CN105165846A - BBIT water emulsion and preparation method thereof - Google Patents
BBIT water emulsion and preparation method thereof Download PDFInfo
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- CN105165846A CN105165846A CN201510594745.XA CN201510594745A CN105165846A CN 105165846 A CN105165846 A CN 105165846A CN 201510594745 A CN201510594745 A CN 201510594745A CN 105165846 A CN105165846 A CN 105165846A
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Abstract
The invention discloses a BBIT water emulsion which comprises the following components in parts by weight: 10-40 percent of BBIT, 1-10 percent of an emulsion, 0.1-3 percent of a thickening agent, 1-5 percent of an anti-freezing agent and the balance of deionized water. The invention further discloses a preparation method of the BBIT water emulsion. The preparation method comprises the following steps: (1) adding the emulsion into the BBIT raw medicine to form an oil phase; (2) adding the thickening agent and a proper amount of deionized water to form a water phase; (3) adding the prepared oil phase into the water phase, and carrying out high-speed shearing emulsification to form stable O/W emulsion; (4) respectively adding the anti-freezing agent, adding the deionized water to 100ml, and uniformly stirring. The BBIT water emulsion prepared by the method is low in manufacturing cost, low in toxicity, unlikely to combust and high in environment compatibility.
Description
Technical field
The invention belongs to function Field of Fine Chemicals, specifically, is about a kind of BBIT aqueous emulsion and preparation method thereof.
Background technology
2-butyl-BIT (BBIT), its molecular structure is:
The sterling of BBIT is light yellow transparent liquid, boiling point is 170 ~ 175 DEG C, relative density 1.15 ~ 1.18, solvability (20 DEG C)≤1mg/L in water, heat endurance is greater than 300 DEG C, pH1 ~ pH13 hydrolysis-stable, has good UV resistant performance, can effectively killing fungus, bacterium, saccharomycete and part algae, use mainly as industrial bactericide at present.
At present in domestic and international selling market, BBIT preparation is mainly using a large amount of alcohols solvent as matrix, and this kind of organic solvent is inflammable and explosive, serious environment pollution, affects the VOC content of product simultaneously, also wastes a large amount of non-renewable resources.In recent years along with the increasingly stringent of environmental requirement, national requirements development environment friendly novel form, industrial bactericide formulation development to water baseization, ultramicronising, without dust and controlled release aspect development.Wherein water baseization is exactly one of Main way of industrial bactericide development.
Summary of the invention
The object of the present invention is to provide a kind of BBIT preparation using no or little organic solvent, Environmental Safety, provide its preparation method simultaneously.
For achieving the above object, the present invention is by the following technical solutions:
A kind of BBIT aqueous emulsion, comprises the formula of following mass percent:
Further, according to actual needs, described BBIT aqueous emulsion also comprises bleeding agent and/or defoamer.
According to the present invention, described emulsifier is dodecyl benzene sulfonate or castor oil/rilanit special and ethylene oxide mixture, castor oil polyoxyethylene base ether, glycerin polyoxyethylene ether fatty ester, aliphatic alcohol polyethenoxy base ether, aliphatic acid polyethenoxy ether phosphoric acid ester, fatty acid and ethylene oxide mixture, polyoxyethylene carboxylate, polyoxyethylene polyoxypropylene block polyether, polyoxyethylene sorbitan fatty acid ester, polyethylene glycol hard fatty acid ester, Castor Oil Phosphate Ester Salt, alkyl polyoxyethylene ether phosphoric acid ester, polyphosphazene polymer phosphoric acid ester/salt, at least one in fatty alcohol-polyoxyethylene ether phosphoric acid ester and salt thereof.
According to the present invention, described thickener is at least one in xanthans or cellulose ether and derivative thereof, polyvinyl alcohol, aluminium-magnesium silicate, gelatin, gum Arabic, bentonite, dextrin, polyvinylpyrrolidone PVP, white carbon.
Preferably, described thickener is at least one in xanthans or cellulose ether and derivative thereof.
According to the present invention, described antifreeze is at least one in ethylene glycol or propane diols, glycerine, polyethylene glycol, isopropyl alcohol, urea.
Preferably, described antifreeze is propane diols.
According to the present invention, described bleeding agent is at least one in organosilicon or aerosol-OT salt, fatty alcohol polyoxyalkyl ether, fatty alcohol-polyoxyethylene ether, fatty alcohol and ethylene oxide mixture, and described defoamer is the one in silicone based defoamer or lower alcohol system defoamer.
A preparation method for BBIT aqueous emulsion described in above-mentioned any one, the method is carried out according to the following steps:
(1) in the BBIT of 10g ~ 40g, add the emulsifier of 1g ~ 10g, form oil phase;
(2) thickener of 0.1 ~ 3g is joined in appropriate amount of deionized water, stir and form aqueous phase;
(3) being joined by the oil phase that step (1) prepares in the aqueous phase that step (2) configures and to open high speed shear emulsification, rotating speed is 3000 revs/min, forms stable O/W emulsion;
(4) after opening stirring, then add the antifreeze of 1 ~ 5g, add deionized water to 100ml, stir, be i.e. obtained BBIT aqueous emulsion.
According to the present invention, also can add defoamer in step (2), in step (4), add bleeding agent.
BBIT aqueous emulsion of the present invention and preparation method thereof, its beneficial effect is: the advantages such as its low cost of manufacture, toxicity are low, nonflammable, environmentally safe, are embodied in the following aspects:
(1) aqueous emulsion of the present invention hardly with an organic solvent, greatly reduces the VOC of product;
(2) without flash-point problem, do not burn and do not explode, produce storage and use safety;
(3) environmental pollution is little, to process operation and Environmental security;
(4) take water as matrix, aboundresources, safety when manufacturing and use, packaging, storage and convenient transportation, expense is low, thus reduces production cost;
(5) mildew-resistant better effects if after bleeding agent is added;
(6) the present invention is high speed homogenizing after oil phase mixes with the aqueous phase that emulsifier, thickener, stabilizing agent, antifreeze etc. form with BBIT, and be finally deployed into BBIT aqueous emulsion, the method technique is simple, is beneficial to suitability for industrialized production.
Embodiment
Below in conjunction with specific embodiment, BBIT aqueous emulsion of the present invention is described in further detail.Should be understood that following examples only for illustration of the present invention but not for limiting scope of the present invention.
The concentration used in following examples, as not dated especially, is mass percent concentration.
Embodiment 1:10%BBIT aqueous emulsion
The formula of the 10%BBIT aqueous emulsion of the present embodiment is in table 1.
The formula of table 110%BBIT aqueous emulsion
The preparation method of 10%BBIT aqueous emulsion: (1) adds the former medicine of BBIT, polyoxyethylene carboxylate, polyphosphazene polymer phosphoric acid ester/salt and glycerin polyoxyethylene ether fatty ester, forms oil phase; (2) add cellulose ether, aluminium-magnesium silicate, white carbon and appropriate amount of deionized water, form aqueous phase; (3) being joined by the oil phase of step (1) in the aqueous phase of step (2) and to open high speed shear emulsification, shear rate controls at 3000 revs/min; (4) add ethylene glycol, then add deionized water to 100ml, stir, mixing time 100 minutes.
Embodiment 2:15%BBIT aqueous emulsion
The formula of the 15%BBIT aqueous emulsion of the present embodiment is in table 2.
The formula of table 215%BBIT aqueous emulsion
The preparation method of 15%BBIT aqueous emulsion: (1) adds the former medicine of BBIT and dodecyl benzene sulfonate, forms oil phase; (2) add xanthans, lower alcohol and appropriate amount of deionized water, form aqueous phase; (3) being joined by the oil phase of step (1) in the aqueous phase of step (2) and to open high speed shear emulsification, shear rate controls at 3000 revs/min; (4) add isopropyl alcohol, then add deionized water to 100ml, stir, mixing time 100 minutes.
Embodiment 3:20%BBIT aqueous emulsion
The formula of the 20%BBIT aqueous emulsion of the present embodiment is in table 3.
The formula of table 320%BBIT aqueous emulsion
The preparation method of 20%BBIT aqueous emulsion: (1) adds the former medicine of BBIT, alkyl polyoxyethylene ether phosphoric acid ester, Castor Oil Phosphate Ester Salt, polyoxyethylene polyoxypropylene block polyether formation oil phase; (2) add xanthans and appropriate amount of deionized water, form aqueous phase; (3) being joined by the oil phase of step (1) in the aqueous phase of step (2) and to open high speed shear emulsification, shear rate controls at 3000 revs/min; (4) add propane diols and penetrating agent JFC, then add deionized water to 100ml, stir, mixing time 100 minutes.
Embodiment 4:30%BBIT aqueous emulsion
The formula of the 30%BBIT aqueous emulsion of the present embodiment is in table 4.
The formula of table 430%BBIT aqueous emulsion
The preparation method of 30%BBIT aqueous emulsion: (1) adds the former medicine of BBIT, fatty acid and ethylene oxide mixture, polyethylene glycol hard fatty acid ester, castor oil/rilanit special and ethylene oxide mixture and forms oil phase; (2) add gelatin, gum Arabic, silicone defoaming agent and appropriate amount of deionized water, form aqueous phase; (3) being joined by the oil phase of step (1) in the aqueous phase of step (2) and to open high speed shear emulsification, shear rate controls at 3000 revs/min; (4) add glycerine, bleeding agent OE-35, isopropyl alcohol, then add deionized water to 100ml, stir, mixing time 100 minutes.
Embodiment 5:35%BBIT aqueous emulsion
The Formulations Formula of the 35%BBIT aqueous emulsion of the present embodiment is in table 5.
The Formulations Formula of table 535%BBIT aqueous emulsion
The preparation method of 35%BBIT aqueous emulsion: (1) adds the former medicine of BBIT, castor oil polyoxyethylene base ether, fatty alcohol-polyoxyethylene ether phosphoric acid ester and salt thereof and forms oil phase; (2) add bentonite, dextrin, polyvinylpyrrolidone PVP and silicone defoaming agent and appropriate amount of deionized water, form aqueous phase; (3) being joined by the oil phase of step (1) in the aqueous phase of step (2) and to open high speed shear emulsification, shear rate controls at 3000 revs/min; (4) add urea, polyethylene glycol, propane diols, aerosol-OT salt and fatty alcohol polyoxyalkyl ether, then add deionized water to 100ml, stir, mixing time 100 minutes.
Embodiment 6:40%BBIT aqueous emulsion
The formula of the 40%BBIT aqueous emulsion of the present embodiment is in table 6.
The formula of table 640%BBIT aqueous emulsion
The preparation method of 40%BBIT aqueous emulsion: (1) adds the former medicine of BBIT, aliphatic acid polyethenoxy ether phosphoric acid ester, aliphatic alcohol polyethenoxy base ether, polyoxyethylene sorbitan fatty acid ester, forms oil phase; (2) add cellulose ether and derivative, polyvinyl alcohol, aluminium-magnesium silicate, lower alcohol defoamer and appropriate amount of deionized water, form aqueous phase; (3) being joined by the oil phase of step (1) in the aqueous phase of step (2) and to open high speed shear emulsification, shear rate controls at 3000 revs/min; (4) add glycerine, polyethylene glycol, aerosol-OT salt, fatty alcohol polyoxyalkyl ether, fatty alcohol and ethylene oxide mixture, then add deionized water to 100ml, stir, mixing time 100 minutes.
The product performance index of above six embodiments is in table 7:
The conventional performance index of table 7BBIT aqueous emulsion
Embodiment 7 thermal storage stability is tested
BBIT aqueous emulsion is stored 14d in (54 ± 2) DEG C insulating box, and before and after storage, use the content of efficient liquid phase chromatographic analysis active ingredient respectively, analytical error is ± 1%, the results are shown in Table 8.Visible BBIT aqueous emulsion thermal storage stability is good.
Table 8BBIT aqueous emulsion thermal storage stability result
Embodiment 8 antimold activity measures
The present embodiment for experimental subjects, tests the minimum inhibitory concentration of 10%BBIT, 20%BBIT, 30%BBIT aqueous emulsion and 10%BBIT, 20%BBIT, 30%BBIT solvent-borne type (commercially available) with aspergillus niger, paecilomyces varioti, penicillium funiculosum, Escherichia coli, staphylococcus aureus etc. respectively.
Test method is as follows:
1, the preparation of variable concentrations sample:
Accurately measure 10%BBIT, 20%BBIT, 30%BBIT aqueous emulsion and 10%BBIT, 20%BBIT, 30%BBIT solvent-borne type, adopting methyl alcohol to be mixed with volumetric concentration as solvent is respectively 0.5% (10%BBIT, 20%BBIT, 30%BBIT aqueous emulsion), 0.5% (solvent-borne type 10%BBIT, 20%BBIT, 30%BBIT), and then dilute successively with methyl alcohol using them as starting soln, thus obtain the sample solution of a series of variable concentrations.
The making of the agar plate 2, containing variable concentrations sample:
First draw 1 ml sample solution, be placed in the culture dish of having sterilized, then the medium of about 50 DEG C is cooled to after adding 19mL sterilization, medium and sample solution are fully mixed, leave standstill cooling (period methyl alcohol volatilization totally), simultaneously not contain the medium of sample solution as blank.
3, the inoculation of bacterium is tested:
Containing the fungi flat board of variable concentrations sample connecting fungi test bacterium, putting into 28 DEG C of incubators and cultivating after 4 ~ 5 days, taking out and observe.
Containing the Bacterial Plate of variable concentrations sample connecting bacterium test bacterium, putting into 37 DEG C of incubators and cultivating after 2 ~ 3 days, taking out and observe.
4, the determination of minimum inhibitory concentration:
The test bacterium observed on the flat board of some sample concentrations does not grow, and the test bacterium energy normal growth on the flat board of adjacent low concentration sample, then this concentration is the minimum inhibitory concentration of this sample to this test bacterium.10%BBIT, 20%BBIT, 30%BBIT aqueous emulsion and the minimum inhibitory concentration (MIC) of 10%BBIT, 20%BBIT, 30%BBIT solvent-borne type to experimental bacteria as shown in table 8.
Table 9 minimum inhibitory concentration (MIC)
Note: above bacterial strain is experimental strain.
As shown in Table 9,10%BBIT, 20%BBIT, 30%BBIT aqueous emulsion is substantially consistent to the minimum inhibitory concentration of above-mentioned test strain with 10%BBIT, 20%BBIT, 30%BBIT solvent-borne type respectively.
Claims (10)
1. a BBIT aqueous emulsion, is characterized in that, comprises the formula of following mass percent:
2. BBIT aqueous emulsion as claimed in claim 1, it is characterized in that, described BBIT aqueous emulsion also comprises bleeding agent or defoamer.
3. BBIT aqueous emulsion as claimed in claim 1, it is characterized in that, described emulsifier is dodecyl benzene sulfonate or castor oil/rilanit special and ethylene oxide mixture, castor oil polyoxyethylene base ether, glycerin polyoxyethylene ether fatty ester, aliphatic alcohol polyethenoxy base ether, aliphatic acid polyethenoxy ether phosphoric acid ester, fatty acid and ethylene oxide mixture, polyoxyethylene carboxylate, polyoxyethylene polyoxypropylene block polyether, polyoxyethylene sorbitan fatty acid ester, polyethylene glycol hard fatty acid ester, Castor Oil Phosphate Ester Salt, alkyl polyoxyethylene ether phosphoric acid ester, polyphosphazene polymer phosphoric acid ester/salt, at least one in fatty alcohol-polyoxyethylene ether phosphoric acid ester and salt thereof.
4. BBIT aqueous emulsion as claimed in claim 1, it is characterized in that, described thickener is at least one in xanthans or cellulose ether and derivative thereof, polyvinyl alcohol, aluminium-magnesium silicate, gelatin, gum Arabic, bentonite, dextrin, polyvinylpyrrolidone PVP, white carbon.
5. BBIT aqueous emulsion as claimed in claim 4, is characterized in that, described thickener is at least one in xanthans or cellulose ether and derivative thereof.
6. BBIT aqueous emulsion according to claim 1, is characterized in that, described antifreeze is at least one in ethylene glycol or propane diols, glycerine, polyethylene glycol, isopropyl alcohol, urea.
7. BBIT aqueous emulsion as claimed in claim 6, it is characterized in that, described antifreeze is propane diols.
8. BBIT aqueous emulsion as claimed in claim 2, it is characterized in that, described bleeding agent is at least one in organosilicon or aerosol-OT salt, fatty alcohol polyoxyalkyl ether, fatty alcohol-polyoxyethylene ether, fatty alcohol and ethylene oxide mixture, and described defoamer is the one in silicone based defoamer or lower alcohol system defoamer.
9. a preparation method for the BBIT aqueous emulsion as described in any one of claim 1-8, is characterized in that, the method is carried out according to the following steps:
(1) in the BBIT of 10g ~ 40g, add the emulsifier of 1g ~ 10g, form oil phase;
(2) thickener of 0.1 ~ 3g is joined in appropriate amount of deionized water, stir and form aqueous phase;
(3) oil phase that step (1) prepares to be joined in the aqueous phase that step (2) configures and to open high speed shear emulsification, forming stable O/W emulsion;
(4) after opening stirring, then add the antifreeze of 1 ~ 5g, add deionized water to 100ml, stir, be i.e. obtained BBIT aqueous emulsion.
10. the preparation method of BBIT aqueous emulsion as claimed in claim 9, is characterized in that, in step (2), add defoamer, in step (4), add bleeding agent.
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CN110280051A (en) * | 2019-07-09 | 2019-09-27 | 四川省蜀爱新材料有限公司 | A kind of low silicon defoaming agent |
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