
PH adjusting agent, thimerosal is set to keep in acidity.
A kind of 6. compound povidone iodine thimerosal for livestock-raising as claimed in claim 5, it is characterised in that addition
PH adjusting agent makes thimerosal pH value maintain 5.3-5.7.
7. a kind of compound povidone iodine thimerosal for livestock-raising as claimed in claim 1, it is characterised in that described point
Powder is lignin or sodium carboxymethylcellulose.
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| CN110204471B (en) * | 2019-06-12 | 2021-03-09 | 万华化学集团股份有限公司 | Method for catalyzing vitamin A isomerization by in-situ generation of iodine |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2461296Y (en) * | 2001-01-10 | 2001-11-28 | 陈书侗 | Sterilizing articles |
| CN101073325A (en) * | 2006-05-19 | 2007-11-21 | 谭惠民 | Povidone-iodine antibacterial material and its production |
| CN101642467A (en) * | 2008-08-06 | 2010-02-10 | 吴天祥 | Long-acting disinfection paste |
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| CN100554296C (en) * | 2007-02-28 | 2009-10-28 | 中山大学 | Reactable polymer antibacterial agent and its production and application |
| CN101168586B (en) * | 2007-09-28 | 2010-09-15 | 东南大学 | Antibacterial macromolecule polymer and preparation method thereof |
| AU2009255322B2 (en) * | 2008-05-29 | 2015-12-03 | Dsm Ip Assets B.V. | Antimicrobial polymers and their uses |
| CN103304755B (en) * | 2013-06-27 | 2016-01-20 | 汕头大学 | A kind of antibacterial polypropylene block copolymer and preparation method thereof and material modified containing this segmented copolymer |
| CN103720713B (en) * | 2013-12-18 | 2016-04-20 | 深圳市安多福消毒高科技股份有限公司 | A kind of high chelated iodine and preparation method thereof |
| CN105694025A (en) * | 2014-11-24 | 2016-06-22 | 天津博克尼科技发展有限公司 | Preparation method of glyceryl polyether and iodine complex |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN2461296Y (en) * | 2001-01-10 | 2001-11-28 | 陈书侗 | Sterilizing articles |
| CN101073325A (en) * | 2006-05-19 | 2007-11-21 | 谭惠民 | Povidone-iodine antibacterial material and its production |
| CN101642467A (en) * | 2008-08-06 | 2010-02-10 | 吴天祥 | Long-acting disinfection paste |
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