CN103525129A - Preparation method of special-purpose nanometer modifier of water-based coating - Google Patents
Preparation method of special-purpose nanometer modifier of water-based coating Download PDFInfo
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- CN103525129A CN103525129A CN201310028534.0A CN201310028534A CN103525129A CN 103525129 A CN103525129 A CN 103525129A CN 201310028534 A CN201310028534 A CN 201310028534A CN 103525129 A CN103525129 A CN 103525129A
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Abstract
The invention discloses a preparation method of a special-purpose nanometer modifier of water-based coating, which belongs to the fields of chemical engineering and fine chemical engineering, and relates to a preparation method of a nanometer modifier added into water-based coating. The preparation method comprises the following steps of preparing nanometer calcium carbonate powder into a sizing agent with mass fraction of 10%-35%; placing the sizing agent into a constant-temperature water-bath slot for heating; slowly adding the prepared modifying agent of a certain proportion into the sizing agent within 5 minutes under a certain stirring speed after a predetermined temperature is reached. After beings stirred for certain time, the modified serous fluid is filled into a container for sealing and storing after being cooled to the room temperature. The preparation method disclosed by the invention has the beneficial effect that the modifier disclosed by the invention is added into a water-based coating formula system, so that a difficult problem that the nanometer calcium carbonate powder is not easy to disperse and easy to unite in the coating formula is successfully solved and dust pollution is reduced; after replacing titanium dioxide according to a proportion, contrast ratio and covering power of the material are improved, washing resistance is obviously strengthened, and fineness of emulsion paint is high; moreover, storage performance is excellent and sedimentation is not easy.
Description
Technical field
The invention belongs to chemical engineering, field of fine chemical, particularly relate to a kind of for the production of in, add the preparation method of the nano level modification agent in water-borne coatings to.
Background technology
Nano-calcium carbonate refers to and comprises that ultra-fine and particle diameter super fine calcium carbonate is less than the ultrafine powder calcium carbonate of 100nm, has the distinctive surface effects of nanoparticle, volume effect, macro quanta tunnel effect.Its specific surface area is very large, causes it to have very high surface energy.Nano-calcium carbonate is with its unique function, it is compared with conventional material aspect a lot of and have obvious advantage, and show excellent performance at aspects such as improving the intensity of goods, toughness, dimensional stability, thermal characteristics, light stability, can replace the expensive stopping composition of part and auxiliary agent, reduce the consumption of resin, thereby for national save energy ，Wei enterprise reduces production costs.The every profession and trades such as plastics, rubber, coating, ink, papermaking have been widely used at present.Along with the continuous progress of science and technology, novel nano-calcium carbonate mineral filler emerges in an endless stream.The a lot of industries of nano-calcium carbonate in being penetrated into unconsciously our life.And through the effort of decades, various places scientific research personnel develop over one hundred kind of nano-calcium carbonate series in succession, and surface treated active nano-calcium carbonate product continues to bring out especially.And why calcium carbonate is subject to the favor of all trades and professions more and more, be because its raw material limestone is cheap and easy to get, there is the features such as production technique is simple, energy consumption is low, performance is more stable, and cost performance is very high.Current scientific research personnel is the continuous Nano-Calcium Carbonate of development of new hardy, and its Application Areas is constantly widened.In coating material production, nano-calcium carbonate is as loading pigment, have exquisiteness, evenly, the advantage such as high, the good in optical property of whiteness, nanometer grade super fine calcium carbonate has space steric effect, in painting, can make the zinc sulfide white that in formula, density is larger suspend, play anti-settling effect.After painting, paint film whiteness increases, and glossiness is high, and abrasion resistance is good, and opacifying power does not decline.Can partly substitute expensive titanium dioxide in formula.This characteristic makes it at coatings industry, by large-scale popularization, be applied.
At present, on market, have a lot of producers all selling nano-calcium carbonate, but real nano-calcium carbonate calcium product is few, although because nano-calcium carbonate has the many advantages of storage, the shortcoming of its maximum is difficult to disperse exactly, is easy to reunite, the shortcoming that this is fatal, has limited its application.Be exactly some nano-calcium carbonate in addition because its light weight, cause that dust pollution is serious in process of production, often to processing, make troubles.Shortcoming based on above nano-calcium carbonate, some illegal producer, has even expected being doped in nano-calcium carbonate calcium product with the larger coarse whiting of particle diameter ratio, drives its abundant dispersion and blanking in superpolymer.Bring great confusion to orderly market.
In the middle of prior art, need badly and want a kind of technology that can consider targetedly nano-calcium carbonate relative merits, it is maximized favourable factors and minimized unfavourable ones in adding procedure, find best method.
Summary of the invention
Technical problem to be solved by this invention is: in order to solve nano-calcium carbonate calcium powder in prior art, add the problems that occur, first the present invention is made into slurries by nano-calcium carbonate, in making processes, add again properties-correcting agent, finally to produce suspension good by wet-process modified, the water-borne coatings special-purpose nanometer modification agent that uniform particles degree is high.
A preparation method for water-borne coatings special-purpose nanometer modification agent, is characterized in that:
Step 1, get the Powdered nano-calcium carbonate of whiteness >=95%, be mixed with mass fraction and be 10%～35% slurry;
Step 2, the slurry configuring in step 1 is put in constant temperature water bath and heated, and progressively reach the preset temperature of 50 ℃～80 ℃;
Step 3, slurry preheated in step 2 is continued to stir with the speed of 300r/min, be 1%～3% to measure the properties-correcting agent sodium polyacrylate preparing in mass ratio, and in 5min, progressively join in slurry, continue to stir 0.5h～3h simultaneously;
Step 4, install in container after the good slurries of modification in step 3 are cooled to room temperature, sealing is preserved.
Described nano-calcium carbonate particles mean diameter is 30nm.The pH value of described nano-calcium carbonate is 8.0～10.0.
Beneficial effect: modification agent of the present invention is added in latex paint formulation system, successfully solved nano-calcium carbonate powder is difficult for disperseing in formulation for coating material, a difficult problem of easily reuniting, reduced dust pollution, after instead of titanium white powder, the contrast ratio of material and opacifying power have been improved in proportion, wash-resistant property obviously strengthens, emulsion paint sophistication is high, and storge quality is good, not free settling.
It is 30% slurry that a certain amount of satisfactory nano-calcium carbonate powder is made to massfraction, putting into constant temperature water bath heats, reach after predetermined 75 ℃ of temperature, under the stirring velocity turning at per minute 300, by the ratio preparing, be that 2.5% properties-correcting agent slowly joins in slurry in 5min, stir after 2h, install in container after the good slurries of modification are cooled to room temperature, sealing is preserved.
The modification agent of above-mentioned making is joined in latex paint formulation, and application report is as follows: table 1 nano-waterborne coating experimental formula
| Starting material | Consumption |
| Water | 200 |
| Dispersion agent | 7 |
| Non-ionic wetting agent | 1 |
| Defoamer | 3 |
| Propylene glycol | 15 |
| Multifunctional assistant | 1.5 |
| Sanitas | 1.5 |
| Titanium dioxide | 175 |
| 1250 order calcined kaolins | 50 |
| 1250 order talcum powder | 100 |
| 1250 order coarse whitings | 100 |
| Natvosol 1%(HEC) | 100 |
| Benzene emulsion | 300 |
| Film coalescence aid | 15 |
| Defoamer | 3-5 |
| Flow agent | 2 |
| Thickening material | In right amount |
Table 2 experiment starting material
The intelligent sand mill of instrument: SF, electronic balance, Albedometer, stormer viscosity meter, Hegman grind gage, the preparing device of filming, polyester film, eternit flat board are made and detected to coating
Table 3 assay
Experimental program: with the titanium dioxide in the nano modified dose of original formula of products substitution, substitution ratio is respectively 15%, 20%, 25%(is by nano-calcium carbonate powder weighing scale).(remarks: be 1. 15%; 2. be 20%; 3. 25%)
Interpretation:
Through to the monitoring of experimentation and the finishing analysis to experimental data, reach a conclusion: the coating that the present invention makes can be successfully applied to coating industry with nano modified dose.And all embodied its superiority in the following aspects:
1) stability in storage of nano modified dose is good: experiment showed, that this product stores 60 days without obviously sedimentation, container bottom produces without lump.
2) stability of nano modified dose is good: this product using for arbitrary day in 1～60 day all can reach good, consistent dispersion effect, unchanged in performance.
3) dispersiveness of emulsion paint is stable: in experimentation, add nano modified dose, without grinding, just can reach good dispersion effect, and after dispersion without the phenomenon of secondary agglomeration.
4) abrasion resistance of emulsion paint is good: from detecting data, along with nano-calcium carbonate substitutes the increase of measuring, wash-resistant property improves rapidly, the washability number of times of basic components sample paint is 310 times, after substituting 15% titanium dioxide, washability number of times increases to 760 times, after substituting 20% titanium dioxide, washability number of times increases to 1400 times, has reached the quality of premium grads.When the amount that substitutes reaches 25%, model is still intact through scrubbing 2700 paint films.
Can find out that thus the use of nano modified dose has improved the wash-resistant property of coating greatly.
5) emulsion paint condition in container is good: after storing, can opening detects, and the phenomenon of layering, caking, precipitation, flocculation does not appear in coating, and coating is still even, and viscosity does not change yet.
6) time of drying: shorten time of drying, paint film does not occur any abnormal.
7) appearance of film is good: the saturation ratio of filming increases, and feel is lubricated fine and smooth.
Embodiment
Below in conjunction with embodiment, the present invention is described in further detail.Of the present invention being characterized in: it is 10%～35% slurry that a certain amount of nano-calcium carbonate powder that meets above-mentioned requirements is made to massfraction, putting into constant temperature water bath heats, reach after predetermined 50 ℃～80 ℃ temperature, under the stirring velocity turning at per minute 300, the properties-correcting agent that is 1%～3% by the ratio preparing slowly joins in slurry in 5min, stir after 0.5h～3h, install in container after the good slurries of modification are cooled to room temperature, sealing is preserved.
Described self-control nano-calcium carbonate index is in Table 1; Properties-correcting agent is sodium polyacrylate.
Table 4 is for making the nano-calcium carbonate physical and chemical index of modification agent
| Project | Index | Detection method |
| Outward appearance | White powder | ------ |
| Particle shape | Cubes | Instrumental method |
| Mean diameter | 30nm | Instrumental method |
| Whiteness | ≥95% | Instrumental method |
| 105 degree volatilization content | ≤0.3% | Weighting method |
| Oil-absorption(number) | ≤30gDOP/100gCaCO 3 | Paddling process |
| PH value | 8.0-10.0 | PH meter |
| Tap density | ≤0.5g/cm 3 | Weighting method |
| Specific surface area | Agreement | Instrumental method |
| 300 screen residues | ≤0.1% | Method of sieving |
| CaCO 3 | ≥98.5% | Complexometry |
| MgO | ≤0.5% | Complexometry |
| W（Fe） | ≤0.1% | Complexometry |
| Hydrochloric acid insoluble substance | ≤0.2% | Weighting method |
Embodiment mono-: it is 15% slurry that a certain amount of nano-calcium carbonate powder that meets above-mentioned requirements is made to massfraction, putting into constant temperature water bath heats, reach after predetermined 60 ℃ of temperature, under the stirring velocity turning at per minute 300, by the ratio preparing, be that 1.2% properties-correcting agent slowly joins in slurry in 5min, stir after 0.5h, install in container after the good slurries of modification are cooled to room temperature, sealing is preserved.
Embodiment bis-: it is 20% slurry that a certain amount of nano-calcium carbonate powder that meets above-mentioned requirements is made to massfraction, putting into constant temperature water bath heats, reach after predetermined 65 ℃ of temperature, under the stirring velocity turning at per minute 300, by the ratio preparing, be that 1.5% properties-correcting agent slowly joins in slurry in 5min, stir after 1h, install in container after the good slurries of modification are cooled to room temperature, sealing is preserved.
Embodiment tri-: it is 25% slurry that a certain amount of nano-calcium carbonate powder that meets above-mentioned requirements is made to massfraction, putting into constant temperature water bath heats, reach after predetermined 70 ℃ of temperature, under the stirring velocity turning at per minute 300, by the ratio preparing, be that 1.8% properties-correcting agent slowly joins in slurry in 5min, stir after 1.5h, install in container after the good slurries of modification are cooled to room temperature, sealing is preserved.
Embodiment tetra-: it is 30% slurry that a certain amount of nano-calcium carbonate powder that meets above-mentioned requirements is made to massfraction, putting into constant temperature water bath heats, reach after predetermined 75 ℃ of temperature, under the stirring velocity turning at per minute 300, by the ratio preparing, be that 2.5% properties-correcting agent slowly joins in slurry in 5min, stir after 2h, install in container after the good slurries of modification are cooled to room temperature, sealing is preserved.
Claims (3)
1. a preparation method for water-borne coatings special-purpose nanometer modification agent, is characterized in that:
Step 1, get the Powdered nano-calcium carbonate of whiteness >=95%, be mixed with mass fraction and be 10%～35% slurry;
Step 2, the slurry configuring in step 1 is put in constant temperature water bath and heated, and progressively reach the preset temperature of 50 ℃～80 ℃;
Step 3, slurry preheated in step 2 is continued to stir with the speed of 300r/min, be 1%～3% to measure the properties-correcting agent sodium polyacrylate preparing in mass ratio, and in 5min, progressively join in slurry, continue to stir 0.5h～3h simultaneously;
Step 4, install in container after the good slurries of modification in step 3 are cooled to room temperature, sealing is preserved.
2. the preparation method of a kind of water-borne coatings special-purpose nanometer modification agent according to claim 1, is characterized in that: described nano-calcium carbonate particles mean diameter is 30nm.
3. the preparation method of a kind of water-borne coatings special-purpose nanometer modification agent according to claim 1, is characterized in that: the pH value of described nano-calcium carbonate is 8.0～10.0.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105778569A (en) * | 2016-05-05 | 2016-07-20 | 中钛集团洛阳市裕星化工有限公司 | Method for preparing composite titanium dioxide powder with titanium-coated light calcium carbonate |
| CN106366697A (en) * | 2016-08-23 | 2017-02-01 | 刘东进 | Preparation method of ceramic white active calcium carbonate applied in aqueous coating |
| CN112409822A (en) * | 2020-12-07 | 2021-02-26 | 江西华明纳米碳酸钙有限公司 | Preparation method of special nano calcium carbonate for water-based paint |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1122309A (en) * | 1995-07-25 | 1996-05-15 | 宁波开发区亚光发展公司 | Wet process for superfine heavy calcium carbonate |
-
2013
- 2013-01-24 CN CN201310028534.0A patent/CN103525129A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1122309A (en) * | 1995-07-25 | 1996-05-15 | 宁波开发区亚光发展公司 | Wet process for superfine heavy calcium carbonate |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105778569A (en) * | 2016-05-05 | 2016-07-20 | 中钛集团洛阳市裕星化工有限公司 | Method for preparing composite titanium dioxide powder with titanium-coated light calcium carbonate |
| CN105778569B (en) * | 2016-05-05 | 2017-10-31 | 中钛集团洛阳市裕星化工有限公司 | A kind of preparation method of the composite titanium dioxide of titanium cladding precipitated calcium carbonate |
| CN106366697A (en) * | 2016-08-23 | 2017-02-01 | 刘东进 | Preparation method of ceramic white active calcium carbonate applied in aqueous coating |
| CN112409822A (en) * | 2020-12-07 | 2021-02-26 | 江西华明纳米碳酸钙有限公司 | Preparation method of special nano calcium carbonate for water-based paint |
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Application publication date: 20140122 |