CN1703958A - Highly efficient broad spectrum disinfectant, its preparation method and application - Google Patents
Highly efficient broad spectrum disinfectant, its preparation method and application Download PDFInfo
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- CN1703958A CN1703958A CN 200410042803 CN200410042803A CN1703958A CN 1703958 A CN1703958 A CN 1703958A CN 200410042803 CN200410042803 CN 200410042803 CN 200410042803 A CN200410042803 A CN 200410042803A CN 1703958 A CN1703958 A CN 1703958A
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Abstract
The invention discloses a highly efficient broad spectrum disinfectant and its preparation method, wherein the disinfecting agent comprises porous phenylethene carrier, iodine and potassium iodide adsorbed thereon, wherein divinylbenzene is used as the sealing film on the phenylethene carrying agent. The disinfectant has stabilized disinfecting effect, and can be used for the sterilization for various water environments and air.
Description
Technical field
The present invention relates to a kind of high-efficiency broad spectrum disinfectant and preparation method thereof, relating in particular to a kind of is high-efficiency broad spectrum disinfectant and preparation method thereof of main effectively sterilization component with iodine, and this disinfectant can be used for various water environments sterilizations and purify air.
Background technology
Along with the development of producing and living, more and more higher to the requirement of disinfectant.Disinfectant is widely used in the various aspects of producing and living, as in the water environment, in the wet environment and in the dry environment.Wherein, disinfectant to water treatments such as drinking water, middle water is a lot, with the chlorine type is many, but the disinfectant toxic and side effect of active ingredient that with chlorine is sterilizing is too strong, the harm that during especially as drinking water disinfect human body is brought is heavier, and " do not advocate with chlorine and do drinking water disinfect " appealed by the World Health Organization.
At present, the disinfectant that is mainly used in drinking water and freshwater aquiculture has: ozone, chlorine dioxide, triiodide resin, high polyiodine resin etc., as, application number is that 89108748.6 Chinese patent application " preparation and the effect thereof of triiodide resin (disinfectant) " discloses a kind of triiodide ion (I
3 -) and strong alkaline quaternary ammonium salt anionic exchanger resin complex compound---triiodide resin, still, owing to defectives such as influence that is subjected to environment, water quality and the easy loss of disinfectant active ingredient can not extensive use.
Iodine type disinfectant especially iodine resin to make disinfectant be current first-selection, also be the main selection and the application direction of following drinking water disinfection bactericide development and water treatment, for example, triiodide resin, high polyiodine resin etc.Yet, iodine resin molecular structure instability, distillation causes active ingredient not lasting easily, has therefore caused shortcomings such as efficient is low, cost height, so can not be widely used.
Summary of the invention
The technical problem that the present invention solves is the stability that has improved iodine type disinfectant resinous molecular structure, has reduced the active ingredient sublimability, thereby has made the gained disinfectant stable, lasting, efficient, easy to use.
Another technical problem that the present invention solves has been to provide the preparation method of this high-efficiency broad spectrum iodine type disinfectant.
The technical problem that the present invention solves also is to provide this high-efficiency broad spectrum iodine type Application of disinfectants.
Basic design of the present invention is to improve iodine type disinfectant molecular structure stabilized and reduce the active ingredient sublimability by changing carrier property.Do envelope film on the polystyrene support with polydivinylbenezene, thereby carrier structure is changed, after effective disinfection composition iodine and carrier are compound, effectively the disinfection composition superficial density strengthens, its distillation is suppressed in the bottom of carrier film, thereby make the disinfectant molecular structure stabilized, be not easy distillation, disinfection effect is stable.
Technical scheme of the present invention is described in further detail below.
The high-efficiency broad spectrum disinfectant that the present invention proposes comprises expanded polystyrene carrier and absorption active ingredient iodine and potassium iodide thereon, and this carrier is prepared by following method:
A. after styrene, divinylbenzene mix, add benzoyl peroxide and paraffin, stir, get oil phase;
B. water, gelatin and methylene blue are mixed, obtain water;
C. water is warming up to 40-46 ℃, adds oil phase, stir and be warming up to 75-80 ℃ to aqueous phase, insulation, oil droplet solidifies 95-98 ℃ of back intensification, and insulation is filtered, and cleans, and oven dry obtains particulate material;
D. with gained particulate material Petroleum ether extraction, discard extract, add chloromethyl methyl ether in solid matter, expand, add alchlor, be warming up to 35-45 ℃, preferred 40 ℃, reaction is filtered, with alcohol washing, vacuum drying;
E. the gained material is added in the benzene, expand, under agitation add the methanol solution of trimethylamine, be warming up to 25-35 ℃, preferred 30 ℃, reaction is filtered, and oven dry is soaked with saturated aqueous common salt, regulating pH with hydrochloric acid is 3-5, washing, and buck cleans, and promptly obtains pelleted substrate.
Wherein, among the step a, described styrene is preferably the 230-260 weight portion, and as polymerization single polymerization monomer, the gained polystyrene is a carrier; Described divinylbenzene is preferably the 30-70 weight portion, and preferred 42-52 weight portion is as carrier envelope film; The preferred 3-4 weight portion of described benzoyl peroxide is as polymerization initiator; The preferred 100-120 weight portion of described paraffin as pore-foaming agent, makes polystyrene support produce the space, thereby can make its compound active ingredient;
Among the step b, the preferred 800-1000 weight portion of described water; The preferred 8-10 weight portion of described gelatin is as dispersant; Described methylene blue solution is as anion carrier dispersant;
Among the step c, stir behind the adding oil phase,, can control the oil droplet size and the uniformity by regulating speed of agitator; Temperature retention time is preferred 1-3 hour for the first time, more preferably 2 hours; Temperature retention time is preferred 6-8 hour for the second time; The insulation back is cleaned for the second time, preferably cleans with 60-80 ℃ of water;
In the steps d, the preferred 1000-1200 weight portion of described chloromethyl methyl ether is as chloromethyl agent; The preferred 3-5 of described expansion hour; The preferred 210-270 weight portion of described anhydrous alchlor as catalyzer, can once add, and preferred gradation adds, and more preferably divides 3 addings; The preferred 6-8 of described reaction hour; Described alcohol washing particular methanol is or/and washing with alcohol; Described vacuum drying, preferred 60-65 ℃ of following vacuum drying;
Among the step e, the preferred 500-600 weight portion of described benzene; Described expansion, preferred 3-5 of time hour; The preferred 30-40% weight of described trimethylamine methanol solution, 33% weight most preferably, its weight preferred 600-650 weight portion as aminating agent, constantly stirs down in preferred 5-7 hour it is added reaction system; The preferred 9-10 of described reaction hour; Described oven dry is preferably 45-55 ℃ of oven dry; Described saline solution is as the agent of vector resin cation exchange remodeling; Described hydrochloric acid is as the agent of vector resin cation exchange remodeling.
Preparation high-efficiency broad spectrum disinfectant also needs following steps:
F. above-mentioned gained carrier is joined in the ethanolic solution that is dissolved with iodine and potassium iodide, stirring reaction leaves standstill after being cooled to room temperature, filter, and the washing of 10% saline solution, water washing, vacuum drying promptly gets the high-efficiency broad spectrum disinfectant.
Wherein, the preferred 300-400 weight portion of described carrier; Preferred 600 weight portions of described ethanolic solution wherein are dissolved with iodine 250-280 weight portion, are dissolved with potassium iodide 130-160 weight portion, make active ingredient iodine and potassium iodide and carrier amount proportioning suitable; The preferred temperature 90-120 of the condition of described stirring reaction ℃, pressure 1.0 * 1.2 * 10
5Pa-2.0 * 1.2 * 10
5Pa, more preferably 1.5 * 1.2 * 10
5Pa, preferred 8-12 of reaction time hour, more preferably 10 hours; Described leaving standstill, preferred 8-12 of time hour, more preferably 10 hours; Described vacuum drying, preferably vacuum drying in the time of 40-45 ℃.
The various raw materials that use among the present invention: styrene, benzoyl peroxide, divinylbenzene, gelatin, methylene blue, benzinum, alcohol, methyl alcohol, ethanol, benzene, hydrochloric acid, sodium chloride, trimethylamine methyl alcohol, chloromethyl methyl ether, alundum (Al, paraffin, potassium iodide are for analyzing pure or chemical pure, iodine (AR level) all can be buied from the chemical reagent shop.
Disinfectant outward appearance of the present invention is a diameter 0.4-2.2mm carbon black look silver photosphere shape particle, and water insoluble, effectively sterilization dose (weight percentage of active ingredient) is 39-42%.This disinfectant lost efficacy after using its active ingredient consumption, was translucent light brown, and the carrier reproducible utilization specifically is that the carrier after losing efficacy is embathed with buck and saline solution respectively, and water embathes and gets final product again.The carrier regeneration cycle is used, and has simplified production technology, has reduced production cost.
With the disinfectant that said method makes, its styrene carrier is sealed film by divinylbenzene, Stability Analysis of Structures, and active ingredient iodine is difficult for distillation, Heat stability is good, long service life.Below in conjunction with experimental data its premium properties is described:
Disinfectant and other iodine type disinfectants that the present invention is proposed heated 2 hours under similarity condition, its loss of effective components amount of weighing measurement then, and the result is as follows:
| Temperature (℃) | ??40 | ??60 | ??80 | ??100 | ??120 |
| Disinfectant loss of effective components of the present invention (% weight) | ??0 | ??0 | ??0 | ??1.8 | ??16 |
| Other iodine type disinfectant loss of effective components (% weight) | ??0 | ??0.4 | ??5 | ??8 | ??22 |
From above experimental result as can be seen, disinfectant of the present invention just begins to lose active ingredient in the time of 100 ℃, and other iodine type disinfectants just begin loss in the time of 60 ℃; And under uniform temp, the loss of effective components amount of disinfectant of the present invention is more much lower than other iodine type disinfectant loss of effective components amounts, and as seen, the disinfectant heat endurance that the present invention proposes will be better than other iodine type disinfectants of the prior art far away.
Disinfectant sterilizing ability of the present invention is extremely strong, especially sterilizing ability is stronger in water, it can be in 0.4 second time, oxidizing bacteria endochylema and combine with the amino of protein, permeability by changing bacterial cell membrane and intracellular matter is exosmosed, solidify its protein, thus blocking-up bacterial reproduction or directly it is killed.This disinfectant can be killed various common noxious bacterias at the utmost point in the short time, as 2.62 * 10
9Cfu/ml, 2.62 * 10
8Cfu/ml, 2.62 * 10
7The Escherichia coli suspension of cfu/ml kills 8.45 * 10 getting final product 100% with this disinfectant contact back moment
9Cfu/ml, 8.45 * 10
8Cfu/ml, 8.45 * 10
7The comma bacillus suspension and 7.3 * 10 of cfu/ml
9Cfu/ml, 7.3 * 10
8Cfu/ml, 7.3 * 10
7The typhoid fever bacteria suspension of cfu/ml gets final product 100% with this disinfectant contact back moment and kills.And this disinfectant can be killed hepatitis A virus in moment.
This disinfectant is a kind of environment-friendly type disinfectant, does not damage human body cell, and is nontoxic to human body.
This disinfectant is water insoluble, and it soaked in distilled water 24 hours, and dilation is 9-10% only, and therefore Disinfection Effect is good in water environment.This disinfectant can be used for drinking water disinfection, Zhong Shui (be lower than drinking water standard, be higher than the sewage standard, usually as water for industrial use) sterilization and freshwater aquiculture sterilization, can efficiently kill malignant bacteria and virus in the water, effectively prevents the pathophorous generation of Jie's water.During use, disinfectant can be placed filter, making needs the water of sterilization to flow through this filter, and total number of bacteria is reduced to below 0.001% like this, also sterilization can be placed the water that needs sterilization.This disinfectant also can be used for purifying air, and is placed on canister and heats and be put in fowl, poultry etc. and raise in the house, can effectively kill airborne harmful germ.
Embodiment
Further specify technical scheme of the present invention below in conjunction with embodiment, but these embodiment and unrestricted embodiments of the present invention, those skilled in the art do not violate the scheme of being finished on the spiritual basis of the present invention should be within the scope of the invention.
Embodiment 1
A. add 245g styrene and 45g divinylbenzene in reactor, stirring fully mixes it, adds 3g benzoyl peroxide and 110g paraffin then, is stirred to the complete molten oil phase that is;
B. in another reactor, add 900g water, 9g gelatin and an amount of methylene blue solution, fully stir, make water;
C. water is warming up to 44 ℃, to wherein adding oil phase, stirs, be warmed up to 78 ℃ with 3 ℃/5 minutes speed simultaneously, be incubated 2 hours, oil droplet is warming up to 96 ℃ after solidifying, and be incubated 7 hours, with 70 ℃ water cleaning, dries then, obtains particulate material;
D. use Petroleum ether extraction gained particulate material, discard extract, in the gained solid matter, add the 1100g chloromethyl methyl ether then, expanded 4 hours in room temperature, continuing to divide the anhydrous alchlor of adding 240g under the stirring condition 3 times, be warming up to 40 ℃ then, reacted 7 hours, filter, use methanol wash then, 60 ℃ of following vacuum dryings;
E. in the gained particulate material, add 550g benzene, at room temperature expanded 4 hours, then in 6 hours, at the trimethylamine methanol solution that continues to be added dropwise under the stirring condition 600g 33% weight, be warming up to 30 ℃ then, reaction is 9 hours under this temperature, filters, with the gained particle 50 ℃ of oven dry, soak with saturated aqueous common salt then, regulating pH with hydrochloric acid is 4, and water cleans, clean with an amount of buck again, obtain pelleted substrate;
F. above-mentioned gained carrier 350g being joined in the reactor, add the solution that 600ml is dissolved with 280g iodine and 150g potassium iodide again, is 1.5 * 1.2 * 10 at 100 ℃, pressure
5Stirring reaction is 10 hours under the Pa condition, and be cooled to room temperature and left standstill 10 hours, filtration, rinsing, with the washing of 10% saline solution, water washing 41 ℃ of vacuum dryings, promptly gets the high-efficiency broad spectrum disinfectant then.
This disinfectant outward appearance is diameter 0.8mm carbon black look silver photosphere shape particle, and is water insoluble.With of the filter-sterilized agent of gained carrier as water purifier, sterilization, good purification, the water quality mouthfeel is good.
Embodiment 2
Method as embodiment 1 prepares disinfectant, and difference is: among the step a, and styrene 255g, divinylbenzene 50g, paraffin 105g; Among the step b, water 950g, gelatin 10g; Among the step c, water is warming up to 40 ℃, to wherein adding oil phase, stirs and be warming up to 79 ℃, be incubated 3 hours, oil droplet is warming up to 98 ℃ after solidifying, and is incubated 6.5 hours; In the steps d, chloromethyl methyl ether 1180g expanded 5 hours, and alchlor 270g is warming up to 44 ℃, reacted 6 hours, with methyl alcohol and washing with alcohol; Among the step e, benzene is 600g, expands 6 hours, and 700g trimethylamine methanol solution 37% weight is warming up to 27 ℃, reacts 10 hours; Among the step f, carrier 250g, 650g solution is dissolved with iodine 290g, potassium iodide 170g, 110 ℃ of temperature, pressure 1.8 * 1.2 * 10
5Pa, stirring reaction 9 hours left standstill 7 hours, 44 ℃ of vacuum dryings.
The gained disinfectant is a carbon black look silver photosphere shape particle, and its diameter is 1.0mm.The gained carrier is used for fresh water shrimp supports the pond sterilization, the water quality benign environment influence of not being bullied in the breeding process, shrimp is not fallen ill.
Embodiment 3
Method as embodiment 1 prepares disinfectant, and difference is: among the step a, and styrene 210g, divinylbenzene 35g, paraffin 90g; Among the step b, water 900g, gelatin 4g; Among the step c, water is warming up to 45 ℃, to wherein adding oil phase, stirs and be warming up to 75 ℃, be incubated 5 hours, oil droplet is warming up to 95 ℃ after solidifying, and is incubated 9 hours; In the steps d, chloromethyl methyl ether 900g expanded 6 hours, and alchlor 180g divides 2 addings, is warming up to 35 ℃, reacts 10 hours, uses washing with alcohol; Among the step e, benzene is 700g, expands 2 hours, and 550g trimethylamine methanol solution 42% weight is warming up to 33 ℃, reacts 6 hours; Among the step f, carrier 250g, 500g solution is dissolved with iodine 240g, potassium iodide 100g, 80 ℃ of temperature, pressure 2.5 * 1.2 * 10
5Pa stirred 6 hours, left standstill 50 ℃ of vacuum dryings 13 hours.
The gained disinfectant is a carbon black look silver photosphere shape particle, and its diameter is 2.0mm.The gained carrier is used for coop sterilizing, purifies air, and with fresh air, Jie's air borne virus is lacked institute's raising chicken health.
Embodiment 4
Method as embodiment 1 prepares disinfectant, and difference is: among the step a, and styrene 300g, divinylbenzene 100g, paraffin 150g; Among the step b, water 1300g, gelatin 13g; Among the step c, water is warming up to 42 ℃, to wherein adding oil phase, stirs and be warming up to 80 ℃, be incubated 1 hour, be warming up to 98 ℃ after the oil droplet curing, be incubated 4 hours with 1 ℃/3 minutes speed; In the steps d, chloromethyl methyl ether 1580g expanded 7 hours, and alchlor 270g is warming up to 44 ℃, reacts 4 hours, uses methanol wash; Among the step e, benzene is 800g, expands 5 hours, and 700g trimethylamine methanol solution 40% weight is warming up to 33 ℃, reacts 8 hours; Among the step f, carrier 400g, 650g solution is dissolved with iodine 300g, potassium iodide 200g, 100 ℃ of temperature, pressure 1.5 * 1.2 * 10
5Pa, stirring reaction 11 hours left standstill 7 hours, 44 ℃ of vacuum dryings.
The gained disinfectant is a carbon black look silver photosphere shape particle, and its diameter is 2.1mm.The gained carrier is used for water sterilization.
Claims (10)
1, a kind of high-efficiency broad spectrum disinfectant comprises carrier and absorption iodine and potassium iodide composition thereon, and wherein said carrier is the expanded polystyrene carrier, polydivinylbenezene is arranged as the envelope film on this carrier top layer.
2, a kind of method for preparing the high-efficiency broad spectrum disinfectant is characterized in that, this method may further comprise the steps:
A. after styrene, divinylbenzene mix, add benzoyl peroxide and paraffin, stir, get oil phase;
B. water, gelatin and methylene blue are mixed, obtain water;
C. water is warming up to 40-46 ℃, oil phase is added wherein, stir and be warming up to 75-80 ℃, insulation, oil droplet solidifies 95-98 ℃ of back intensification, and insulation is filtered, and cleans, and oven dry obtains particulate material;
D. with gained particulate material Petroleum ether extraction, discard extract, add chloromethyl methyl ether in solid matter, expand, add alchlor, be warming up to 35-45 ℃, preferred 40 ℃, reaction is filtered, with alcohol washing, vacuum drying;
E. the gained material is added in the benzene, expand, under agitation add the trimethylamine methanol solution, be warming up to 25-35 ℃, preferred 30 ℃, reaction is filtered, and oven dry is soaked with saturated aqueous common salt, and regulating pH with hydrochloric acid is 3-5, washing, and buck cleans, and promptly obtains pelleted substrate;
F. above-mentioned gained carrier is joined in the ethanolic solution that is dissolved with iodine and potassium iodide, stirring reaction leaves standstill after being cooled to room temperature, filter, and the washing of 10% saline solution, water washing, vacuum drying promptly gets the high-efficiency broad spectrum disinfectant.
3, the preparation method of high-efficiency broad spectrum disinfectant as claimed in claim 2 is characterized in that, among the step a, weight proportion is: styrene 230-260 part, divinylbenzene 42-52 part, benzoyl peroxide 3-4 part, paraffin 100-120 part.
4, the preparation method of high-efficiency broad spectrum disinfectant as claimed in claim 2 is characterized in that, among the step b, weight proportion is: water 800-1000 part, gelatin 8-10 part.
5, the preparation method of high-efficiency broad spectrum disinfectant as claimed in claim 2 is characterized in that, among the step c, is incubated 1-3 hour, preferred 2 hours for the first time; For the second time be incubated 6-8 hour; Insulation is for the second time cleaned with 60-80 ℃ of water.
6, the preparation method of high-efficiency broad spectrum disinfectant as claimed in claim 2 is characterized in that, in the steps d, described chloromethyl methyl ether weight is 1000-1200 part; Described expansion 3-5 hour; Described anhydrous alchlor weight is 210-270 part, and its gradation adds, and preferably divides 3 addings; Described reaction 6-8 hour; Described alcohol is that methyl alcohol is or/and ethanol; Described vacuum drying is 60-65 ℃ of following vacuum drying.
7, the preparation method of high-efficiency broad spectrum disinfectant as claimed in claim 2 is characterized in that, among the step e, described benzene weight is 500-600 part; Described expansion 3-5 hour; The methanol solution weight percent concentration of described trimethylamine is 30-40%, and is preferred 33%, and the preferred 600-650 weight portion of its consumption constantly stirs down in 5-7 hour it is added reaction system; The preferred 9-10 of described reaction hour; Described oven dry is 45-55 ℃ of oven dry.
8, the preparation method of high-efficiency broad spectrum disinfectant as claimed in claim 2 is characterized in that, among the step f, and described carrier, weight is 300-400 part; Described ethanolic solution is dissolved with iodine 250-280 weight portion, is dissolved with potassium iodide 130-160 weight portion; Described stirring reaction, condition are temperature 90-120 ℃, pressure 1.0 * 1.2 * 10
5Pa-2.0 * 1.2 * 10
5Pa, preferred 1.5 * 1.2 * 10
5Pa, reaction time 8-12 hour, preferred 10 hours; Described leaving standstill, the time is 8-12 hour, preferred 10 hours; Described vacuum drying, vacuum drying during for 40-45 ℃.
9, high-efficiency broad spectrum disinfectant as claimed in claim 8 is used for water environment sterilization or air cleaning.
10, high-efficiency broad spectrum disinfectant as claimed in claim 9 is used for the water environment sterilization, it is characterized in that described water environment is drinking water, middle water or freshwater aquiculture pond.
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|---|---|---|---|
| CN 200410042803 CN1703958A (en) | 2004-05-26 | 2004-05-26 | Highly efficient broad spectrum disinfectant, its preparation method and application |
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| CN 200410042803 CN1703958A (en) | 2004-05-26 | 2004-05-26 | Highly efficient broad spectrum disinfectant, its preparation method and application |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104542704A (en) * | 2015-01-08 | 2015-04-29 | 河南黑马动物药业有限公司 | Controlled-release iodine disinfection tablet |
| CN106035390A (en) * | 2016-06-15 | 2016-10-26 | 寻航 | Disinfectant for radiotherapy department |
| CN107788013A (en) * | 2017-11-17 | 2018-03-13 | 侯英 | Drink water purifying disinfectant and preparation method thereof |
| CN114533929A (en) * | 2022-02-15 | 2022-05-27 | 右行健康生物科技(广州)有限公司 | Borneol and preparation process thereof |
-
2004
- 2004-05-26 CN CN 200410042803 patent/CN1703958A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104542704A (en) * | 2015-01-08 | 2015-04-29 | 河南黑马动物药业有限公司 | Controlled-release iodine disinfection tablet |
| CN104542704B (en) * | 2015-01-08 | 2017-10-03 | 河南黑马动物药业有限公司 | A kind of long-acting iodine disinfection tablet |
| CN106035390A (en) * | 2016-06-15 | 2016-10-26 | 寻航 | Disinfectant for radiotherapy department |
| CN107788013A (en) * | 2017-11-17 | 2018-03-13 | 侯英 | Drink water purifying disinfectant and preparation method thereof |
| CN114533929A (en) * | 2022-02-15 | 2022-05-27 | 右行健康生物科技(广州)有限公司 | Borneol and preparation process thereof |
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