CN104604934B - A kind of compound iodine disinfectant and its preparation method and application - Google Patents
A kind of compound iodine disinfectant and its preparation method and application Download PDFInfo
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- CN104604934B CN104604934B CN201510030080.XA CN201510030080A CN104604934B CN 104604934 B CN104604934 B CN 104604934B CN 201510030080 A CN201510030080 A CN 201510030080A CN 104604934 B CN104604934 B CN 104604934B
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Abstract
The invention provides a kind of compound iodine disinfectant and its preparation method and application.Compound iodine disinfectant, weight percent is made up of the raw material comprising quaternary ammonium salt, iodine, Potassiumiodate, inorganic acid and water.Preparation method is：Quaternary ammonium salt, inorganic acid and water are stirred into Hybrid Heating first and are incubated, iodine and Potassiumiodate is added, continuation insulated and stirred, which is reacted to iodine, to be completely dissolved.Both the characteristics of fast sterilization degree of sterilization with iodine class disinfectant fast efficiency high, the characteristics of having the quaternary ammonium disinfectant bactericidal duration long again, so as to reach the effect of reduction frequency of use.Preparation method is simple, and technical process is simple, is easily controlled, with short production cycle, production cost is low, is adapted to industrialized production.Can be as the disinfection product prepared applied to key component, stability is good, nontoxic non-stimulated.It can also apply in the sterilization of animal husbandry sterilization and aquatic products industry, sterilization and good antimicrobial effect.
Description
Technical field
The present invention relates to disinfectant technical field, one kind that more particularly to animal husbandry sterilization and aquatic products industry sterilization are used is combined
Iodine disinfectant and its preparation method and application.
Background technology
In order to reach sterilisation purpose to pollutant, different classes of, different dosage forms, different efficacies iodine sterile products it is just extensive
In terms of health, daily life, agriculture and animal husbandry aquaculture and drinking water, now widely used disinfectant is mainly iodine
Class, quaternary ammonium salt, and chloride class disinfectant, but in actual use, there is apparent lack in single disinfectant
Fall into, such as：Quaternary ammonium disinfectant bactericidal effect is poor, and concentration is high, although good containing iodine and chlorine-containing disinfectant bactericidal effect,
Duration is short, and frequency of use is high.Therefore, occur in that quaternary ammonium salt is complexed iodine disinfectant, have that bactericidal effect is good and the duration concurrently
Long advantage, but existing quaternary ammonium salt chelated iodine existence and stability is poor, the drawbacks of rate of recovery of iodine is low result in resource significantly
Waste.
The content of the invention
For the drawbacks described above and problem of prior art, it is an object of the invention to provide a kind of compound iodine disinfectant and its system
Preparation Method, it is that quaternary ammonium salt is complexed disinfectant germicide to be combined iodine disinfectant, and stability is good, and bactericidal effect is good, and the duration is long；And
And preparation method is simple.Solve that existing quaternary ammonium salt chelated iodine existence and stability is poor, the low technical problem of the rate of recovery of iodine.
In order to achieve the above object, the present invention provides following technical scheme：
A kind of compound iodine disinfectant, weight percent, by comprising 5%~60% quaternary ammonium salt, 0.1%~5% iodine,
What the raw material of 0~0.5% Potassiumiodate, 1%~25% inorganic acid and excess water was made.
Further, weight percent, by comprising 30%~50% quaternary ammonium salt, 1%~3% iodine, 0.01~
What the raw material of 0.1% Potassiumiodate, 5%~25% inorganic acid and excess water was made.
Further, weight percent, by comprising 50% quaternary ammonium salt, 2.1% iodine, 0.05% Potassiumiodate,
What 22% inorganic acid and the raw material of excess water were made.
Further, the quaternary ammonium salt is dication quaternary ammonium salt.
Specifically, chemical entitled 2- hydroxy-ns-Alkyl-methyl propane -1,3 ammonium chloride of dication quaternary ammonium salt, it is tied
Structure formula is as follows：Wherein R1, R2The carbon chain lengths of group are 1~16
Individual carbon atom.It is preferred that R1The carbon chain lengths of group are 1 carbon atom, R2The carbon chain lengths of group are 12 carbon atoms.
Further, the inorganic acid is phosphoric acid and/or hydrochloric acid.When inorganic acid is the mixture of phosphoric acid and hydrochloric acid, two
Person is with any than mixing.
A kind of preparation method of compound iodine disinfectant of the present invention, through the following steps that realize：Weight percent,
Weigh each raw material；Quaternary ammonium salt, inorganic acid and water are added in reactor, 40 DEG C~80 DEG C, insulation are heated to while stirring；After
Continuous stirring, adds iodine and Potassiumiodate, and then insulation reaction to iodine is completely dissolved, and cools down, obtains compound iodine disinfectant.
A kind of application of the compound iodine disinfectant of the present invention in aquatic products industry sterilization.
A kind of application of the compound iodine disinfectant of the present invention in animal husbandry sterilization.
The compound iodine disinfectant of the present invention is the good quaternary ammonium salt chelated iodine disinfection of a kind of environmental protection, efficient stable
Agent.Both the characteristics of fast sterilization degree of sterilization with iodine class disinfectant fast efficiency high, again with quaternary ammonium disinfectant bactericidal
The characteristics of duration is long, so as to reach the effect for reducing frequency of use.Inorganic acid in the compound iodine disinfectant of the present invention
The addition of (or Potassiumiodate and inorganic acid) so that have excessive H in whole system+Ion (or IO3 -Ion and H+Ion),
So that disproportionated reaction (the I that iodine occurs in water2+ 3H2O=5HI+HIO3), it is impossible to forward reaction, so that the stabilization of iodine
Property improve, the iodine rate of recovery is high, up to more than 99%.Its preparation method is simple, and technical process is simple, is easily controlled, with short production cycle,
Production cost is low, is adapted to industrialized production.
Want based on the compound iodine disinfectant of the present invention component preparation disinfection product stability is good, usability
Good, dissolubility is good, use cost is low, and safety and environmental protection the characteristics of degradable, belongs to nontoxic nonirritant Green Product.
The compound iodine disinfectant of the present invention, sterilization and good antimicrobial effect, to Candida albicans, Escherichia coli, golden yellow grape
Sugared bacterium etc. is respectively provided with sterilization and fungistatic effect well.
Embodiment
Below in conjunction with embodiments of the invention, technical scheme is clearly and completely described, it is clear that
Described embodiment is only a part of embodiment of the invention, rather than whole embodiments.Based on the implementation in the present invention
Example, the every other embodiment that those of ordinary skill in the art are obtained under the premise of creative work is not made is belonged to
The scope of protection of the invention.
Embodiment 1
Compound iodine disinfectant, weight percent, by including 60% dication quaternary ammonium salt, 3% iodine, 1% phosphorus
What the raw material of acid and the water of surplus was made.
The dication quaternary ammonium salt is 2- hydroxy-ns-Alkyl-methyl propane -1,3 ammonium chloride, and its structural formula is as follows：R1The carbon chain lengths of group are 1 carbon atom, R2The carbochain of group
Length is 12 carbon atoms.Its synthetic method is shown in the content described in embodiment 8.
Being combined iodine disinfectant preparation method is：By above-mentioned percetage by weight, each raw material is weighed；By dication quaternary ammonium salt,
Phosphoric acid and water are added in reactor, 40 DEG C are heated to while stirring, insulation improves and continues to stir after mixing speed, adds iodine,
Insulated and stirred is reacted 6 hours afterwards, is completely dissolved to iodine, is cooled down, is obtained the compound iodine disinfectant of embodiment 1.
Embodiment 2
Compound iodine disinfectant, weight percent, by including 60% dication quaternary ammonium salt, 5% iodine, 5% phosphorus
What the raw material of acid and the solvent of surplus was made.The solvent is water and ethylene glycol, and wherein ethylene glycol accounts for 3% in the feed, and water is accounted for
12%.
The dication quaternary ammonium salt is using 2- hydroxy-ns-chlorination of Alkyl-methyl propane -1,3 described in embodiment 1
Ammonium.
Being combined iodine disinfectant preparation method is：By above-mentioned percetage by weight, each raw material is weighed；By dication quaternary ammonium salt,
Phosphoric acid, ethylene glycol and water are added in reactor, 40 DEG C are heated to while stirring, insulation improves and continues to stir after mixing speed,
Iodine is added, insulated and stirred is reacted 6 hours afterwards, is completely dissolved to iodine, cool down, obtain the compound iodine disinfectant of embodiment 2.
Embodiment 3
Compound iodine disinfectant, weight percent, by including 30% dication quaternary ammonium salt, 1.6% iodine, 1%
What the raw material of the alcohol solvent of phosphoric acid, 5% hydrochloric acid and surplus was made.
The dication quaternary ammonium salt is using 2- hydroxy-ns-chlorination of Alkyl-methyl propane -1,3 described in embodiment 1
Ammonium.
Being combined iodine disinfectant preparation method is：By above-mentioned percetage by weight, each raw material is weighed；By dication quaternary ammonium salt,
Phosphoric acid, hydrochloric acid and ethanol are added in reactor, 60 DEG C are heated to while stirring, insulation improves and continues to stir after mixing speed,
Iodine is added, insulated and stirred is reacted 2 hours afterwards, is completely dissolved to iodine, cool down, obtain the compound iodine disinfectant of embodiment 3.
Embodiment 4
Compound iodine disinfectant, weight percent, by including 50% dication quaternary ammonium salt, 1.05% iodine, 0.5%
Phosphoric acid, the raw material of the ethylene glycol solvent of 5% hydrochloric acid and surplus is made.
The dication quaternary ammonium salt is using 2- hydroxy-ns-chlorination of Alkyl-methyl propane -1,3 described in embodiment 1
Ammonium.
Being combined iodine disinfectant preparation method is：By above-mentioned percetage by weight, each raw material is weighed；By dication quaternary ammonium salt,
Phosphoric acid, hydrochloric acid and ethylene glycol are added in reactor, 80 DEG C are heated to while stirring, insulation continues to stir after improving mixing speed
Mix, add iodine, insulated and stirred is reacted 4 hours afterwards, is completely dissolved to iodine, cool down, obtain the compound iodine disinfectant of embodiment 4.
Embodiment 5
Compound iodine disinfectant, weight percent, by comprising 50% dication quaternary ammonium salt, 1.05% iodine,
0.05% Potassiumiodate, 0.5% phosphoric acid, the raw material of the ethylene glycol solvent of 5% hydrochloric acid and surplus are made.
The dication quaternary ammonium salt is using 2- hydroxy-ns-chlorination of Alkyl-methyl propane -1,3 described in embodiment 1
Ammonium.
Being combined iodine disinfectant preparation method is：By above-mentioned percetage by weight, each raw material is weighed；By dication quaternary ammonium salt,
Phosphoric acid, hydrochloric acid and ethylene glycol are added in reactor, 80 DEG C are heated to while stirring, insulation continues to stir after improving mixing speed
Mix, add iodine and Potassiumiodate, insulated and stirred is reacted 4 hours afterwards, is completely dissolved to iodine, cool down, the compound iodine for obtaining embodiment 5 disappears
Toxic agent.
Embodiment 6
Compound iodine disinfectant, weight percent, by including 50% dication quaternary ammonium salt, 2.1% iodine, 0.05%
Potassiumiodate, 20% phosphoric acid, 2% hydrochloric acid, 1% ethanol, the raw material of the water of 6% ethylene glycol and surplus be made.It is molten
Agent includes ethanol, ethylene glycol and water.
The dication quaternary ammonium salt is using 2- hydroxy-ns-chlorination of Alkyl-methyl propane -1,3 described in embodiment 1
Ammonium.
Being combined iodine disinfectant preparation method is：By above-mentioned percetage by weight, each raw material is weighed；By dication quaternary ammonium salt,
Phosphoric acid, hydrochloric acid, ethanol, ethylene glycol and water are added in reactor, 40 DEG C are heated to while stirring, insulation improves mixing speed
Continue to stir afterwards, add iodine and Potassiumiodate, insulated and stirred is reacted 5 hours afterwards, is completely dissolved to iodine, cool down, obtain embodiment 6
Compound iodine disinfectant.
The contrast experiment of embodiment 7 example is without inorganic acid
Compound iodine disinfectant, weight percent, by including 50% dication quaternary ammonium salt, 2.1% iodine, 0.05%
Potassiumiodate, 1% ethanol, the raw material of the water of 6% ethylene glycol and surplus be made.Solvent includes ethanol, ethylene glycol and water.
The dication quaternary ammonium salt is using 2- hydroxy-ns-chlorination of Alkyl-methyl propane -1,3 described in embodiment 1
Ammonium.
Being combined iodine disinfectant preparation method is：By above-mentioned percetage by weight, each raw material is weighed；By dication quaternary ammonium salt,
Ethanol, ethylene glycol and water are added in reactor, 40 DEG C are heated to while stirring, insulation improves and continues to stir after mixing speed,
Iodine and Potassiumiodate are added, insulated and stirred is reacted 5 hours afterwards, is completely dissolved to iodine, cooled down, obtain the compound iodine sterilization of embodiment 7
Agent.
Embodiment 8
Dication quaternary ammonium salt (the 2- hydroxy-ns-Alkyl-methyl propane -1,3 that above-described embodiment 1 is used into embodiment 7
Ammonium chloride) synthetic method, it is as follows：
Step 1: by weight, weigh including 100 parts of Dodecyl Dimethyl Amines, 50 parts of epoxychloropropane, 45 part three
The raw material of methylamine hydrochloride, 0.05~0.2 part of complexing agent and 50~200 parts of water；
Step 2: trimethylamine hydrochloride, complexing agent and water are added in reactor, after being well mixed, dodecane is added
Base dimethyl tertiary amine, stirs, and obtains mixed reactant；
Step 3: mixed reactant is heated into 75 DEG C~85 DEG C, then insulation is added dropwise epoxy chlorine into mixed reactant
Propane, control completion of dropping in 1 hour；Then insulated and stirred is reacted 2~4 hours within the temperature range of 78 DEG C~82 DEG C；
Obtain 2- hydroxy-ns-ammonium chloride of Alkyl-methyl propane -1,3.
The present invention places the compound iodine disinfectant of embodiment 1 to embodiment 7 after different time, carries out available iodine to it and contains
The measure of amount and quaternary ammonium salt content.Determination data see the table below 1.
Wherein, determination of the content of iodine：Example 1 is distinguished to the compound iodine disinfectant 10g of embodiment 7, it is accurately weighed, put iodine
In measuring bottle, the 50mL that adds water is allowed to be completely dissolved, be titrated to sodium thiosulfate titrating solution (0.1mol/L) it is colourless, per 1ml it is thio
The I of sodium sulphate titrating solution (0.1mol/L) equivalent to 12.69mg2。
Quaternary ammonium salt assay：Precision weighs embodiment 1 to the compound iodine disinfectant 0.15g of embodiment 7, puts 250mL iodine
In measuring bottle, the 30mL that adds water makes dissolving, sequentially adds sodium hydroxide test solution 1mL, chloroform 15mL, bromophenol blue indicator solution 0.5mL, shakes
Shake uniform.Titrated again with tetraphenylboron sodium titrating solution, in titration with forced oscillation untill the blueness in chloroform layer disappears.Record four
Benzene boron sodium titrating solution (0.02mol/L) consumes volume, and the tetraphenylboron sodium titrating solution (0.02mol/L) per 1mL is equivalent to 7.23mg
Double-chain quaternary ammonium salt.
Table 1
It can be drawn from the detection data of table 1, the rate of recovery of iodine can reach in compound iodine disinfectant of the invention
100%, almost do not waste, and also available iodine content is only slightly reduced with the resting period, and stability is fine.
Application example 1
Application of the compound iodine disinfectant of the present invention in aquatic products industry sterilization.To Candida albicans, Escherichia coli, golden yellow Portugal
Grape sugar bacterium etc. is respectively provided with sterilization and fungistatic effect well.
Application example 2
Application of the compound iodine disinfectant of the present invention in animal husbandry sterilization.To Candida albicans, Escherichia coli, golden yellow Portugal
Grape sugar bacterium etc. is respectively provided with sterilization and fungistatic effect well.
The present invention carries out sterilization experiment using the compound iodine disinfectant sample of embodiment 5, respectively to Candida albicans, large intestine
Bacillus and Staphylococcus aureus carry out fungi killing test.Killed simultaneously using the existing sterilization of two kinds of last of the ten Heavenly stems Matsubain and PVP-I
Microbial inoculum sample makees parallel contrast experiment.The nertralizer used in experiment is 0.5%Na2S2O3The Tween-80 of+0.7% lecithin+2%
0.03mol/L PBS solution.Test basis are《Disinfection technology standard》The content that (version in 2002) 2.1.1.9 sections are recorded.
Experimental result is respectively as shown in table 2 below, table 3 and table 4.
The Candida albicans sterilization experiment result of table 2
The experimental data provided according to above-mentioned table 2, sterilizes logarithm value>When 5, last of the ten Heavenly stems Matsubain and PVP-I are used alone most
Low concentration is respectively that 1000mg/L acts on effect in 10 minutes and 50mg/L 10 minutes.And the compound iodine sterilization of the embodiment of the present invention 5
(dication quaternary ammonium salt presses 20 with iodine for agent:1 compounding complexing), it is 12.5mg/L in iodine concentration, quaternary ammonium salinity is 250mg/L
When, effect can reach for 10 minutes>5 sterilization logarithm value.Therefore, in sterilization experiment, the present invention has very to Candida albicans
Good sterilization and bacteriostasis effect.
Table 3, Escherichia coli sterilization experiment result
The experimental data provided according to above-mentioned table 3, sterilizes logarithm value>When 5, last of the ten Heavenly stems Matsubain and PVP-I are used alone most
Low concentration is respectively that 1000mg/L acts on effect in 10 minutes and 50mg/L 10 minutes.And the compound iodine sterilization of the embodiment of the present invention 5
(dication quaternary ammonium salt presses 20 with iodine for agent:1 compounding complexing), it is 12.5mg/L in iodine concentration, surfactant concentration is
During 312.5mg/L, effect can reach for 10 minutes>5 sterilization logarithm value.Therefore, in sterilization experiment, the present invention is to large intestine bar
Bacterium has good sterilization and bacteriostasis effect.
The Staphylococcus aureus sterilization experiment result of table 4
According to the experimental data of above-mentioned table 4, logarithm value is sterilized>When 5, last of the ten Heavenly stems Matsubain and PVP-I exclusive use are minimum dense
Degree is respectively that 1500mg/L acts on effect in 10 minutes and 75mg/L 10 minutes.And the compound iodine disinfectant of the embodiment of the present invention 5 is (double
Cation quaternary ammonium salt presses 20 with iodine:1 compounding complexing), it is 25mg/L in iodine concentration, when surfactant concentration is 500mg/L, makees
It can reach with 10 minutes>5 sterilization logarithm value.Therefore, in sterilization experiment, the present invention has well to Staphylococcus aureus
Sterilization and bacteriostasis effect.
Therefore, compound iodine sanitizer disinfecting effect of the invention is better than sterilization individually with PVP-I or last of the ten Heavenly stems Matsubain
Effect, can be applied in animal husbandry sterilization and aquatic products industry sterilization, to Candida albicans, Escherichia coli, golden yellow glucose fungus etc.
It is respectively provided with sterilization and fungistatic effect well.
The foregoing is only a specific embodiment of the invention, but protection scope of the present invention is not limited thereto, any
Those familiar with the art the invention discloses technical scope in, change or replacement can be readily occurred in, should all be contained
Cover within protection scope of the present invention.Therefore, protection scope of the present invention described should be defined by scope of the claims.
Claims (4)
1. a kind of compound iodine disinfectant, it is characterised in that：Weight percent, by comprising 50% dication quaternary ammonium salt,
2.1% iodine, 0.05% Potassiumiodate, 20% phosphoric acid, 2% hydrochloric acid, 1% ethanol, the water of 6% ethylene glycol and surplus
Raw material be made；Solvent includes ethanol, ethylene glycol and water；
Chemical entitled 2- hydroxy-ns-Alkyl-methyl propane -1,3 ammonium chloride of the dication quaternary ammonium salt, its structural formula is such as
Under：Wherein, R1The carbon chain lengths of group are 1 carbon atom, R2Base
The carbon chain lengths of group are 12 carbon atoms.
2. a kind of preparation method of compound iodine disinfectant as claimed in claim 1, it is characterised in that：Through the following steps that real
Existing：Weight percent, weighs dication quaternary ammonium salt, phosphoric acid, hydrochloric acid, ethanol, ethylene glycol and water and adds in reactor, stir
40 DEG C are heated to while mixing, insulation improves and continues to stir after mixing speed, adds iodine and Potassiumiodate, insulated and stirred is anti-afterwards
Answer 5 hours, be completely dissolved to iodine, cool down, obtain compound iodine disinfectant.
3. a kind of application of the compound iodine disinfectant as claimed in claim 1 in aquatic products industry sterilization.
4. a kind of application of the compound iodine disinfectant as claimed in claim 1 in animal husbandry sterilization.
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Families Citing this family (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| US10092006B2 (en) | 2014-03-31 | 2018-10-09 | Iotech International | Stable compositions of uncomplexed iodine and methods of use |
| CN106259442A (en) * | 2016-07-19 | 2017-01-04 | 成都科宏达科技有限公司 | A kind of compound disinfectant containing iodine |
| CN111035674A (en) * | 2020-03-06 | 2020-04-21 | 吉林云飞医药有限公司 | Aner iodine skin mucosa disinfectant as well as preparation method and application thereof |
| CN111328806A (en) * | 2020-03-07 | 2020-06-26 | 郑州大学 | Double-linear alkyl quaternary ammonium salt complex iodine bactericide |
| CN112841181B (en) * | 2020-12-31 | 2022-06-17 | 佛山市正典生物技术有限公司 | Stable iodine-containing disinfectant and preparation method thereof |
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