CN109704348A - A kind of dedicated flatting silica of water paint and preparation method thereof - Google Patents
A kind of dedicated flatting silica of water paint and preparation method thereof Download PDFInfo
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- CN109704348A CN109704348A CN201910131137.3A CN201910131137A CN109704348A CN 109704348 A CN109704348 A CN 109704348A CN 201910131137 A CN201910131137 A CN 201910131137A CN 109704348 A CN109704348 A CN 109704348A
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Abstract
The invention discloses dedicated flatting silica of a kind of water paint and preparation method thereof, for preparation method the following steps are included: water, SiO 2 powder are added into reaction kettle, adjusting solution ph with waterglass I is 8~11；After mixing evenly, then into reaction kettle waterglass II and aqueous sulfuric acid is added, the time of cocurrent is 30~120min, and the temperature of cocurrent is 30~90 DEG C；Cocurrent after reaction, modified additive is added into reaction kettle；The pH value for adjusting solution in reaction kettle is 9,90 DEG C of 0.5~3h of aging again；The pH value for adjusting solution in reaction kettle is 2.5~3, then reacts 30min to get reaction product；Reaction product is filtered, is washed to 100 μ S of conductivity <, then up to the dedicated flatting silica of water paint after dry, pulverize at 100~200 DEG C.The compatibility of silica flatting silica and resin prepared by the present invention is stronger, enhances the water resistance and transparency of water paint paint film.
Description
Technical field
The invention belongs to technical field of coatings more particularly to a kind of dedicated flatting silica of water paint and preparation method thereof.
Background technique
Traditional oil paint contains a large amount of volatile organic solvent (VOC), and the discharge of a large amount of VOC not only makes environment
At huge destruction, the health of harmful to human is gone back.And water paint using environmentally protective water as solvent, can be significantly
Reduce the harm of organic volatile (VOC) to environment and human body in ground.
In recent years, environmental problem is more prominent, and haze weather becomes a part of daily life, therefore country puts into effect a system
The policy about environmental protection of column, a large amount of seriously polluted factories that varnish furniture shut down rectification because of environmental issue.Therefore, environmentally protective
Water paint replace the heavy-polluted oil paint of tradition that certainly will become a kind of trend.However, comparing oil paint, water paint
Also have certain disadvantages in performance: rate of drying is slower, and the patience of paint film is poor.
In the synthesis process due to water-base resin, in order to make resin compatible with water and form homogeneous water-base resin system,
A large amount of surfactant must not be added without；And these surfactants will be always present in water-based system in, in paint film
After drying, due to the presence of the extremely strong surfactant of these hydrophilies, the paint film water resistance of water paint greatly reduces.
Further, since most of water-base resins are to exist in the form of an emulsion, film curing is to be aided with emulsion particle by physics mode
Certain intermolecular force is attached, and lacks the effect of chemical bond, to keep the crosslink density of paint film lower, reduces paint
The patience of film.After water-base resin system is added in common silica flatting silica, due to poor with the compatibility of resin, dispersing
It is entrained between resin and resin again afterwards, so that just not strong enough intermolecular force becomes weaker originally, to more reduce
The crosslink density of paint film, declines paint film patience more.
Therefore, it needs to improve flatting silica in existing water paint, to provide good patience and transparency.
Summary of the invention
Present invention aims to overcome that the shortcomings of the prior art, and provide a kind of dedicated flatting silica of water paint and its
Preparation method, the present invention make silica flatting silica and resin by using special silica synthesis and modified technique
Compatibility it is stronger, improve the active force between silica and resin, enhance the crosslink density of paint film, to enhance aqueous
The water resistance of coating paint film, and due to more preferable with resin compatible, the transparency of paint film is also improved.
To achieve the above object, the technical scheme adopted by the invention is as follows: a kind of preparation side of the dedicated flatting silica of water paint
Method comprising following steps:
S1 water, SiO 2 powder) are added into reaction kettle, adjusting solution ph with waterglass I is 8~11；Stirring is equal
After even, then waterglass II and aqueous sulfuric acid are added into reaction kettle, the time of cocurrent is 30~120min, and the temperature of cocurrent is
30~90 DEG C；
S2) cocurrent after reaction, modified additive is added into reaction kettle；The pH value for adjusting solution in reaction kettle is 9,90
DEG C again 0.5~3h of aging；
S3 the pH value for) adjusting solution in reaction kettle is 2.5~3, then reacts 30min to get reaction product；
S4) reaction product is filtered, is washed to 100 μ S of conductivity <, then in 100~200 DEG C of dryings；It is dry
It is crushed afterwards until the partial size of reaction product is 2.5~6 μm to get the dedicated flatting silica of water paint；
Dioxide-containing silica >=99% of the dedicated flatting silica of water paint, BET specific surface area are 50~300m2/ g,
Pore volume is 0.2~1.8ml/g；
In step sl, if occurring gel in co-current process, stop cocurrent and stop that remaining waterglass II and sulphur is added
Aqueous acid, and close stirring and stand 30~90min；Again after stirring 30min, remaining water glass is added into reaction kettle
Glass II and aqueous sulfuric acid continue to start cocurrent；Period, the time for standing and stirring are not counted in the time of cocurrent.
As an improvement of the above technical solution, the mass percentage of silica is 8%~20% in the waterglass,
The mass percentage of sulfuric acid is 10%~50% in the aqueous sulfuric acid.
As an improvement of the above technical solution, in step sl, the SiO 2 powder by vapor phase method, the precipitation method or coagulates
Prepared by glue method, the partial size D50 of SiO 2 powder is 3~15 μm；Dioxy in the SiO 2 powder and waterglass II
The mass ratio of SiClx is 0.2%~1%.
It is further improved as above-mentioned technical proposal, the modified additive is at least KH550, span 20, sapn 21, department
One of disk 60, sapn 61, sorbester p17, sapn 81, polysorbas20, tween 21, polysorbate60, Tween61, Tween 80, sorbimacrogol oleate100,
The mass ratio of silica is 1%~10% in the modified additive and waterglass II.
It is further improved as above-mentioned technical proposal, the dedicated flatting silica of water paint includes following parts by weight
Raw material: 300~700 parts of water, 0.2~1 part of SiO 2 powder, II 500~1250 parts of waterglass, aqueous sulfuric acid 105~
525 parts and 1~10 part of modified additive.
It is further improved as above-mentioned technical proposal comprising following steps:
S1 700 parts of water) are added into reaction kettle, the precipitated silica powder that 1 part of partial size is 3 μm, are adjusted with waterglass I
Whole solution ph is 11；After mixing evenly, then into reaction kettle the waterglass II and 50% that silica concentration is 10% is added
Aqueous sulfuric acid, the time of cocurrent are 60min, and the temperature of cocurrent is 30 DEG C；During cocurrent, when gel to appear, stop cocurrent
And stop that remaining waterglass II and aqueous sulfuric acid is added, it closes and stirs and stand 60min；After stirring 30min again again, to
Remaining waterglass II and aqueous sulfuric acid are added in reaction kettle, continue to start cocurrent；The waterglass II being added in reaction kettle
It is 1000 parts, aqueous sulfuric acid is 105 parts；
S2) cocurrent after reaction, 2.5 parts of Tween 80s and 2.5 number sorbester p17s is added into reaction kettle；Sulfuric acid adjusts anti-
The pH value for answering solution in kettle is 9,90 DEG C of aging 3h again；
S3 it is 2.5 that) sulfuric acid, which adjusts the pH value of solution in reaction kettle, then reacts 30min to get reaction product；
S4) reaction product is filtered, is washed to 100 μ S of conductivity <, 100~200 DEG C of crushed after being dried are straight
Partial size to reaction product is 2.5~6 μm to get the dedicated flatting silica of water paint.
It is further improved as above-mentioned technical proposal comprising following steps:
S1 300 parts of water) are added into reaction kettle, the gel silica powder that 0.5 part of partial size is 5 μm, with waterglass I
Adjusting solution ph is 9；After mixing evenly, then into reaction kettle the waterglass II and 25% that silica concentration is 8% is added
Aqueous sulfuric acid, the time of cocurrent are 30min, and the temperature of cocurrent is 50 DEG C；During cocurrent, when gel to appear, stop cocurrent
And stop that remaining waterglass II and aqueous sulfuric acid is added, it closes and stirs and stand 90min；After stirring 30min again again, to
Remaining waterglass II and aqueous sulfuric acid are added in reaction kettle, continue to start cocurrent；The waterglass II being added in reaction kettle
It is 1250 parts, aqueous sulfuric acid is 210 parts；
S2) cocurrent after reaction, 5 parts of polysorbate60s and 5 parts of sorbester p18s is added into reaction kettle；Sulfuric acid is adjusted in reaction kettle
The pH value of solution is 9,90 DEG C of aging 2h again；
S3 it is 3 that) sulfuric acid, which adjusts the pH value of solution in reaction kettle, then reacts 30min to get reaction product；
S4 washing) is filtered to 100 μ S of conductivity < to the reaction product, 100~200 DEG C of crushed after being dried until
The partial size of reaction product is 2.5~6 μm to get the dedicated flatting silica of water paint.
In addition, the present invention also provides a kind of dedicated flatting silicas of water paint prepared using the preparation method.
In addition, the present invention also provides the dedicated flatting silicas of the water paint to prepare the application in water paint.
The beneficial effects of the present invention are: the present invention to provide a kind of dedicated flatting silica of water paint and preparation method thereof, this
Invention is by using special synthesis technology: 1) phase addition SiO 2 powder controls silica as crystal seed before the reaction
The growth of particle；2) further surface is carried out to silica surface using special modified additive in the ageing step to be modified,
Improve the active force between silica and resin；This will increase the crosslink density of paint film, micro- after reduction later period paint film is dry
The generation of crackle；Allowing silica, easily dispersion, anti-settling property are good in water-based system, and paint film has the transparency good and with water-fast
Property and scratch resistance energy.
Specific embodiment
Purposes, technical schemes and advantages in order to better illustrate the present invention, below in conjunction with specific embodiment to the present invention
It is described further.
It should be noted that waterglass I and waterglass II are intended merely to same type of information area each other in the present invention
It separates.
Embodiment 1
The present embodiment provides a kind of preparation methods of the dedicated flatting silica of water paint comprising following steps:
S1 700 parts of water) are added into reaction kettle, the precipitated silica powder that 1 part of partial size is 3 μm, are adjusted with waterglass I
Whole solution ph is 11；After mixing evenly, then into reaction kettle the waterglass II and 50% that silica concentration is 10% is added
Aqueous sulfuric acid, the time of cocurrent are 60min, and the temperature of cocurrent is 30 DEG C；During cocurrent, when gel to appear, stop cocurrent
And stop that remaining waterglass II and aqueous sulfuric acid is added, it closes and stirs and stand 60min；After stirring 30min again again, to
Remaining waterglass II and aqueous sulfuric acid are added in reaction kettle, continue to start cocurrent；The waterglass II being added in reaction kettle
It is 1000 parts, aqueous sulfuric acid is 105 parts；
S2) cocurrent after reaction, 2.5 parts of Tween 80s and 2.5 parts of sorbester p17s is added into reaction kettle；Sulfuric acid adjusts reaction
The pH value of solution is 9,90 DEG C of aging 3h again in kettle；
S3 it is 2.5 that) sulfuric acid, which adjusts the pH value of solution in reaction kettle, then reacts 30min to get reaction product；
S4) reaction product is filtered, is washed to 100 μ S of conductivity <, 100~200 DEG C of crushed after being dried are until anti-
The partial size for answering product is 2.5~6 μm to get the dedicated flatting silica of water paint.
Physical and chemical performance test is carried out to 5 batch flatting silicas of preparation, physical and chemical performance is as shown in table 1.
Table 1
| Number index | Dioxide-containing silica % | Hole holds ml/g | Specific surface area m2/g |
| Embodiment 1-1 | 99% | 1.61 | 232 |
| Embodiment 1-2 | 99% | 1.64 | 242 |
| Embodiment 1-3 | 99% | 1.62 | 228 |
| Embodiment 1-4 | 99% | 1.59 | 233 |
| Embodiment 1-5 | 99% | 1.65 | 238 |
Embodiment 2
The present embodiment provides a kind of preparation methods of the dedicated flatting silica of water paint comprising following steps:
S1 500 parts of water) are added into reaction kettle, the fumed silica powder that 0.2 part of partial size is 15 μm, use waterglass
I adjustment solution ph is 8；After mixing evenly, then into reaction kettle II He of waterglass that silica concentration is 10% is added
25% aqueous sulfuric acid, the time of cocurrent are 90min, and the temperature of cocurrent is 90 DEG C；During cocurrent, when gel to appear, stop
Remaining waterglass II and aqueous sulfuric acid is added in cocurrent and stopping, closing stirring and simultaneously stands 30min；Stir 30min again again
Afterwards, remaining waterglass II and aqueous sulfuric acid are added into reaction kettle, continue to start cocurrent；The water glass being added in reaction kettle
Glass II is 1000 parts, and aqueous sulfuric acid is 210 parts；
S2) cocurrent after reaction, 5 parts of polysorbas20s and 5 parts of span 20s is added into reaction kettle；Caustic soda is adjusted in reaction kettle
The pH value of solution is 9,90 DEG C of aging 0.5h again；
S3 it is 3 that) sulfuric acid, which adjusts the pH value of solution in reaction kettle, then reacts 30min to get reaction product；
S4) reaction product is filtered, is washed to 100 μ S of conductivity <, 100~200 DEG C of crushed after being dried are until anti-
The partial size for answering product is 2.5~6 μm to get the dedicated flatting silica of water paint.
Physical and chemical performance test is carried out to 5 batch flatting silicas of preparation, physical and chemical performance is as shown in table 2.
Table 2
| Number index | Dioxide-containing silica % | Hole holds ml/g | Specific surface area m2/g |
| Embodiment 2-1 | 99% | 0.31 | 58 |
| Embodiment 2-2 | 99% | 0.35 | 55 |
| Embodiment 2-3 | 99% | 0.28 | 64 |
| Embodiment 2-4 | 99% | 0.35 | 62 |
| Embodiment 2-5 | 99% | 0.29 | 68 |
Embodiment 3
The present embodiment provides a kind of preparation methods of the dedicated flatting silica of water paint comprising following steps:
S1 300 parts of water) are added into reaction kettle, the gel silica powder that 0.5 part of partial size is 5 μm, with waterglass I
Adjusting solution ph is 9；After mixing evenly, then into reaction kettle the waterglass II and 25% that silica concentration is 8% is added
Aqueous sulfuric acid, the time of cocurrent are 30min, and the temperature of cocurrent is 50 DEG C；During cocurrent, when gel to appear, stop cocurrent
And stop that remaining waterglass II and aqueous sulfuric acid is added, it closes and stirs and stand 90min；After stirring 30min again again, to
Remaining waterglass II and aqueous sulfuric acid are added in reaction kettle, continue to start cocurrent；The waterglass II being added in reaction kettle
It is 1250 parts, aqueous sulfuric acid is 210 parts；
S2) cocurrent after reaction, 5 parts of polysorbate60s and 5 parts of sorbester p18s is added into reaction kettle；Sulfuric acid is adjusted in reaction kettle
The pH value of solution is 9,90 DEG C of aging 2h again；
S3 it is 3 that) sulfuric acid, which adjusts the pH value of solution in reaction kettle, then reacts 30min to get reaction product；
S4) reaction product is filtered, is washed to 100 μ S of conductivity <, 100~200 DEG C of crushed after being dried are until anti-
The partial size for answering product is 2.5~6 μm to get the dedicated flatting silica of water paint.
Physical and chemical performance test is carried out to 5 batch flatting silicas of preparation, physical and chemical performance is as shown in table 3.
Table 3
| Number index | Dioxide-containing silica % | Hole holds ml/g | Specific surface area m2/g |
| Embodiment 3-1 | 99% | 1.33 | 185 |
| Embodiment 3-2 | 99% | 1.38 | 178 |
| Embodiment 3-3 | 99% | 1.25 | 187 |
| Embodiment 3-4 | 99% | 1.32 | 183 |
| Embodiment 3-5 | 99% | 1.30 | 188 |
Embodiment 4
The present embodiment provides a kind of preparation methods of the dedicated flatting silica of water paint comprising following steps:
S1 700 parts of water) are added into reaction kettle, the fumed silica powder that 1 part of partial size is 3 μm, are adjusted with waterglass I
Whole solution ph is 11；After mixing evenly, then into reaction kettle the waterglass II and 10% that silica concentration is 20% is added
Aqueous sulfuric acid, the time of cocurrent are 60min, and the temperature of cocurrent is 90 DEG C；During cocurrent, when gel to appear, stop cocurrent
And stop that remaining waterglass II and aqueous sulfuric acid is added, it closes and stirs and stand 30min；After stirring 30min again again, to
Remaining waterglass II and aqueous sulfuric acid are added in reaction kettle, continue to start cocurrent；The waterglass II being added in reaction kettle
It is 500 parts, aqueous sulfuric acid is 525 parts；
S2) cocurrent after reaction, 0.5 part of KH550,2.5 parts of sapn 21 and 2.5 part tweens 21 is added into reaction kettle；
The pH value that sulfuric acid adjusts solution in reaction kettle is 9,90 DEG C of aging 3h again；
S3 it is 3 that) sulfuric acid, which adjusts the pH value of solution in reaction kettle, then reacts 30min to get reaction product；
S4) reaction product is filtered, is washed to 100 μ S of conductivity <, 100~200 DEG C of crushed after being dried are until anti-
The partial size for answering product is 2.5~6 μm to get the dedicated flatting silica of water paint.
Physical and chemical performance test is carried out to 5 batch flatting silicas of preparation, physical and chemical performance is as shown in table 4.
Table 4
| Number index | Dioxide-containing silica % | Hole holds ml/g | Specific surface area m2/g |
| Embodiment 4-1 | 99% | 0.65 | 109 |
| Embodiment 4-2 | 99% | 0.69 | 112 |
| Embodiment 4-3 | 99% | 0.68 | 115 |
| Embodiment 4-4 | 99% | 0.65 | 113 |
| Embodiment 4-5 | 99% | 0.61 | 107 |
Embodiment 5
The present embodiment provides a kind of preparation methods of the dedicated flatting silica of water paint comprising following steps:
S1 700 parts of water) are added into reaction kettle, the fumed silica powder that 1 part of partial size is 15 μm, with waterglass I
Adjusting solution ph is 11；After mixing evenly, then into reaction kettle II He of waterglass that silica concentration is 20% is added
10% aqueous sulfuric acid, the time of cocurrent are 60min, and the temperature of cocurrent is 90 DEG C；During cocurrent, when gel to appear, stop
Remaining waterglass II and aqueous sulfuric acid is added in cocurrent and stopping, closing stirring and simultaneously stands 30min；Stir 30min again again
Afterwards, remaining waterglass II and aqueous sulfuric acid are added into reaction kettle, continue to start cocurrent；The water glass being added in reaction kettle
Glass II is 500 parts, and aqueous sulfuric acid is 525 parts；
S2) cocurrent after reaction, 2.5 parts of sapn 61 and 2.5 part tweens 21 is added into reaction kettle；Sulfuric acid adjusts reaction
The pH value of solution is 9,90 DEG C of aging 3h again in kettle；
S3 it is 3 that) sulfuric acid, which adjusts the pH value of solution in reaction kettle, then reacts 30min to get reaction product；
S4) reaction product is filtered, is washed to 100 μ S of conductivity <, 100~200 DEG C of crushed after being dried are until anti-
The partial size for answering product is 2.5~6 μm to get the dedicated flatting silica of water paint.
Physical and chemical performance test is carried out to 5 batch flatting silicas of preparation, physical and chemical performance is as shown in table 5.
Table 5
| Number index | Dioxide-containing silica % | Hole holds ml/g | Specific surface area m2/g |
| Embodiment 5-1 | 99% | 0.58 | 94 |
| Embodiment 5-2 | 99% | 0.56 | 92 |
| Embodiment 5-3 | 99% | 0.62 | 99 |
| Embodiment 5-4 | 99% | 0.55 | 94 |
| Embodiment 5-5 | 99% | 0.54 | 95 |
Embodiment 6
The present embodiment provides a kind of preparation methods of the dedicated flatting silica of water paint comprising following steps:
S1 700 parts of water) are added into reaction kettle, the gel silica powder that 1 part of partial size is 3 μm, are adjusted with waterglass I
Whole solution ph is 10；After mixing evenly, then into reaction kettle the waterglass II and 10% that silica concentration is 20% is added
Aqueous sulfuric acid, the time of cocurrent are 90min, and the temperature of cocurrent is 70 DEG C；During cocurrent, when gel to appear, stop cocurrent
And stop that remaining waterglass II and aqueous sulfuric acid is added, it closes and stirs and stand 30min；After stirring 30min again again, to
Remaining waterglass II and aqueous sulfuric acid are added in reaction kettle, continue to start cocurrent；The waterglass II being added in reaction kettle
It is 500 parts, aqueous sulfuric acid is 525 parts；
S2) cocurrent after reaction, 2.5 parts of sapn 81 and 2.5 part sorbimacrogol oleate100s is added into reaction kettle；Sulfuric acid adjusts reaction
The pH value of solution is 9,90 DEG C of aging 3h again in kettle；
S3 it is 3 that) sulfuric acid, which adjusts the pH value of solution in reaction kettle, then reacts 30min to get reaction product；
S4) reaction product is filtered, is washed to 100 μ S of conductivity <, 100~200 DEG C of crushed after being dried are until anti-
The partial size for answering product is 2.5~6 μm to get the dedicated flatting silica of water paint.
Physical and chemical performance test is carried out to 5 batch flatting silicas of preparation, physical and chemical performance is as shown in table 6.
Table 6
| Number index | Dioxide-containing silica % | Hole holds ml/g | Specific surface area m2/g |
| Embodiment 6-1 | 99% | 0.88 | 148 |
| Embodiment 6-2 | 99% | 0.84 | 139 |
| Embodiment 6-3 | 99% | 0.89 | 144 |
| Embodiment 6-4 | 99% | 0.83 | 140 |
| Embodiment 6-5 | 99% | 0.90 | 152 |
Embodiment 7
The present embodiment provides a kind of preparation methods of the dedicated flatting silica of water paint comprising following steps:
S1 700 parts of water) are added into reaction kettle, the gel silica powder that 1 part of partial size is 3 μm, are adjusted with waterglass I
Whole solution ph is 10；After mixing evenly, then into reaction kettle the waterglass II and 10% that silica concentration is 20% is added
Aqueous sulfuric acid, the time of cocurrent are 120min, and the temperature of cocurrent is 70 DEG C；During cocurrent, when gel to appear, stop cocurrent
And stop that remaining waterglass II and aqueous sulfuric acid is added, it closes and stirs and stand 90min；After stirring 30min again again, to
Remaining waterglass II and aqueous sulfuric acid are added in reaction kettle, continue to start cocurrent；The waterglass II being added in reaction kettle
It is 500 parts, aqueous sulfuric acid is 525 parts；
S2) cocurrent after reaction, 0.5 part of sapn 81 and 0.5 part sorbimacrogol oleate100 is added into reaction kettle；Sulfuric acid adjusts reaction
The pH value of solution is 9,90 DEG C of aging 3h again in kettle；
S3 it is 2.8 that) sulfuric acid, which adjusts the pH value of solution in reaction kettle, then reacts 30min to get reaction product；
S4 washing) is filtered to 100 μ S of conductivity < to reaction product, 100~200 DEG C of crushed after being dried are until reaction
The partial size of product is 2.5~6 μm to get the dedicated flatting silica of water paint.
Physical and chemical performance test is carried out to 5 batch flatting silicas of preparation, physical and chemical performance is as shown in table 7.
Table 7
The application performance of flatting silica product
1) preparation of aqueous wooden ware one-component matte varnish sample, formula are shown in Table 8；
Table 8
2) preparation process: after mixing by XK-14 and E-129, BYK346, SN5040 is added, disperses 5 minutes；It will disappear
Light powder sample is slowly added into mixed liquor, high speed dispersion 20 minutes, tests fineness < 35 μm；Speed is reduced, will be diluted with water
Even BYK024 is slowly added into, and is dispersed 10 minutes；It after DPM, DPnB are diluted with water, is slowly added into, moderate-speed mixer 5 minutes；Successively
D1293, TEGO-450, Drewslip738, BYK513 is added, every kind of auxiliary agent disperses to add lower one kind again in 5 minutes after being added；It will
It after DSX2000 and DSX3290 is diluted with water, is slowly added in scattered mixed liquor, stirring filters and packages for 10 minutes；Respectively
By the one-component matte varnish sample of the above formula and technique preparation embodiment 1-6 flatting silica.
3) preparation of specimen: according to the method for GB/T1727-1992 by construction in the tinplate sheet for meet GB9271-88
It one of standard spray finishing coat, uses 400 mesh waterproof abrasive papers to carry out wet-milling after 24 hours dry, is marked after air drying 168h according to corresponding
Standard is tested.After the dry 30min of 50 ± 2 DEG C of bakings, second paint is sprayed, control total film thickness is 40 ± 2 μm and (uses GB1764
Non-destructive method is tested), use paraffin: rosin=1:1 mixture carries out edge sealing.After paint film is 168 hours dry
It is tested.
4) test of paint film property
Testing standard
Gloss: " 20 °, 60 °, the 85 ° of bright lusters of paint and varnish, colored paint paint film without metallic pigments of GB/T 9754
Measurement " using the test of 60 ° of angles；Hardness: it is carried out by GB/T 6739-2006 " paint and varnish pencil method measures hardness of paint film "
Test；Water resistance: it is impregnated 24 hours in the normal-temperature distilled water of first method in GB/T 1733-93 " paint film water resistance measuring method ", second method
It impregnates 15 minutes in 100 DEG C of boiling water, grades by standard GB/T1766-2008；Resistance to marring: GB/T 9279-1988 is pressed
" paint and varnish scratch experiment " carries out the test resistance to needle of film using film scratch tester firm demand and draws permeability energy.Specifically comment
Grade standard is as follows:
0 grade: being tested with the load of 300g, there is obvious scratch；1 grade: being tested with 350g load, without obvious scratch
Or only shadow scratch, it is tested with 400g load, there is obvious scratch；2 grades: being tested with 400g load, drawn without obvious
Trace or only shadow scratch have obvious scratch with 450g Road test；3 grades: tested with 500g load, without obvious scratch or
Only shadow scratch；Test result is shown in Table 9.
Table 9
As shown in table 9, when being used to prepare coating using flatting silica prepared by the embodiment of the present invention 1~7, paint film has transparent
Water resistance and scratch resistance energy are got well and had to property.
Finally, it should be noted that above embodiments protect the present invention to illustrate technical solution of the present invention
The limitation of range, although the invention is described in detail with reference to the preferred embodiments, those skilled in the art should be managed
Solution, can modify to technical solution of the present invention or replace on an equal basis, without departing from technical solution of the present invention essence and
Range.
Claims (9)
1. a kind of preparation method of the dedicated flatting silica of water paint, spy are, comprising the following steps:
S1 water, SiO 2 powder) are added into reaction kettle, adjusting solution ph with waterglass I is 8~11；After mixing evenly,
It is added waterglass II and aqueous sulfuric acid into reaction kettle again, the time of cocurrent is 30~120min, the temperature of cocurrent is 30~
90℃；
S2) cocurrent after reaction, modified additive is added into reaction kettle；Adjust reaction kettle in solution pH value be 9,90 DEG C again
0.5~3h of aging；
S3 the pH value for) adjusting solution in reaction kettle is 2.5~3, then reacts 30min to get reaction product；
S4) reaction product is filtered, is washed to 100 μ S of conductivity <, then in 100~200 DEG C of dryings；Powder after drying
It is broken until reaction product partial size be 2.5~6 μm to get the dedicated flatting silica of water paint；
Dioxide-containing silica >=99% of the dedicated flatting silica of water paint, BET specific surface area are 50~300m2/ g, pore-body
Product is 0.2~1.8ml/g；
In step sl, if occurring gel in co-current process, stop cocurrent and stop that remaining waterglass II and sulfuric acid water is added
Solution, and close stirring and stand 30~90min；Again after stirring 30min, remaining waterglass II is added into reaction kettle
And aqueous sulfuric acid, continue to start cocurrent；Period, the time for standing and stirring are not counted in the time of cocurrent.
2. preparation method as described in claim 1, which is characterized in that the mass percentage of silica in the waterglass
It is 8%~20%, the mass percentage of sulfuric acid is 10%~50% in the aqueous sulfuric acid.
3. preparation method as described in claim 1, which is characterized in that in step sl, the SiO 2 powder is by gas phase
Prepared by method, the precipitation method or gel method, the partial size D50 of SiO 2 powder is 3~15 μm；The SiO 2 powder and water
The mass ratio of silica is 0.2%~1% in glass II.
4. preparation method as claimed in claim 3, which is characterized in that the modified additive is at least KH550, span 20, department
Disk 21, sorbester p18, sapn 61, sorbester p17, sapn 81, polysorbas20, tween 21, polysorbate60, Tween61, Tween 80, in sorbimacrogol oleate100
One kind, the mass ratio of silica is 1%~10% in the modified additive and waterglass II.
5. preparation method as claimed in claim 4, which is characterized in that the dedicated flatting silica of water paint includes following weight
The raw material of number: 300~700 parts of water, 0.2~1 part of SiO 2 powder, II 500~1250 parts of waterglass, aqueous sulfuric acid
105~525 parts and 1~10 part of modified additive.
6. preparation method as claimed in claim 5, which comprises the following steps:
S1 700 parts of water) are added into reaction kettle, the precipitated silica powder that 1 part of partial size is 3 μm, are adjusted with waterglass I molten
Liquid pH value is 11；After mixing evenly, then into reaction kettle the waterglass II and 50% sulfuric acid that silica concentration is 10% is added
Aqueous solution, the time of cocurrent are 60min, and the temperature of cocurrent is 30 DEG C；During cocurrent, when gel to appear, stops cocurrent and stop
Remaining waterglass II and aqueous sulfuric acid is only added, closes and stirs and stand 60min；After stirring 30min again again, Xiang Fanying
Remaining waterglass II and aqueous sulfuric acid are added in kettle, continue to start cocurrent；The waterglass II being added in reaction kettle is
1000 parts, aqueous sulfuric acid is 105 parts；
S2) cocurrent after reaction, 2.5 parts of Tween 80s and 2.5 number sorbester p17s is added into reaction kettle；Sulfuric acid adjusts reaction kettle
The pH value of interior solution is 9,90 DEG C of aging 3h again；
S3 it is 2.5 that) sulfuric acid, which adjusts the pH value of solution in reaction kettle, then reacts 30min to get reaction product；
S4) reaction product is filtered, is washed to 100 μ S of conductivity <, 100~200 DEG C of crushed after being dried are until anti-
The partial size for answering product is 2.5~6 μm to get the dedicated flatting silica of water paint.
7. preparation method as claimed in claim 5, which comprises the following steps:
S1 300 parts of water) are added into reaction kettle, the gel silica powder that 0.5 part of partial size is 5 μm, are adjusted with waterglass I
Solution ph is 9；After mixing evenly, then into reaction kettle the waterglass II and 25% sulfuric acid that silica concentration is 8% is added
Aqueous solution, the time of cocurrent are 30min, and the temperature of cocurrent is 50 DEG C；During cocurrent, when gel to appear, stops cocurrent and stop
Remaining waterglass II and aqueous sulfuric acid is only added, closes and stirs and stand 90min；After stirring 30min again again, Xiang Fanying
Remaining waterglass II and aqueous sulfuric acid are added in kettle, continue to start cocurrent；The waterglass II being added in reaction kettle is
1250 parts, aqueous sulfuric acid is 210 parts；
S2) cocurrent after reaction, 5 parts of polysorbate60s and 5 parts of sorbester p18s is added into reaction kettle；Sulfuric acid adjusts solution in reaction kettle
PH value be 9,90 DEG C of aging 2h again；
S3 it is 3 that) sulfuric acid, which adjusts the pH value of solution in reaction kettle, then reacts 30min to get reaction product；
S4) reaction product is filtered, is washed to 100 μ S of conductivity <, 100~200 DEG C of crushed after being dried are until anti-
The partial size for answering product is 2.5~6 μm to get the dedicated flatting silica of water paint.
8. a kind of dedicated flatting silica of water paint prepared using preparation method as described in any one of claims 1 to 7.
9. the dedicated flatting silica of water paint as claimed in claim 8 is preparing the application in water paint.
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| CN110591416A (en) * | 2019-08-23 | 2019-12-20 | 广州凌玮科技股份有限公司 | Preparation method of amorphous silicon dioxide antirust pigment |
| CN110628256A (en) * | 2019-08-23 | 2019-12-31 | 广州凌玮科技股份有限公司 | Preparation method of amorphous silicon dioxide antirust pigment |
| CN112960677B (en) * | 2021-04-01 | 2021-10-26 | 广州市飞雪材料科技有限公司 | Precipitation method for preparing oral silicon dioxide with high oil absorption value and low viscosity |
| CN115403955A (en) * | 2022-11-03 | 2022-11-29 | 广州凌玮科技股份有限公司 | Special matting powder for high-matting-property UV (ultraviolet) photocureable coating and preparation method thereof |
| CN115974090A (en) * | 2023-03-17 | 2023-04-18 | 广州凌玮科技股份有限公司 | Preparation method of silica for weak solvent ink-jet printing coating |
| CN116396650A (en) * | 2023-02-21 | 2023-07-07 | 吉安天晟新材料有限公司 | Ink-absorbing coating |
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| CN112960677B (en) * | 2021-04-01 | 2021-10-26 | 广州市飞雪材料科技有限公司 | Precipitation method for preparing oral silicon dioxide with high oil absorption value and low viscosity |
| CN115403955A (en) * | 2022-11-03 | 2022-11-29 | 广州凌玮科技股份有限公司 | Special matting powder for high-matting-property UV (ultraviolet) photocureable coating and preparation method thereof |
| CN116396650A (en) * | 2023-02-21 | 2023-07-07 | 吉安天晟新材料有限公司 | Ink-absorbing coating |
| CN115974090A (en) * | 2023-03-17 | 2023-04-18 | 广州凌玮科技股份有限公司 | Preparation method of silica for weak solvent ink-jet printing coating |
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Application publication date: 20190503 |