CN104530770A - Preparation method of high-transparency low-oil-absorption-number matting powder - Google Patents
Preparation method of high-transparency low-oil-absorption-number matting powder Download PDFInfo
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- CN104530770A CN104530770A CN201510037855.6A CN201510037855A CN104530770A CN 104530770 A CN104530770 A CN 104530770A CN 201510037855 A CN201510037855 A CN 201510037855A CN 104530770 A CN104530770 A CN 104530770A
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- flatting silica
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- high transparency
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- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- 239000000843 powder Substances 0.000 title abstract description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 74
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 37
- 238000010521 absorption reaction Methods 0.000 claims abstract description 19
- 235000012239 silicon dioxide Nutrition 0.000 claims abstract description 12
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims abstract description 11
- 229910052731 fluorine Inorganic materials 0.000 claims abstract description 11
- 239000011737 fluorine Substances 0.000 claims abstract description 11
- 238000006243 chemical reaction Methods 0.000 claims abstract description 8
- 238000010298 pulverizing process Methods 0.000 claims abstract description 7
- 238000004132 cross linking Methods 0.000 claims abstract description 5
- 238000001035 drying Methods 0.000 claims abstract description 3
- 238000005406 washing Methods 0.000 claims abstract description 3
- 239000002253 acid Substances 0.000 claims description 17
- -1 siloxanes Chemical class 0.000 claims description 17
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 238000001914 filtration Methods 0.000 claims description 10
- 229960001866 silicon dioxide Drugs 0.000 claims description 9
- 239000002002 slurry Substances 0.000 claims description 8
- 230000004048 modification Effects 0.000 claims description 7
- 238000012986 modification Methods 0.000 claims description 7
- 239000002245 particle Substances 0.000 claims description 7
- QAOWNCQODCNURD-UHFFFAOYSA-N Sulfuric acid Chemical compound OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 6
- 150000004645 aluminates Chemical class 0.000 claims description 6
- 235000019353 potassium silicate Nutrition 0.000 claims description 6
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 6
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims description 5
- 239000007822 coupling agent Substances 0.000 claims description 5
- 229910000077 silane Inorganic materials 0.000 claims description 5
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims description 4
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 4
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 4
- BFKJFAAPBSQJPD-UHFFFAOYSA-N tetrafluoroethene Chemical group FC(F)=C(F)F BFKJFAAPBSQJPD-UHFFFAOYSA-N 0.000 claims description 4
- 238000010792 warming Methods 0.000 claims description 4
- 150000004759 cyclic silanes Chemical class 0.000 claims description 3
- 239000003607 modifier Substances 0.000 claims description 3
- 229920000573 polyethylene Polymers 0.000 claims description 3
- 239000004698 Polyethylene Substances 0.000 claims description 2
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 2
- 229920000642 polymer Polymers 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000000576 coating method Methods 0.000 abstract description 17
- 239000011248 coating agent Substances 0.000 abstract description 15
- 238000000034 method Methods 0.000 abstract description 2
- 230000008569 process Effects 0.000 abstract description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 2
- 239000005416 organic matter Substances 0.000 abstract 3
- 239000003921 oil Substances 0.000 abstract 2
- 238000011085 pressure filtration Methods 0.000 abstract 1
- 238000003756 stirring Methods 0.000 description 10
- 239000003973 paint Substances 0.000 description 6
- 239000000839 emulsion Substances 0.000 description 5
- 230000015572 biosynthetic process Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 238000005507 spraying Methods 0.000 description 4
- 230000008033 biological extinction Effects 0.000 description 3
- 238000009413 insulation Methods 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 2
- 239000006185 dispersion Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229920001296 polysiloxane Polymers 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000000725 suspension Substances 0.000 description 2
- 206010015535 Euphoric mood Diseases 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- 229920000180 alkyd Polymers 0.000 description 1
- 239000008199 coating composition Substances 0.000 description 1
- 230000006378 damage Effects 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000001877 deodorizing effect Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000001879 gelation Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 239000010985 leather Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000035699 permeability Effects 0.000 description 1
- 229920000728 polyester Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 201000007094 prostatitis Diseases 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000002966 varnish Substances 0.000 description 1
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- Silicon Compounds (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
Abstract
The invention relates to a preparation method of high-transparency low-oil-absorption-number matting powder. The preparation method comprises the following steps: acidifying, fluoridizing, double coating, water washing, pressure filtration, drying and pulverization. After the fluorine-containing organic matter is added, the product can not easily spill in the use process; and the gap of the silicon dioxide is filled with the fluorine-containing organic matter to lower the oil absorption number. The crosslinkable long-chain organic matter, which can perform crosslinking reaction with silicon dioxide, is added and grafted to the silicon dioxide surface, and the wax is recoated and sealed, thereby further lowering the oil absorption number.
Description
Technical field
The invention belongs to flatting silica and manufacture field, be specifically related to the preparation method of the low oil-absorption(number) flatting silica of a kind of high transparency.
Background technology
Flatting silica can be divided into oiliness flatting silica and water-based flatting silica.Be widely used in emulsion paint, coating for internal and external wall, leather coating, in the multiple coating such as alkyd varnish and Polyester Paint system.In application of paint, paint, control film coated surface gloss that can be balanced, plays anti-settling effect to color stuffing, improves the feel of paint film, increases wear resistance and the mar-resistance of film, dries, deodorizing, to purify air, sound insulation, waterproof and heat insulation, permeability.
In recent years, the coatings industry of China is in the ascendant, and coating ultimate production also leaps to the prostatitis in the world, defines an industrial groups related to this, actively promotes technological revolution and the development of traditional field of coating.The advantages such as the light coating of high gloss is bright in colour with it, bright are in the meantime well received by consumers, and within considerable time, unify Coating Market.But, along with improving constantly of people's living standard, on the one hand human consumer felt high gloss light coating film forming after reflective relatively more serious, the eyes of people are harmful to; The aesthetic standards of human consumer more and more tend to leisure, fashion and personalization on the other hand.Add China's automobile and the flourish demand of household electric appliances.These factors just result in the demand of people to the coatings with low gloss finish with soft outward appearance sharply to be increased.Meanwhile, also make how to produce the coating with eliminate optical property and become the problem that coating Designerss must consider.
Existing silicon-dioxide flatting silica product technology, its oil-absorption(number), at more than 250g/100g, makes to add in coating, and the viscosity of system is comparatively large, easily produces gel in dispersion process, makes dispersion more difficult; The technology of existing flatting silica generally realizes good transparency by adjustment particle diameter, but makes the extinction effect of product decline simultaneously.
Current silicon-dioxide flatting silica technology, mainly contain by adding wax emulsion coated, or add silane coupling agent, titanic acid ester, aluminate coupling agent carry out surface modification to silicon-dioxide.The coated product of wax in use, in use easily separated out by solvent, causes very big destruction to the performance of coating by the wax on its surface; The product of titanic acid ester and Aluminate is higher due to refractive index, and its extinction effect is weakened, and transparency declines.
Patent 2004800072875 discloses a kind of matte powder coating composition.Wherein shorten gelation time containing resin and solidifying agent, but its product can form larger space when applying, oil-absorption(number) is higher, bad dispersibility.The density of product is comparatively large simultaneously, and extinction effect is poor.
The present invention is directed to above defect and done corresponding improvement, mainly through repeatedly coated, make flatting silica surface pore less, reduce oil-absorption(number); Improve and the consistency of coating and promote dispersiveness; Refractive index is adopted to enhance the transparency close to the material of flatting silica.
Summary of the invention
A preparation method for the low oil-absorption(number) flatting silica of high transparency, is characterized in that, the step of described preparation method is:
(1) acid adding: add water glass in a kettle., opens and stirs, add acid.After forming gel, stop acid adding, be warming up to 48-52 DEG C immediately, adding acid for adjusting pH value is 4-5, stirs 60 minutes;
(2) fluoridize: add organic fluorocompound, one or more simultaneously adding in coupling agent carry out surface modification, and the reaction times is 55-65 minute;
(3) secondary capsulation: be warming up to 55-85 DEG C, add the long-chain organism with bridging property, and silicon-dioxide carries out crosslinking reaction, adds ethanol simultaneously, and reaction 1.5-2.5 hour, carries out secondary capsulation;
(4) wash, press filtration: slurry to be washed, press filtration;
(5) dry, pulverizing: finally drying and pulverizing are carried out to flatting silica.
Described fluorine-containing organic modifiers is one or more of tetrafluoroethylene wax, fluorine containing silane coupling agent and fluorine-containing cyclic silane.The described long-chain organism with bridging property is long-chain siloxanes and with one or more of the molecular weight polymers of siloxane structure.
Described coupling agent is one or more in silane, Aluminate, titanic acid ester, polyethylene wax.
Described washing, press filtration make slurries specific conductivity be reduced to 300 below μ s/cm.
Described pulverizing gained flatting silica particle diameter is 4.0-6.0 μm, is preferably 4.0-5.0 μm.
After the present invention adds organic fluorocompound, product is in use not easily overflowed, organic fluorocompound is filled in the space of silicon-dioxide, reduces its oil-absorption(number).Add siloxanes organism, this siloxanes organism can carry out crosslinking reaction with silicon-dioxide, is grafted to silica sphere, and again coated to wax wherein, closes, oil-absorption(number) is reduced further.Siloxanes organism can bring the less density of product and better suspension property simultaneously, is in use easily suspended on the surface, improves flatting efficiency.Secondary is coated can be again coated complete by wax above, makes it in use not overflow.Meanwhile, because this layer of coating itself is similar with the resin structure in paint, silicon-dioxide glossiness in use and transparency are improved.The use of linking agent can strengthen bridging property and the hiding power of product, improves flatting efficiency further.
Embodiment
embodiment 1:
Add 3000kg water glass in a kettle., open and stir, start to add hydrofluoric acid, after formation gel, stop acid adding, be warmed up to 48 DEG C immediately, again add acid for adjusting pH value to 4, stir 60 minutes.
Add tetrafluoroethylene wax emulsion wherein, 500kg, add silane and each 40kg of Aluminate carries out surface modification, react 65 minutes.
Be warmed up to 58 DEG C, add the water-soluble acrylic 50kg of grafted silicone, allocate 50kg ethanol simultaneously into, insulation reaction 1.5 hours, make its secondary coated.
Slurry is washed, press filtration, make its specific conductivity be reduced to 300 below μ s/cm.Spraying dry, is then crushed to the particle diameter of 4 μm.
embodiment 2:
Add 3000kg water glass in a kettle., open and stir, start to add phosphoric acid, after formation gel, stop acid adding, be warmed up to 52 DEG C immediately, again add acid for adjusting pH value to 5, stir 60 minutes.
Add fluorine containing silane coupling agent wherein, 400kg, add polythene wax emulsion and each 50kg of titanic acid ester carries out surface modification, react 90 minutes.
Be warmed up to 84 DEG C, add linear siloxanes 35kg, allocate 70kg ethanol simultaneously into, react 2.5 hours, make its secondary coated.
Slurry is washed, press filtration, make its specific conductivity be reduced to 300 below μ s/cm.Spraying dry, is then crushed to the particle diameter of 6 μm.
embodiment 3:
Add 3000kg water glass in a kettle., open and stir, start to add sulfuric acid, after formation gel, stop acid adding, be warmed up to 50 DEG C immediately, again add acid for adjusting pH value to 4.5, stir 60 minutes.
Add fluorine-containing cyclic silane wherein, 1000kg, add silane and each 25kg of titanic acid ester carries out surface modification, react 1 hour.
Be warmed up to 68 DEG C, add the aqurous ployurethane 30kg of grafted silicone, linear siloxanes 40kg, allocate 50kg ethanol simultaneously into, react 2 hours, make its secondary coated.
Slurry is washed, press filtration, make its specific conductivity be reduced to 300 below μ s/cm.Spraying dry, is then crushed to the particle diameter of 5 μm.
embodiment 4:
Add 3000kg water glass in a kettle., open and stir, start to add sulfuric acid, after formation gel, stop acid adding, be warmed up to 48 DEG C immediately, again add acid for adjusting pH value to 4, stir 60 minutes.
Add tetrafluoroethylene wax emulsion wherein, 800kg, add silane and each 40kg of Aluminate carries out surface modification, react 120 minutes.
Slurry is washed, press filtration, make its specific conductivity be reduced to 300 below μ s/cm.Spraying dry, is then crushed to the particle diameter of 5 μm.
With following table 1 pair of embodiment 1, embodiment 2, embodiment 4 and patent 2004800072875(documents) embodiment carry out the detection of oil-absorption(number), anti-settling and glossiness,
Table 1
From above table 1, add bridging property siloxanes organism, this long-chain organism can carry out crosslinking reaction with silicon-dioxide, be grafted to silica sphere, and it is again coated to wax wherein, close, make oil-absorption(number) be reduced to 102g/100g from 150g/100g, and documents is 271 g/100g.Simultaneously due to the suspension characteristic of its long-chain, anti-settling test is made to have original 25ml/70ml(3 days) bring up to 40ml/70ml(3 days).Density simultaneously due to product is light, is in use easily suspended on the surface, flatting efficiency is improved, and the glossiness that product originally adds 3.0% is 57 °, and the glossiness of modified product can reach 18 °.
Above-mentioned detailed description is illustrating for one of them possible embodiments of the present invention, and this embodiment is also not used to limit the scope of the claims of the present invention, and the equivalence that all the present invention of disengaging do is implemented or changed, and all should be contained in the scope of technical solution of the present invention.
Claims (7)
1. a preparation method for the low oil-absorption(number) flatting silica of high transparency, is characterized in that, the step of described preparation method is:
(1) acid adding: add acid in water glass, after forming gel, stop acid adding, be warming up to 48-52 DEG C immediately, adding acid for adjusting pH value is 4-5;
(2) fluoridize: add fluorine-containing organic modifiers, one or more simultaneously adding coupling agent carry out surface modification, and the reaction times is 55-65 minute;
(3) secondary capsulation: be warming up to 55-85 DEG C, add bridging property long-chain organism, and silicon-dioxide carries out crosslinking reaction, adds ethanol simultaneously, and reaction 1.5-2.5 hour, carries out secondary capsulation;
(4) wash, press filtration: slurry to be washed, press filtration;
(5) dry, pulverizing: finally drying and pulverizing are carried out to flatting silica.
2. the preparation method of the low oil-absorption(number) flatting silica of high transparency according to claim 1, is characterized in that, described fluorine-containing organic modifiers is one or more of tetrafluoroethylene wax, fluorine containing silane coupling agent and fluorine-containing cyclic silane.
3. the preparation method of the low oil-absorption(number) flatting silica of high transparency according to claim 1, is characterized in that, described in there is bridging property long-chain organism be long-chain siloxanes and with one or more of the molecular weight polymers of siloxane structure.
4. the preparation method of the low oil-absorption(number) flatting silica of high transparency according to claim 1, is characterized in that, described coupling agent is one or more in silane, Aluminate, titanic acid ester, polyethylene wax.
5. the preparation method of the low oil-absorption(number) flatting silica of high transparency according to claim 1, is characterized in that, described washing, press filtration make slurries specific conductivity be reduced to 300 below μ s/cm.
6. the preparation method of the low oil-absorption(number) flatting silica of high transparency according to claim 1, is characterized in that, described pulverizing gained flatting silica particle diameter is 4.0-6.0 μm, is preferably 4.0-5.0 μm.
7. the preparation method of the low oil-absorption(number) flatting silica of high transparency according to claim 1, is characterized in that, described acid comprises one or more of sulfuric acid, phosphoric acid and hydrofluoric acid.
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| CN201510037855.6A CN104530770B (en) | 2015-01-26 | 2015-01-26 | The preparation method of the low oil-absorption(number) flatting silica of a kind of high transparency |
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| CN201510037855.6A CN104530770B (en) | 2015-01-26 | 2015-01-26 | The preparation method of the low oil-absorption(number) flatting silica of a kind of high transparency |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108641463A (en) * | 2018-05-09 | 2018-10-12 | 冷水江三A新材料科技有限公司 | A kind of preparation method of UV showerings flatting silica |
| CN109535812A (en) * | 2018-12-05 | 2019-03-29 | 苏州锦艺新材料科技有限公司 | The preparation method and delustring filler of delustring filler |
| CN109704348A (en) * | 2019-02-21 | 2019-05-03 | 长沙凌玮新材料科技有限公司 | A kind of dedicated flatting silica of water paint and preparation method thereof |
| CN111543753A (en) * | 2020-06-05 | 2020-08-18 | 杭州天龙手袋股份有限公司 | Handbag with cowhide finishing layer |
| CN112175432A (en) * | 2020-10-16 | 2021-01-05 | 北京航天赛德科技发展有限公司 | Composite anticorrosive pigment and preparation method and application thereof |
| CN112251106A (en) * | 2020-10-16 | 2021-01-22 | 北京航天赛德科技发展有限公司 | Composite anticorrosive paint and application thereof |
| CN112251063A (en) * | 2020-10-16 | 2021-01-22 | 北京航天赛德科技发展有限公司 | Preparation method and application of composite anticorrosive paint |
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| CN102850913A (en) * | 2012-09-21 | 2013-01-02 | 广东大盈化工有限公司 | Preparation method of indoor flatting powder paint |
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2015
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| WO2003042293A1 (en) * | 2001-11-13 | 2003-05-22 | Ineos Silicas Limited | Silica matting agents |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108641463A (en) * | 2018-05-09 | 2018-10-12 | 冷水江三A新材料科技有限公司 | A kind of preparation method of UV showerings flatting silica |
| CN109535812A (en) * | 2018-12-05 | 2019-03-29 | 苏州锦艺新材料科技有限公司 | The preparation method and delustring filler of delustring filler |
| CN109704348A (en) * | 2019-02-21 | 2019-05-03 | 长沙凌玮新材料科技有限公司 | A kind of dedicated flatting silica of water paint and preparation method thereof |
| CN111543753A (en) * | 2020-06-05 | 2020-08-18 | 杭州天龙手袋股份有限公司 | Handbag with cowhide finishing layer |
| CN111543753B (en) * | 2020-06-05 | 2022-07-12 | 杭州天龙手袋股份有限公司 | Handbag with cowhide finishing layer |
| CN112175432A (en) * | 2020-10-16 | 2021-01-05 | 北京航天赛德科技发展有限公司 | Composite anticorrosive pigment and preparation method and application thereof |
| CN112251106A (en) * | 2020-10-16 | 2021-01-22 | 北京航天赛德科技发展有限公司 | Composite anticorrosive paint and application thereof |
| CN112251063A (en) * | 2020-10-16 | 2021-01-22 | 北京航天赛德科技发展有限公司 | Preparation method and application of composite anticorrosive paint |
| CN112251063B (en) * | 2020-10-16 | 2022-04-08 | 北京航天赛德科技发展有限公司 | Preparation method and application of composite anticorrosive paint |
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| CN104530770B (en) | 2016-03-30 |
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Denomination of invention: Preparation method of high-transparency low-oil-absorption-number matting powder Effective date of registration: 20170517 Granted publication date: 20160330 Pledgee: Guangdong Nanhai Rural Commercial Bank branch branch of Limited by Share Ltd. Pledgor: GUANGDONG HAISUN NEW MATERIAL TECHNOLOGY Co.,Ltd. Registration number: 2017440000023 |
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Denomination of invention: Preparation method of high-transparency low-oil-absorption-number matting powder Effective date of registration: 20200701 Granted publication date: 20160330 Pledgee: Shunde Guangdong rural commercial bank Limited by Share Ltd. Daliang branch Pledgor: GUANGDONG HAISUN NEW MATERIAL TECHNOLOGY Co.,Ltd. Registration number: Y2020980003703 |
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