CN101403194B - Preparation method for slow-releasing mosquito-killing finishing agent - Google Patents
Preparation method for slow-releasing mosquito-killing finishing agent Download PDFInfo
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- CN101403194B CN101403194B CN2008102009556A CN200810200955A CN101403194B CN 101403194 B CN101403194 B CN 101403194B CN 2008102009556 A CN2008102009556 A CN 2008102009556A CN 200810200955 A CN200810200955 A CN 200810200955A CN 101403194 B CN101403194 B CN 101403194B
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Abstract
The invention relates to a preparation method of a slow-releasing mosquito repelling and killing finishing agent, which comprises the steps: (1) a mosquito repelling and killing chemical is dissolved in an organic solvent according to the weight ratio of 1 to 1; an oil-soluble reactive monomer and an emulsifier are added to form an oil phase; 100ml of distilled water is measured, and a water-soluble reactive monomer PEG is added into the distilled water to form a water phase; the oil and the water are mixed and shaken up; (2) the oil-in-water emulsion is transferred into a three-mouth flask and is stirred while being added with a catalyst, namely, dibutyl tin laurate, so as to induce the two monomers to react, the stirring is continued for 2 hours, polymers generated by the monomer reaction cover effective components; and (3) a curing-crosslinking agent is added, and the stirring is continued for 1 hour to obtain the slow-releasing mosquito repelling and killing finishing agent. The preparation method of the slow-releasing mosquito repelling and killing finishing agent of the invention is low in equipment requirement, simple in operation, easy-controllable in condition, lower in cost and convenient in application, and is suitable for large-scale production; and the mosquito repelling and killing textiles finished by the finishing agent is better in washing resistance and durability.
Description
Technical field
The invention belongs to the preparation field of mosquito-killing finishing agent, particularly relate to a kind of preparation method of slow-releasing mosquito-killing finishing agent.
Background technology
Mosquito not only bites people and animals, also can propagate a lot of diseases, as malaria, dengue fever, filariasis, encephalitis B etc., serious harm health.The media mosquito control is the important measures of this class disease popularity of control, and for the disease of still not having effective vaccine (as dengue fever) and disease (as malaria) that medicine is developed immunity to drugs, media is controlled at prevention, and it takes place and the importance of popular aspect just seems particularly important.For a long time, people attempt a lot of methods and the media mosquito is struggled, and have obtained significant effect, but have also found many problems.The mosquito control technology is of a great variety, mainly contains physical control, chemical prevention, biological control etc.The action principle of various technology is all different with occupation mode, the activity of killing of different mosquito kinds is also had difference, but limitation is separately all arranged, as easily develop immunity to drugs, onset is slow or be detrimental to health etc. [1].
Along with the development of society, the human living standard improves constantly, and people are to healthy and self-protection pay attention to day by day.The deterioration of living environment in addition makes that the mankind are urgent further to the research and development that improve environmental product, and we have developed the mosquito repellent microcapsules under this background.
Traditional mosquito repellent, kill mosquito product have mosquito-repellent incense, electric mosquito repellent, aerosol mosquitocide, floral water, mosquito-dispelling cream, dimethyl carbate etc., and the said goods all has inevitable shortcoming:
(1) active ingredient is exposed in air, and health is had certain toxic and side effect;
(2) under the situation of circulation of air, the effect of kill mosquito or mosquito repellent is very weak;
(3) the aerosol microparticle is suspended in the air environment is polluted;
Microcapsules technology just was applied on the no carbon required by the American as far back as the 1950's, had from then on started the New Times of microcapsules technology.Microcapsules technology is as a kind of method of field of textiles processing and sorting, and is very general in Japan, America and Europe, and the product that utilizes microcapsules technology to produce has promoted textile to be developed to directions such as high added value, superior, diversity.This microcapsules safety, toxic and side effect are little, and have avoidance effect efficient, long-acting, broad-spectrum, and people, animal are not had any harm, and also pollution-free to environment.
Summary of the invention
Technical problem to be solved by this invention provides a kind of preparation method of slow-releasing mosquito-killing finishing agent, and this method equipment needed thereby is simple, and cost is low, and is easy to operate, is fit to suitability for industrialized production.
The preparation method of a kind of slow-releasing mosquito-killing finishing agent of the present invention comprises:
(1) preparation of O/w emulsion
To kill the mosquito chemicals and be dissolved in organic solvent at 1: 1 by mass ratio; Add the oil soluble reaction monomer, emulsifying agent 2201 forms oil phase; Measure 100mL distilled water, and, form water to wherein adding water-soluble reaction monomer polyethylene glycol (PEG); The profit two-phase is mixed, shake up;
(2) coat
O/w emulsion is changed in the there-necked flask, add catalyst dibutyl tin dilaurate 0.02% while stirring, to bring out two kinds of monomer reactions, continue to stir 2h, the polymer that monomer reaction generates coats active ingredient;
(3) solidify
Add cure-crosslinking agent, continue to stir 1h, promptly get slow-releasing mosquito-killing finishing agent.
It is decis that described step (1) is killed the mosquito chemicals, effective cypermethrin, Permethrin, ammonia chrysanthemum ester, allethrin, propine chrysanthemum ester or methothrin.
Described step (1) organic solvent is carrene or ethyl acetate.
Described step (1) oil soluble reaction monomer be 2,4 toluene di-isocyanate(TDI)s, 2,6 toluene di-isocyanate(TDI)s, diphenyl methane-4,4 '-vulcabond, triphenyl methane-4,4 ' 4 " a kind of in the triisocyanate.
Described step (1) oil soluble reaction monomer is 1 with the mass ratio of killing the mosquito chemicals: 1-1.5.
Emulsifying agent is 2201 type emulsifying agents (Hai'an, Jiangsu petrochemical plant commodity, non-ionic surface active agent and anion surfactant compounds) in the described step (1).
Described step (1) emulsifying agent consumption be kill the mosquito chemicals 4-5 doubly.
Described step (1) monomer polyethylene glycol PEG molecular weight is 400, its consumption be kill the mosquito chemicals 3-3.5 doubly.
Described step (3) cure-crosslinking agent is ethylenediamine or benzenediol.
The present invention adopts interfacial polymerization to prepare finishing agent and can be used as microcapsule suspensions, and it is significantly spherical that the gained microcapsule granule becomes, and the smooth surface densification does not have adhesion each other, and particle is little, and particle diameter is evenly distributed; The microcapsule suspensions good stability is placed and fortnight is not had apparent coagulation; Use simple and convenient.
Interfacial polymerization prepares microcapsule suspensions, and it is low, simple to operate to have an equipment requirement, and condition is controlled easily, and cost is lower and use advantages such as convenient, therefore, is suitable for carrying out large-scale production.In addition, the mosquito microcapsule product of killing of the present invention, with macromolecular material as the wall material, with the active ingredient parcel wherein, make the active ingredient constant speed volatilization kill mosquito slowly discharge, reach the effect of long-time expelling mosquito, with this finishing agent put in order kill mosquito textile washability, durability is better, can kill the mosquito effect and reach 6 months through 10 washings.
Beneficial effect
(1) the finishing agent microcapsule granule of the present invention's preparation becomes significantly spherical, and particle diameter is evenly distributed and the microcapsule suspensions good stability is used simple and convenient;
(2) finishing agent of the present invention's preparation can with the active ingredient parcel wherein, make the active ingredient constant speed volatilization of killing mosquito slowly discharge with macromolecular material as the wall material, reaches the effect of long-time expelling mosquito.
The specific embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment only to be used to the present invention is described and be not used in and limit the scope of the invention.Should be understood that in addition those skilled in the art can make various changes or modifications the present invention after the content of having read the present invention's instruction, these equivalent form of values fall within the application's appended claims institute restricted portion equally.
Embodiment 1
Get the 1.5g decis and be dissolved in the 1.5g carrene, after the dissolving, add 2.0gTDI and 7.0g emulsifying agent 2201 and obtain oil phase fully; Getting 4.5gPEG400 is dissolved in the 100mL distilled water and obtains water; The profit two-phase is mixed, stir, obtain the general O/w emulsion that obvious blue light is arranged; Emulsion is changed in the there-necked flask, add 0.02%, two kind of monomer of catalyst dibutyl tin dilaurate while stirring and react the generation performed polymer with oil phase coating formation microcapsules at oil-water interfaces; Behind the reaction 2h, add the cure-crosslinking agent ethylenediamine, reaction 1h promptly gets microcapsule suspensions.With the content of decis in the extraction-spectrophotometry raffinate, and then to calculate the microcapsules clad ratio be 71.2%.
Embodiment 2
Get 1.5g ammonia chrysanthemum ester and be dissolved in the 1.5g ethyl acetate, add 2.2gTDI and 7.5g emulsifying agent 2201 and obtain oil phase; Get in the 100mL distilled water as water; The profit two-phase is mixed, stir, obtain the general O/w emulsion that obvious blue light is arranged.Emulsion is changed in the there-necked flask, add 4.5gPEG400,0.02%, two kind of monomer of catalyst dibutyl tin dilaurate while stirring and react at oil-water interfaces and generate performed polymer and oil phase is coated form microcapsules; Behind the reaction 2h, add the cure-crosslinking agent ethylenediamine, reaction 1h promptly gets microcapsule suspensions.With the content of decis in the extraction-spectrophotometry raffinate, and then to calculate the microcapsules clad ratio be 67.9%.
Embodiment 3
Get the 2g Permethrin and be dissolved in the 2g carrene, dissolving back adding oiliness reaction monomers TDI, adding 2gTDI and 9.0g emulsifying agent 2201 obtain oil phase fully; Getting 6.0g PEG400 is dissolved in the 100mL distilled water and obtains water; The profit two-phase is mixed, stir, obtain the general O/w emulsion that obvious blue light is arranged; Emulsion is changed in the there-necked flask, add a small amount of 0.02% catalyst dibutyl tin dilaurate while stirring, two kinds of monomers react at oil-water interfaces and generate performed polymer with oil phase coating formation microcapsules; Behind the reaction 2h, add the cure-crosslinking agent benzenediol, reaction 1h promptly gets microcapsule suspensions.With the content of decis in the extraction-spectrophotometry raffinate, and then to calculate the microcapsules clad ratio be 65.4%.
Claims (8)
1. the preparation method of a slow-releasing mosquito-killing finishing agent comprises:
(1) preparation of O/w emulsion
To kill the mosquito chemicals and be dissolved in organic solvent at 1: 1 by mass ratio; Add the oil soluble reaction monomer, emulsifying agent forms oil phase; Measure 100mL distilled water, and, form water to wherein adding water-soluble reaction monomer polyethylene glycol PEG; The profit two-phase is mixed, shake up; Described oil soluble reaction monomer be 2,4 toluene di-isocyanate(TDI)s, 2,6 toluene di-isocyanate(TDI)s, diphenyl methane-4,4 '-vulcabond, triphenyl methane-4,4 ' 4 " a kind of in the triisocyanate;
(2) coat
O/w emulsion is changed in the there-necked flask, add catalyst dibutyl tin dilaurate 0.02% while stirring, to bring out two kinds of monomer reactions, continue to stir 2h, the polymer that monomer reaction generates coats active ingredient;
(3) solidify
Add cure-crosslinking agent, continue to stir 1h, promptly get slow-releasing mosquito-killing finishing agent.
2. the preparation method of a kind of slow-releasing mosquito-killing finishing agent according to claim 1, it is characterized in that: the mosquito chemicals of killing in the described step (1) is a decis, effective cypermethrin, Permethrin, ammonia chrysanthemum ester, allethrin, propine chrysanthemum ester or methothrin.
3. the preparation method of a kind of slow-releasing mosquito-killing finishing agent according to claim 1, it is characterized in that: the organic solvent in the described step (1) is carrene or ethyl acetate.
4. the preparation method of a kind of slow-releasing mosquito-killing finishing agent according to claim 1 is characterized in that: the oil soluble reaction monomer in the described step (1) is 1 with the mass ratio of killing the mosquito chemicals: 1-1.5.
5. the preparation method of a kind of slow-releasing mosquito-killing finishing agent according to claim 1, it is characterized in that: the emulsifying agent in the described step (1) is non-ionic surface active agent and anion surfactant compound.
6. the preparation method of a kind of slow-releasing mosquito-killing finishing agent according to claim 1 is characterized in that: the emulsifying agent consumption in the described step (1) be kill the mosquito chemicals 4-5 doubly.
7. the preparation method of a kind of slow-releasing mosquito-killing finishing agent according to claim 1, it is characterized in that: the monomer polyethylene glycol PEG molecular weight in the described step (1) is 400, its consumption be kill the mosquito chemicals 3-3.5 doubly.
8. the preparation method of a kind of slow-releasing mosquito-killing finishing agent according to claim 1, it is characterized in that: the cure-crosslinking agent in the described step (3) is ethylenediamine or benzenediol.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN2008102009556A CN101403194B (en) | 2008-10-09 | 2008-10-09 | Preparation method for slow-releasing mosquito-killing finishing agent |
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| CN2008102009556A CN101403194B (en) | 2008-10-09 | 2008-10-09 | Preparation method for slow-releasing mosquito-killing finishing agent |
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| CN101403194A CN101403194A (en) | 2009-04-08 |
| CN101403194B true CN101403194B (en) | 2010-11-17 |
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Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102051819A (en) * | 2010-11-19 | 2011-05-11 | 志向（中国）集团有限公司 | Method for producing mosquito prevention textile fabric |
| SG11201911634WA (en) * | 2017-06-12 | 2020-01-30 | Cypress Bio Tech Company Ltd | Multi-application insect repellent additive |
| CN113016792A (en) * | 2021-03-24 | 2021-06-25 | 文水县是大高分子材料有限公司 | Polyurethane pesticide microcapsule suspending agent and preparation method thereof |
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