CN103627242A - Preparation method of delustering agent for UV (ultraviolet) curing coating - Google Patents
Preparation method of delustering agent for UV (ultraviolet) curing coating Download PDFInfo
- Publication number
- CN103627242A CN103627242A CN201310627382.6A CN201310627382A CN103627242A CN 103627242 A CN103627242 A CN 103627242A CN 201310627382 A CN201310627382 A CN 201310627382A CN 103627242 A CN103627242 A CN 103627242A
- Authority
- CN
- China
- Prior art keywords
- raw material
- matting agent
- preparation
- coating
- reactor
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Landscapes
- Paints Or Removers (AREA)
- Silicon Compounds (AREA)
Abstract
The invention discloses a preparation method of a delustering agent for a UV (ultraviolet) curing coating. The preparation method comprises the steps of firstly adding 5-40% by mass of inorganic acid solution to a reactor while stirring; heating 5-50% by mass of alkali metal inorganic silicate solution, then adding the alkali metal inorganic silicate solution and 60-90 parts of wax emulsion required by an end product to the reactor simultaneously, and controlling the pH value to be 0.5-5.5; heating to 95-100 DEG C while stirring, preserving heat for 0.5-4 hours, and aging; washing and spray-drying the aged material to obtain a crude product; atomizing 10-40 parts of remaining wax emulsion, fully mixing the wax emulsion with the crude product at 92-100 DEG C, and preserving heat for 1-6 hours; carrying out ultrafine grinding on the uniformly mixed material until the mean grain size is 3-5mu m, wherein the loss on ignition of the end product is 22-24%. The delustering agent prepared by the method has uniform grain size, stable pore structure and stable quality, has excellent delustering performance when used in the UV curing coating, has little effect of changing the viscosity of a UV coating system, and is beneficial to film formation of the coating.
Description
Technical field
The present invention relates to matting agent field, particularly, relate to the coating material solidified preparation method with matting agent of a kind of UV.
Background technology
UV is coating material solidified because its environmental protection, curing speed are fast and film and have excellent physicochemical property, thereby the application in the industrial production such as timber floor and furniture is more and more extensive, the surface daub on a wall field of the object of, surface imperfection little at some small household appliances, ornament equal-volume, bring into play especially its characteristic, put it over.Because UV is coating material solidified not containing volatile solvent, the volumetric shrinkage of filming when curing is very little, be usually less than 10%, the matting agent product that conventional precipitation method is produced is difficult to appear at coatingsurface therein, thereby does not reach desirable flatting efficiency, the matting agent product that vapor phase process is produced, production cost is higher, and its BET is bigger than normal, in the coating material solidified production process of UV, can make dope viscosity enlarge markedly, be unfavorable for the film process of filming.
Produced in the technique of matting agent in the past, and conventionally first to add a certain amount of alkali lye in reactor, and then under whipped state, added mineral acid to carry out, the pore structure that this generic operation obtains conventionally, pore volume is bigger than normal, does not meet the coating material solidified use needs of UV.Multiple research explanation, UV is coating material solidified is different from conventional matting agent product by the selected pore structure scope of matting agent, requires pore structure to be the bigger the better, but requires pore volume smaller, and pore structure is stable.
As can be seen here, the matting agent of producing by above-mentioned preparation method cannot meet the coating material solidified demand of UV, and is urgently further improved.
Summary of the invention
The object of the present invention is to provide the coating material solidified preparation method with matting agent of a kind of UV, the matting agent epigranular that makes to prepare by the method, pore structure are stable, steady quality, and it is good that this matting agent is used in the coating material solidified middle eliminate optical property of UV, less to UV coating system viscosity-modifying, be beneficial to coating film forming.
For achieving the above object, the present invention adopts following technical scheme:
The coating material solidified preparation method with matting agent of UV, comprising:
(1) raw material:
Raw material A: the inorganic acid solution that mass ratio is 5～40%;
Raw material B: the basic metal inorganic silicic acid salts solution that mass ratio is 5～50%;
Raw material C: the wax emulsion that end product requires;
(2) preparation process:
(a) in reactor, add raw material A, keep stirring; Raw material B temperature after heating is controlled to 50～85 ℃, then joins in the reactor that contains raw material A with the raw material C of 60-90% part simultaneously, material pH value in reactor is controlled to 0.5～5.5;
(b) after having fed in raw material, keep stirring to be warming up to 95～100 ℃, be incubated 0.5～4 hour, carry out aging;
(c) aging complete material washs, sprays to be dried and obtains crude product;
(d) by remaining 10-40% part raw material C atomization, at 92～100 ℃, make it fully mix with crude product, be incubated 1～6 hour;
(e) material mixing is 3～5 μ m through superfine grinding to median size, and the burning decrement of end product is 22～24%.
Further, described raw material A adopts the inorganic acid solution that mass ratio is 10～15%; Described raw material B adopts the basic metal inorganic silicic acid salts solution that mass ratio is 15～20%.
Further, described mineral acid adopts sulfuric acid, hydrochloric acid or nitric acid, and described basic metal inorganic silicate adopts water glass, potassium silicate, sodium-potassium silicate, lithium silicate or silicic acid quaternary ammonium.
Further, in described step (a), raw material B temperature after heating is controlled to 75～80 ℃; In reactor, material pH value is controlled at 2.5～3.5.
Further, in described step (a), raw material B first mixes with raw material C, and mixed discharge port material is fan-shaped state, enters reactor.
Further, in described step (b), keep stirring to be warming up to 98 ℃, be incubated 1～2 hour.
Further, in described step (d), at 95 ℃, make the raw material C after atomization fully mix with crude product, be incubated 4 hours.
Further, the matting agent of preparing through the method has following technical indicator:
BET 100～250cm
2/g；
DBP absorption value 0.4～2.2g/g.
Compared with prior art, the present invention has following beneficial effect:
1, in the present invention, adopting mineral alkali to add in mineral acid operates; obtain the product of low BET, low DBP absorption value; and the multi-level interpolation of passing through wax emulsion obtains suspension effect when UV is coating material solidified to be applied; final obtain UV good feel and viscosity reliably in coating material solidified, and product formation large-scale industrial manufactures a finished product and only accounts for 1/3rd of imported product price.
2, the cost of material that the present invention uses is cheap, different from traditional matting agent, coating material solidified applicable to UV through the matting agent of special surperficial organic process and superfine grinding complete processing.Matting agent epigranular prepared by this preparation method, pore structure are stable, steady quality, purity is high and viscosity is low, has solved the variety of issue that traditional matting agent production technique committed step is brought in the coating material solidified middle use of UV for product.
3, the matting agent of preparing through preparation method of the present invention, makes after flatting silica in UV coating eliminate optical property good, less to UV coating system viscosity-modifying, is beneficial to coating film forming, becomes film coating flatting silica particle alignment homogeneous, and gloss is soft.
Embodiment
Below the preferred embodiments of the present invention are described, should be appreciated that preferred embodiment described herein, only for description and interpretation the present invention, is not intended to limit the present invention.
The coating material solidified preparation method with matting agent of a kind of UV of the present invention, comprising:
(1) raw material:
Raw material A: the inorganic acid solution that mass ratio is 5～40%; Preferred mass is than the inorganic acid solution that is 10～15%; Wherein, mineral acid can adopt sulfuric acid or hydrochloric acid, or other can reach the mineral acid of effect of the present invention, as nitric acid etc.
Raw material B: the basic metal inorganic silicic acid salts solution that mass ratio is 5～50%; Preferred mass is than the basic metal inorganic silicic acid salts solution that is 15～20%, and wherein, basic metal inorganic silicate can adopt water glass, or potassium silicate, sodium-potassium silicate, lithium silicate and silicic acid quaternary ammonium etc. can obtain the product of same texts.
Raw material C: the wax emulsion that end product requires; Wherein, wax emulsion comprises that the wax of any routine is dispersed in water-adds if desired the emulsion of emulsifying agent-formation; As the wax emulsion of the method institute emulsification in available CN101481115.
The addition of above-mentioned wax emulsion is directly proportional to the burning decrement of end product, the preparation method of concrete addition is: by method of the present invention, do preliminary experiment, but wherein do not add wax emulsion, can obtain the burning decrement of the end product while not doing wax processing, be generally 3-5%, and the present invention requires when making wax and processing, the burning decrement of end product is 22-24%, burning decrement when burning decrement deducts and do not do wax processing during as wax processing can be determined the amount of the solid wax in wax emulsion, and then the addition of definite wax emulsion.
(2) preparation process:
(a) in reactor, add raw material A, keep stirring; Raw material B temperature after heating is controlled to 50～85 ℃, preferably 75～80 ℃, then join in the reactor that contains raw material A with the raw material C of 60-90% part simultaneously, material pH value in reactor is controlled to 0.5～5.5, preferably 2.5～3.5, keep dispersion state; Preferably, raw material B can first adopt the mixing tank of CN102476802A to mix with raw material C, then makes mixed discharge port material be fan-shaped state, enters reactor.
(b), after having fed in raw material, keep stirring to be warming up to 95～100 ℃, preferably 98 ℃, be incubated 0.5～4 hour, preferably 1～2 hour, carry out aging.
(c) aging complete material filters and uses deionized water wash, the drier crude product that obtains of spraying.
(d) by remaining 10-40% part raw material C atomization, at 92～100 ℃, preferably 95 ℃, it is fully mixed with crude product, be incubated 1～6 hour, preferably 4 hours; The mixing device that wherein, can pass through CN103170267A is by raw material C atomization.
(e) material that mixes is through Ultrafine Jet Milling, to median size be 3～5 μ m.
The matting agent of preparing through aforesaid method has following technical indicator:
BET 100～250cm
2/g；
DBP absorption value 0.4～2.2g/g;
Burning decrement 22～24%.
Embodiment 1-10
In reaction vessel, add raw material A (take sulfuric acid as example), keep stirring, raw material B(be take to water glass as example) temperature after heating is controlled at 75～80 ℃, adopt the mixing tank of CN102476802A and the raw material C of 60-90% part to be mixed to join in reaction vessel, reaction mass pH value is controlled to 2.5～3.5; Stirring is warming up to 95～100 ℃, is incubated 1～2 hour; Washing, the dry rear crude product that obtains; Mixing device by CN103170267A, by the raw material C atomization of 10-40% part, fully mixes insulation 1～6 hour at 92～100 ℃ with crude product, and superfine grinding is to median size 3～5 μ m.By changing reaction conditions etc., obtain different embodiment products.
Test data BET100～250cm
2/ g; DBP absorption value 0.4～2.2g/g; Burning decrement 22～24%.
| Embodiment | BETcm 2/g | DBPg/g | Burning decrement % | Median size μ m |
| 1 | 188 | 0.8 | 23.4 | 4.05 |
| 2 | 192 | 0.9 | 23.4 | 4.10 |
| 3 | 220 | 1.3 | 23.2 | 4.11 |
| 4 | 210 | 1.2 | 23.8 | 3.98 |
| 5 | 190 | 0.8 | 22.9 | 3.66 |
| 6 | 199 | 0.9 | 22.4 | 4.20 |
| 7 | 201 | 1.0 | 23.8 | 4.15 |
| 8 | 203 | 1.0 | 22.7 | 4.23 |
| 9 | 209 | 1.0 | 22.3 | 3.87 |
| 10 | 218 | 1.3 | 22.4 | 4.09 |
Comparative example 1
The sodium silicate solution that adds 20 ℃ of 100kg15% in reactor, after adding 20% sulphur acid for adjusting pH value to be 9 under whipped state, after stirring 20min, adding acid for adjusting pH value is 4, is heated to 60 ℃, and adding ammoniacal liquor to regulate pH value is 10, be warming up to 100 ℃ aging 2 hours, add acid for adjusting pH value to 3, add wax emulsion 41kg, ageing 30min, through washing, dry, finished product is processed in superfine grinding.The key technical indexes:
Comparative example 2
The sodium silicate solution that adds 20 ℃ of 110kg10% in reactor, under whipped state, adding 30% sulphur acid for adjusting pH value is 10, after stirring 20min, adding acid for adjusting pH value is 3, is heated to 60 ℃, and adding ammoniacal liquor to regulate pH value is 10, be warming up to 100 ℃ aging 5 hours, add acid for adjusting pH value to 3, add wax emulsion 30kg, ageing 30min, through washing, dry, finished product is processed in superfine grinding.
The key technical indexes:
Comparative example 3
The coating material solidified matting agent the key technical indexes of using of import UV:
Application examples 1
The UV that uses is coating material solidified has following composition:
Epoxy acrylate
TPGDA:TMPTA mass ratio is 2:1
IHT-PI1173
Flatting silica 10%
By above-mentioned coating composition and ratio, be coated with-4 glasss while being controlled at 30～40s, add flatting silica, with high speed dispersor, with 3000r/min, disperse 5 minutes, the coating having disperseed is coated to deep base paint material ground, through UV, solidify machine and solidify after 2 seconds, the flatting silica that contrast different process is produced and import UV are coating material solidified with matting agent, make feel, extinction and the outward appearance of coating.Shown in comparing result following table:
Above-mentioned 10 embodiment that provide are only for preferred embodiment, and wherein each reactive component and reaction conditions can be done suitable variation in allowed limits, be applied to UV coating material solidified in, also can reach similar effect, the transparency is good, the slightly thick and good fluidity of viscosity.
Finally it should be noted that: the foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, although the present invention is had been described in detail with reference to previous embodiment, for a person skilled in the art, its technical scheme that still can record previous embodiment is modified, or part technical characterictic is wherein equal to replacement.Within the spirit and principles in the present invention all, any modification of doing, be equal to replacement, improvement etc., within all should being included in protection scope of the present invention.
Claims (8)
1. the coating material solidified preparation method with matting agent of UV, is characterized in that, comprising:
(1) raw material:
Raw material A: the inorganic acid solution that mass ratio is 5～40%;
Raw material B: the basic metal inorganic silicic acid salts solution that mass ratio is 5～50%;
Raw material C: the wax emulsion that end product requires;
(2) preparation process:
(a) in reactor, add raw material A, keep stirring; Raw material B temperature after heating is controlled to 50～85 ℃, then joins in the reactor that contains raw material A with the raw material C of 60-90% part simultaneously, material pH value in reactor is controlled to 0.5～5.5;
(b) after having fed in raw material, keep stirring to be warming up to 95～100 ℃, be incubated 0.5～4 hour, carry out aging;
(c) aging complete material washs, sprays to be dried and obtains crude product;
(d) by remaining 10-40% part raw material C atomization, at 92～100 ℃, make it fully mix with crude product, be incubated 1～6 hour;
(e) material mixing is 3～5 μ m through superfine grinding to median size, and the burning decrement of end product is 22～24%.
2. the coating material solidified preparation method with matting agent of UV according to claim 1, is characterized in that, described raw material A adopts the inorganic acid solution that mass ratio is 10～15%; Described raw material B adopts the basic metal inorganic silicic acid salts solution that mass ratio is 15～20%.
3. the coating material solidified preparation method with matting agent of UV according to claim 1 and 2, it is characterized in that, described mineral acid adopts sulfuric acid, hydrochloric acid or nitric acid, and described basic metal inorganic silicate adopts water glass, potassium silicate, sodium-potassium silicate, lithium silicate or silicic acid quaternary ammonium.
4. the coating material solidified preparation method with matting agent of UV according to claim 1, is characterized in that, in described step (a), raw material B temperature after heating is controlled to 75～80 ℃; In reactor, material pH value is controlled at 2.5～3.5.
5. the coating material solidified preparation method with matting agent of UV according to claim 1, is characterized in that, in described step (a), raw material B first mixes with raw material C, and mixed discharge port material is fan-shaped state, enters reactor.
6. the coating material solidified preparation method with matting agent of UV according to claim 1, is characterized in that, in described step (b), keeps stirring to be warming up to 98 ℃, is incubated 1～2 hour.
7. the coating material solidified preparation method with matting agent of UV according to claim 1, is characterized in that, in described step (d), makes the raw material C after atomization fully mix with crude product at 95 ℃, is incubated 4 hours.
8. the coating material solidified preparation method with matting agent of described UV according to claim 1, is characterized in that, the matting agent of preparing through the method has following technical indicator:
BET 100～250cm
2/g；
DBP absorption value 0.4～2.2g/g.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310627382.6A CN103627242B (en) | 2013-11-29 | 2013-11-29 | Preparation method of delustering agent for UV (ultraviolet) curing coating |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310627382.6A CN103627242B (en) | 2013-11-29 | 2013-11-29 | Preparation method of delustering agent for UV (ultraviolet) curing coating |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN103627242A true CN103627242A (en) | 2014-03-12 |
| CN103627242B CN103627242B (en) | 2015-03-04 |
Family
ID=50208705
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310627382.6A Active CN103627242B (en) | 2013-11-29 | 2013-11-29 | Preparation method of delustering agent for UV (ultraviolet) curing coating |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN103627242B (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105062187A (en) * | 2015-09-01 | 2015-11-18 | 邯郸市龙翔化工材料有限公司 | Physical delustering micro powder and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4097302A (en) * | 1976-02-17 | 1978-06-27 | Scm Corporation | Flatting agents |
| CN1585800A (en) * | 2001-11-13 | 2005-02-23 | 伊尼奥斯硅石有限公司 | Silica matting agents |
| CN103043670A (en) * | 2012-12-26 | 2013-04-17 | 青岛中能集团有限公司 | Process flow of novel water-absorbent silica gel |
-
2013
- 2013-11-29 CN CN201310627382.6A patent/CN103627242B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US4097302A (en) * | 1976-02-17 | 1978-06-27 | Scm Corporation | Flatting agents |
| CN1585800A (en) * | 2001-11-13 | 2005-02-23 | 伊尼奥斯硅石有限公司 | Silica matting agents |
| CN103043670A (en) * | 2012-12-26 | 2013-04-17 | 青岛中能集团有限公司 | Process flow of novel water-absorbent silica gel |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105062187A (en) * | 2015-09-01 | 2015-11-18 | 邯郸市龙翔化工材料有限公司 | Physical delustering micro powder and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| CN103627242B (en) | 2015-03-04 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN100522807C (en) | Method for preparing silicon dioxide with large pore volume and large aperture | |
| CN103911021B (en) | A kind of transparent magnesium hydroxide liquid dispersion and preparation method and application | |
| CN105400239A (en) | Preparation method of modified silicon dioxide obtained via super-hydrophobic modification | |
| CN101812289B (en) | Nanometer polysilicon particles and preparation method and application thereof | |
| CN106044790B (en) | A kind of method of preparing white carbon black by precipitation method | |
| CN105178008A (en) | Synthetic leather surface treatment agent and preparation method thereof | |
| CN105417565A (en) | Cubic CaCO3 and SiO2 composite particles and preparing method thereof | |
| CN101121841A (en) | Water exterior wall paint and its preparing process | |
| CN106317421B (en) | A kind of high-performance cationic rosin size and preparation method thereof | |
| DE112020000050T5 (en) | Process for the production of hollow glass microsphere with high floating ratio | |
| CN110845878A (en) | Preparation method of inorganic modified water-based environment-friendly interior wall coating | |
| CN103627242B (en) | Preparation method of delustering agent for UV (ultraviolet) curing coating | |
| CN103965759A (en) | Composite leather coating agent and preparation method thereof | |
| CN105819484A (en) | Preparation method and dispersing method of nano CaCO3/SiO2 composite particle | |
| CN104610783B (en) | A kind of transparent aluminium hydroxide liquid dispersion and preparation method and application | |
| CN101481115B (en) | Silicon dioxide, preparation and use thereof | |
| CN117106349B (en) | Preparation method of high-performance fireproof water-based inorganic coating | |
| CN105217673B (en) | A kind of preparation method of high thixotropic silicone adhesive special-purpose nanometer activated Calcium carbonate | |
| CN106905751A (en) | The preparation method of parental type silica dioxide delustring agent | |
| CN105273593A (en) | Waterborne one-component glass coating and preparation method thereof | |
| CN106147892A (en) | A kind of white oil nanometer additive, preparation method and modified white oil thereof | |
| CN106085160A (en) | A kind of environmentally friendly alkide resin emulsion of zero VOC content and preparation method thereof | |
| CN110205865A (en) | A kind of preparation method of tensile type hydrophobic paper | |
| CN103087203A (en) | Method for preparing low-viscosity sodium carboxymethyl cellulose by adopting low-viscosity sodium carboxymethyl cellulose | |
| CN210915902U (en) | Modified aluminum hypophosphite apparatus for producing |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant |