CN101638537A - Antibacterial emulsion paint and manufacture method thereof - Google Patents
Antibacterial emulsion paint and manufacture method thereof Download PDFInfo
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- CN101638537A CN101638537A CN200910146839A CN200910146839A CN101638537A CN 101638537 A CN101638537 A CN 101638537A CN 200910146839 A CN200910146839 A CN 200910146839A CN 200910146839 A CN200910146839 A CN 200910146839A CN 101638537 A CN101638537 A CN 101638537A
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Abstract
The invention discloses an antibacterial emulsion paint and a manufacture method thereof. The method comprises the following steps: (1) pre-emulsifying process: adding 80% of total quantity of water,all emulsifier, part mixed monomer and all ammonia, and then heating and stirring at high speed and emulsifying to obtain a pre-emulsified mixed monomer solution, heating to the temperature of 80 DEGC, stirring at lower speed, dripping 20% of total quantity of an initiator; (2) emulsifying process: after pre-emulsifying for 1.5 h, simultaneously dripping the rest of mixed monomer and the initiator solution, keeping the temperature at 81-83 DEG C, after adjusting the pH of the ammonia to 7-8, discharging; (3) processing nano particles: adding a certain quantity of nano powder in proper amountof water to carry out an ultrasonic dispersion to obtain a suspension solution of the nano powder; (4) preparing slurry: adding a dispersant in the prepared suspension solution of the nano powder to stir uniformly for 5-8 min to obtain the slurry; (5) mixing paint: using a slow disperser, sequentially and slowly adding an emulsion solution in the slurry and dispersing with low speed. After dispersing for 10-12 min, the antibacterial emulsion paint is obtained. The antibacterial emulsion paint made by the invention has advantages of low temperature of forming films, low content of formaldehyde,good cost performance and better application prospect.
Description
Technical field
The present invention relates to building material field, particularly a kind of antibiotic emulsion paint and preparation method.
Background technology
The tradition emulsion paint adds sterilant, can prevent going mouldy of emulsion paint, and it can not kill airborne unwanted bacteria, and environment is polluted.Nanoparticle is subjected to extensive concern because of its particular performances, and more than ten years have been obtained develop rapidly recently.Copper nanoparticle has stronger antibiotic, sterilizing function, and it is one of effective inorganic antiseptic.Can consider the inorganic antiseptic copper nanoparticle is added into emulsion paint, prepare emulsion paint with good anti-microbial property.
Summary of the invention
At the deficiencies in the prior art, the object of the present invention is to provide a kind of antibiotic emulsion paint and preparation method.
The antibacterial latex paint formula is as follows:
(1) mix monomer vinylbenzene volume is 53%～58%.
(2) the emulsifying agent Triton X-100 18%～21%.
(3) the initiator potassium persulfate volume is 0.43%～0.47%.
(4) pH buffer reagent ammoniacal liquor, volume are 2%～3%.
(5) the copper nanoparticle volume is 0.025%.
(6) dispersion agent ethanol volume is 0.1%～0.2%.
(7) water: 18%～24%
Optimal proportion is:
(1) mix monomer vinylbenzene volume is 55%.
(2) emulsifying agent Triton X-100 volume is 20%.
(3) the initiator potassium persulfate volume is 0.45%.
(4) pH buffer reagent ammoniacal liquor, volume are 2.5%:
(5) the copper nanoparticle volume is 0.025%.
(6) dispersion agent ethanol volume is 0.15%.
(7) water: 21.5%
Antibiotic emulsion paint is preparation technology comprise:
(1) pre-emulsification technology
Add 80% of water inventory, whole emulsifying agents, partially mixed monomer, and whole ammoniacal liquor.Heat up then, and high-speed stirring emulsification, pre-emulsification mixed monomer solution obtained.When temperature is raised to 80 ℃, turn stirring velocity down, drip 20% of initiator total amount.
(2) emulsifying process
Behind the pre-emulsification 1.5h, drip remaining mix monomer and initiator solution simultaneously, temperature remains on about 81～83 ℃.Regulating pH with ammoniacal liquor then is 7～8 back dischargings.
(3) nanoparticle is handled
In an amount of water, add the certain amount of nano powder, carry out ultra-sonic dispersion, make the suspension of nanometer powder.
(4) preparation slurry
Adding dispersion agent in the nano-powder suspension for preparing stirs and can get slurry behind 5～8min.
(5) paint
Use dispersion machine at a slow speed, in slurry, slowly add emulsion successively, and carry out low speed and disperse.After disperseing 10～12min, can get antibiotic emulsion paint.
The made emulsion paint of the present invention has the advantage that film-forming temperature is low, formaldehyde content is low, and good cost performance has application promise in clinical practice.
Embodiment
Embodiment makes antibiotic emulsion paint with the following methods:
The antibacterial latex paint formula is as follows:
(1) mix monomer vinylbenzene volume is 55%.
Table 1 vinylbenzene volume influences the latex paint emulsion polymeric
| Vinylbenzene (%) | Cohesion rate (%) | Emulsion viscosity (s) | Thickening viscosity |
| ??35 | ??0.69 | ??10.8 | ??15.7 |
| ??45 | ??0.31 | ??11.9 | ??22.8 |
| ??55 | ??0.23 | ??16.4 | ??32.8 |
| ??65 | ??1.42 | ??21.7 | ??72.0 |
| ??75 | Sudden and violent poly- | ??22.9 | Can't measure |
Table 1 is the influence of vinylbenzene consumption to letex polymerization.As shown in Table 1, increase with the vinylbenzene consumption, emulsion viscosity increases, and the cohesion rate reduces.This is because carboxyl is a polar group, and very strong wetting ability is arranged, and the carboxyl major part that is incorporated on the polymer lateral chain covers the latex particle surface, stops between particle to bond mutually, obviously suppresses the generation of gel.In addition, the vinylbenzene consumption is very remarkable to emulsion viscosity influence, particularly when emulsion by ammoniacal liquor in and generate carboxylate salt after, carboxyl is repulsion mutually between the interface region, and makes macromolecular chain become straight configuration by rolled state, and emulsion viscosity is sharply increased.When the vinylbenzene consumption was increased to a certain degree, the cohesion rate increased on the contrary, and this is because a kind of strongly hydrophilic monomer of vinylbenzene, with carboxyl be a kind of hydrophilic radical, the autohemagglutination phenomenon takes place in water; And the increase of vinylbenzene consumption can make the film forming properties variation of filming, and water tolerance descends.Table 1 shows: the optimum consumption of vinylbenzene is 55% of a monomer total amount, and cohesion this moment rate is lower, and emulsion viscosity is moderate.The lip-deep carboxylic acid ion of emulsion particle provides certain cross-linking set for adding the metal-salt linking agent simultaneously.
(2) emulsifying agent Triton X-100 volume is 20%.
Table 2 emulsifying agent consumption is to the influence of letex polymerization
| Emulsifying agent consumption/% | Cohesion rate/% | ??Ca 2+Stability | Dilution stability | Mechanical stability |
| ??16 | ??2.57 | Precipitation is arranged at the bottom | By | Breakdown of emulsion has a small amount of throw out |
| ??20 | ??1.76 | By | By | By |
| ??24 | ??3.15 | By | By | By |
| ??28 | ??3.95 | By | By | By |
| ??32 | ??---- | Precipitation is arranged at the bottom | Precipitation is arranged at the bottom | By |
Table 2 is the influence of emulsifying agent consumption to letex polymerization.Table 2 shows works as the emulsifying agent total amount more after a little while, and the cohesion rate is bigger, and emulsion appearance is relatively poor, this is because emulsification is insufficient, can not cover particle surface, and reaction is unstable, have more coarse particles in the emulsion that generates, and the emulsion residual monomer content is many, causes film-forming properties poor. and when the emulsifying agent consumption is too much, condensation product is also more, at this moment because the micella number that emulsifying agent forms increases, reaction aggravates, and heat of polymerization has little time to leave, can cause sudden and violent gathering, produce more grumeleuse.Table 2 shows that the Calcium ion stability of emulsion is poor when the emulsifying agent consumption is lower than 20%, and this is that promptly electrokinetic potential has reduced because the introducing of calcium ion is dwindled the distance of electrostatic double layer.If ionogen reaches enough big concentration, the electrokinetic potential of emulsion particle equals zero, and mutual expelling force disappears.Phase suction between particulate makes a large amount of cohesions of colloidal particle and sedimentation is separated out.When the emulsifying agent consumption more than or equal to 4% the time, the Calcium ion stability of emulsion is fine, this mainly is the consumption foot of emulsifying agent, so that emulsion-stabilizing is dispersed in the system.So emulsifying agent the optimum mix amount of the present invention is that about 20% of monomer total amount is advisable.
(3) the initiator potassium persulfate volume is 0.45%.
Table 3 initiator amount influences polymeric
| Initiator amount/% | Cohesion rate/% |
| ??0.25 | ??0.83 |
| ??0.35 | ??2.12 |
| ??0.45 | ??0.39 |
| ??0.55 | ??0.78 |
| ??0.65 | Sudden and violent poly- |
Table 3 influences polymeric for initiator amount.The consumption of initiator directly has influence on the stability of reaction and the performance of emulsion.Table 3 shows that the consumption of initiator is less than at 0.45% o'clock, and the polymerization process instability thinks that initiator concentration is low, speed of reaction is little, and monomer conversion is little, and level of residual monomers is big in the emulsion, do not react completely, this makes that also the dried coating film time is long, and the objectionable impurities residual concentration is big; And initiator concentration is low, and the polymer emulsion number of particles of formation is few, and particle diameter is big, and the emulsion instability is so the cohesion rate is bigger.Amount of initiator is 0.65% o'clock, produces poly-ly cruelly, and this is that rate of polymerization is too fast because the free radical that forms is many, and the stability of emulsion reduces, the particle diameter chap.Speed of reaction is fast, and reaction heat has little time to discharge, and has produced sudden and violent poly-ly, and undecomposed initiator remains in the product emulsion, influences the performance of emulsion.Initiator amount when 0.45% left and right sides, stable reaction, the gained emulsion appearance is better, this polymer emulsion population that may be interpreted as formation is many, and polymerization rate is fast, and latex particle size is little, initiator remaining in the emulsion is few, and this is all favourable to polyreaction and emulsion property.The volume that is determined by experiment initiator is 0.45%.
(4) pH buffer reagent ammoniacal liquor, volume are 2.5%.
The Potassium Persulphate initiator carries out in the thermal decomposition process generating hydrogen ion at aqueous phase, so along with the carrying out of emulsion polymerization, the pH value of system descends gradually, can drop to pH in normal conditions is 1～3.The thermolysis of Potassium Persulphate initiator belongs to autocatalytic reaction, and along with the reduction of pH value is carried out in reaction, its rate of decomposition increases.System pH reduction simultaneously makes stability of emulsion descend again, thus constant in order to ensure the pH value of system in reaction process, usually need to add pH buffer reagent ammoniacal liquor.
(5) nano-powder adopts copper nanoparticle, and volume is 0.025%.
As can be seen from Table 4, along with the increase of copper nanoparticle consumption, antibiotic rate improves.The sterilization rate of contact 4h generally a little more than contact 1h, illustrates that the copper nanoparticle antibiotic emulsion paint can continue sterilization within a certain period of time.This is because this metallic copper is cupric ion in the water layer activation of its surface adsorption, cupric ion contacts with bacterium and reacts, when metal copper ion contact microorganism cells film, because of cytolemma has negative charge, metal copper ion is positively charged, the two relies on coulombic force firmly to be attached together, metal ion penetration cell wall enters in the born of the same parents, react with organic thio group, carboxyl, hydroxyl, make protein coagulating, destroy the activity of cell synthetic enzyme, cell is lost the division growth ability and death.Simultaneously, cupric ion also can destroy microorganisms electric transmission system, respiratory system, material transfer system.But along with the increase of copper nanoparticle consumption, cost increases, and is unfavorable for practical application.And as can be seen from Table 4, when the copper consumption was 0.025%, sterilization rate also reached about 92.38%, increased the consumption of copper nanoparticle again, and meaning is not very big, and has increased cost.
Table 4 copper nanoparticle consumption is to antibiotic Effect on Performance
| ??Cu(％) | Contact 1h sterilization rate (%) | Contact 4h sterilization rate (%) |
| ??0 | ??2.00 | ??18.00 |
| ??0.025 | ??87.62 | ??92.38 |
| ??0.05 | ??92.2 | ??93.15 |
| ??0.075 | ??95.23 | ??94.95 |
| ??0.1 | ??95.47 | ??95.63 |
(6) dispersion agent ethanol volume is 0.15%.
For mix monomer vinylbenzene, need to adopt the strong dispersion medium ethanol of polarity, only in this way can guarantee just that monomer and polymkeric substance are distributed in the system with tear drop and particle form respectively, rather than be solution state.
Antibiotic emulsion paint is preparation technology comprise:
(1) pre-emulsification technology
Add 80% of water inventory, whole emulsifying agents, partially mixed monomer, and whole ammoniacal liquor.Heat up then, and high-speed stirring emulsification, pre-emulsification mixed monomer solution obtained.When temperature is raised to 80 ℃, turn stirring velocity down, drip 20% of initiator total amount.
Table 5 is the influence of initiator amount to letex polymerization.Table 5 shows the increase along with initiator amount, and polyreaction stability is improved by bad, and when initiator amount was 20%, pre-emulsion polymerization was the most stable, and the emulsion particle of making is also thinner.But along with initiator amount continues to increase, pre-emulsion polymerization stability decreases, emulsion particle is chap also.Therefore, suitable initiator amount is 20% to be advisable.
Table 5 initiator amount is to the influence of letex polymerization
(2) emulsifying process
Behind the pre-emulsification 1.5h, drip remaining mix monomer and initiator solution simultaneously, temperature remains on about 81～83 ℃.Regulating the pH of mixed value with ammoniacal liquor then is 7～8 back dischargings.
(3) nanoparticle is handled
In an amount of water, add the certain amount of nano powder, carry out ultra-sonic dispersion, make the suspension of nanometer powder.
(4) preparation slurry
In the nano-powder suspension for preparing, add and to get slurry after dispersion agent stirs 5～8min.
(5) paint
Use dispersion machine at a slow speed, in slurry, slowly add emulsion successively, and carry out low speed and disperse.After disperseing 10～12min, can get antibiotic emulsion paint.
The antibiotic emulsion paint formaldehyde content low especially (0.0006g/kg) of the present invention's preparation, well below the requirement (0.10g/kg) of GB GB18582-2001, content of volatile organic compound (113g/L) also requires (200g/L) far below GB; It is a kind of interiro wall latex paint of environment-friendly type.
Claims (3)
1, a kind of antibiotic emulsion paint and preparation method, its feature may further comprise the steps:
(1) pre-emulsification technology
Add 80% of water inventory, whole emulsifying agents, partially mixed monomer, and whole ammoniacal liquor.Heat up then, and high-speed stirring emulsification, pre-emulsification mixed monomer solution obtained.When temperature is raised to 80 ℃, turn stirring velocity down, drip 20% of initiator total amount.
(2) emulsifying process
Behind the pre-emulsification 1.5h, drip remaining mix monomer and initiator solution simultaneously, temperature remains on about 81 ℃～83 ℃.Regulating pH with ammoniacal liquor then is 7～8 back dischargings.
(3) nanoparticle is handled
In an amount of water, add the certain amount of nano powder, carry out ultra-sonic dispersion, make the suspension of nanometer powder.
(4) preparation slurry
Adding dispersion agent in the nano-powder suspension for preparing stirs and can get slurry behind 5～8min.
(5) paint
Use dispersion machine at a slow speed, in slurry, slowly add emulsion successively, and carry out low speed and disperse.After disperseing 10～12min, can get antibiotic emulsion paint.
2, according to described antibiotic emulsion paint of claim 1 and preparation method, it is as follows to it is characterized in that filling a prescription:
(1) mix monomer vinylbenzene volume is 53%～58%.
(2) the emulsifying agent Triton X-100 18%～21%.
(3) the initiator potassium persulfate volume is 0.43%～0.47%.
(4) pH buffer reagent ammoniacal liquor, volume are 2%～3%.
(5) the copper nanoparticle volume is 0.025%.
(6) dispersion agent ethanol volume is 0.1%～0.2%.
(7) water: 18%～24%
3, according to claim 1 or described antibiotic emulsion paint of claim 2 and preparation method, it is characterized in that optimization formula is as follows:
(1) mix monomer vinylbenzene volume is 55%.
(2) emulsifying agent Triton X-100 volume is 20%.
(3) the initiator potassium persulfate volume is 0.45%.
(4) pH buffer reagent ammoniacal liquor volume is 2.5%.
(5) the copper nanoparticle volume is 0.025%.
(6) dispersion agent ethanol volume is 0.15%.
(7) water: 21.5%.
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| CN200910146839A CN101638537A (en) | 2009-06-09 | 2009-06-09 | Antibacterial emulsion paint and manufacture method thereof |
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| CN200910146839A CN101638537A (en) | 2009-06-09 | 2009-06-09 | Antibacterial emulsion paint and manufacture method thereof |
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| CN101638537A true CN101638537A (en) | 2010-02-03 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105111859A (en) * | 2015-08-28 | 2015-12-02 | 中科纳达控股股份有限公司 | Nano antimicrobial internal wall paint containing illite-montmorillonite clay and preparation method thereof |
| US11039620B2 (en) | 2014-02-19 | 2021-06-22 | Corning Incorporated | Antimicrobial glass compositions, glasses and polymeric articles incorporating the same |
| US11039619B2 (en) | 2014-02-19 | 2021-06-22 | Corning Incorporated | Antimicrobial glass compositions, glasses and polymeric articles incorporating the same |
| US11039621B2 (en) | 2014-02-19 | 2021-06-22 | Corning Incorporated | Antimicrobial glass compositions, glasses and polymeric articles incorporating the same |
-
2009
- 2009-06-09 CN CN200910146839A patent/CN101638537A/en active Pending
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US11039620B2 (en) | 2014-02-19 | 2021-06-22 | Corning Incorporated | Antimicrobial glass compositions, glasses and polymeric articles incorporating the same |
| US11039619B2 (en) | 2014-02-19 | 2021-06-22 | Corning Incorporated | Antimicrobial glass compositions, glasses and polymeric articles incorporating the same |
| US11039621B2 (en) | 2014-02-19 | 2021-06-22 | Corning Incorporated | Antimicrobial glass compositions, glasses and polymeric articles incorporating the same |
| US11464232B2 (en) | 2014-02-19 | 2022-10-11 | Corning Incorporated | Antimicrobial glass compositions, glasses and polymeric articles incorporating the same |
| US11470847B2 (en) | 2014-02-19 | 2022-10-18 | Corning Incorporated | Antimicrobial glass compositions, glasses and polymeric articles incorporating the same |
| US11751570B2 (en) | 2014-02-19 | 2023-09-12 | Corning Incorporated | Aluminosilicate glass with phosphorus and potassium |
| CN105111859A (en) * | 2015-08-28 | 2015-12-02 | 中科纳达控股股份有限公司 | Nano antimicrobial internal wall paint containing illite-montmorillonite clay and preparation method thereof |
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Application publication date: 20100203 |