CN109735153A - A kind of preparation method of calcium ion-exchanged silica rust resisting pigment - Google Patents
A kind of preparation method of calcium ion-exchanged silica rust resisting pigment Download PDFInfo
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Abstract
The invention discloses a kind of preparation methods of calcium ion-exchanged silica rust resisting pigment, comprising the following steps: S1. ingredient: preparing the water glass solution that dioxide-containing silica is 10~20wt%, compound concentration is the sulfuric acid solution of 30~90wt%；S2. it synthesizes: water being added into reaction kettle, adjustment system pH is 1~4, is stirred evenly；The pH value of mixed solution is adjusted to 7, calcium ion-exchanged agent, and ion exchange 1~8 hour at 90 DEG C is then added；S3. then regulation system pH value is added organic-silicon-modified auxiliary agent, reacts 0.5~3 hour to 2.5.The preparation method of calcium ion-exchanged silica rust resisting pigment of the present invention is easy to operate, equipment requirement is low, high production efficiency, and the compatibility of silica and resin can be promoted by the organic hydrophobic modified processing in surface, improve the consistency of paint film, the infiltration for reducing paint film moisture content, further improves rustless property.
Description
Technical field
The invention belongs to chemical industry rust resisting pigment technical fields, and in particular to a kind of calcium ion-exchanged silica rust resisting pigment
Preparation method.
Background technique
The whole world is annual because the steel amount of loss caused by getting rusty has accounted for a quarter of annual output according to statistics, therefore how
Steel is protected, loss caused by reducing due to getting rusty becomes an important topic.Most common method is to metal
Surface carry out surface covering preservative treatment, prevent metal surface in air moisture content and oxygen directly contact, in this external coating
Rust resisting pigment can play deeper anti-corrosion effect.Traditional rust resisting pigment has red lead, lead powder, chromate etc., but this
Class rust resisting pigment generally has stronger murder by poisoning, pollutes environment and is detrimental to health.With the process of environmental protection legislation, Hen Duoguo
Family, which has begun, to be forbidden using such rust resisting pigment.
Current more commonly used non-poisonous antirust pigment is broadly divided into two kinds, physics rust resisting pigment and chemical anti-rust pigment.Object
Reason rust resisting pigment mainly has iron oxide red, mica powder, glass flake, stainless steel flakes etc..The rust-proof mechanism of such rust resisting pigment
It is to form one layer of fine and close protective layer in metal surface, but the rustless property of such rust resisting pigment is general using its chemical inertness.
Chemical anti-rust pigment mainly has phosphate rust resisting pigment, borate rust resisting pigment etc..The mechanism of action of such rust resisting pigment is main
To be had an effect with metal using its chemical property, form one layer of fine and close passivating film in metal surface prevent metal into
The corrosion of one step.But due to its slightly solubility, rustless property is also not good enough.In addition, there are also be concerned in recent years it is novel from
Sub- crossover rust resisting pigment, wherein calcium ion-exchanged silica non-poisonous antirust pigment be exactly meet the tendency of in this case and
It is raw, have many advantages, such as without heavy metal, nontoxic and pollution-free, efficient, synergistic effect is good.
Silica is a kind of high activity adsorbent material, and strong adsorption can adsorb many kinds of substance, has open porous knot
Structure, silica form different microcellular structures because of the difference of preparation method.Calcium ion-exchanged silica pigment and corruption
The anticorrosion mechanism for losing pigment is completely different, when aggressive electrolyte enters film by external environment, hands over first with calcium ion
Change silica pigment reaction, corrosive ion is trapped within silica surface, be adsorbed on the calcium of silica surface from
Exchange interaction occurs for son, releases the calcium ion with anticorrosive property, and the anticorrosion calcium ion layer of formation is deposited in metal and applies
On the interface of both layers, barrier action is played, isolates ground with external environment, while enhancing the adhesive force of coating again.
Calcium ion-exchanged silica pigment has the advantages that following uniqueness: discharging calcium ion by " need ", effectively and adequately utilizes
Pigment, silica do not dissolve in the coating, occur in the exchange reaction of Oxide-supports to be molecular level, to face
Material form has no influence, therefore coating can be made muchly to keep complete.
Preparation method as referred to calcium ion-exchanged type aluminosilicate rust resisting pigment in Chinese patent CN102391698A.
But the whole process reaction step of this patent is complicated, the operating time is long, and equipment requirement is high, affects production efficiency.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation methods of calcium ion-exchanged silica rust resisting pigment.Operation
Simply, equipment requirement is low, high production efficiency, when obtained rust resisting pigment is applied to resin paint film, significantly improves rust resisting pigment
With the active force between resin paint film, increase the crosslink density of paint film, reduces infiltration of the moisture content to paint film.
The present invention also provides the antirusts that the preparation method by above-mentioned calcium ion-exchanged silica rust resisting pigment is prepared
Pigment.
To achieve the above object, The technical solution adopted by the invention is as follows:
A kind of preparation method of calcium ion-exchanged silica rust resisting pigment, comprising the following steps:
S1. ingredient: preparing the water glass solution that dioxide-containing silica is 10~20wt%, and compound concentration is 30~90wt%
Sulfuric acid solution；
S2. it synthesizes: water being added into reaction kettle, adjustment system pH is 1~4, is stirred evenly；The waterglass that S1 is prepared
Cocurrent is added in reaction kettle simultaneously for solution and sulfuric acid solution, and cocurrent total time is 30~120 minutes, and cocurrent temperature is 30~90
℃；The pH value of mixed solution is adjusted after cocurrent to 6~8, calcium ion-exchanged agent is then added, and at 80~100 DEG C from
Son exchange 1~8 hour；
S3. then regulation system pH value is added organic-silicon-modified auxiliary agent, reacts 0.5~3 hour to 2~4；
S4. reaction product is filtered washing, then dry, pulverize.
Calcium ion-exchanged amount is to influence the main index of calcium ion-exchanged silica rust resisting pigment antiseptic property.This hair
Bright to carry out calcium ion-exchanged to it in the synthesis process of silica by the way of synthetic silica, inventor analyzes
In synthesis technology when the type and content, the pH value of reaction of each factor such as silica, calcium ion source, reaction temperature and reaction
Between equal hole configurations and calcium ion-exchanged amount to silica influence, determine optimal synthetic technological condition.The two of synthesis
Silica has microcellular structure abundant, and large specific surface area, surface hydroxyl quantity is more, and improve calcium ion and hydroxyl exchanges speed
Degree and exchange capacity, make the exchange capacity of calcium ion reach maximum value, improve the rustless property of production efficiency and product.Furthermore lead to again
It is modified to silica progress surface hydrophobicity to cross organic-silicon-modified auxiliary agent, dioxy is improved by the organic hydrophobic modified processing in surface
The compatibility of SiClx and resin improves the consistency of resin paint film, reduces the infiltration of paint film moisture content, further improves rust-preventing characteristic
Energy.
Preferably, the preparation method of the calcium ion-exchanged silica rust resisting pigment, comprising the following steps:
S1. ingredient: preparing the water glass solution that dioxide-containing silica is 15wt%, and compound concentration is that the sulfuric acid of 45wt% is molten
Liquid；
S2. it synthesizes: water being added into reaction kettle, adjustment system pH is 2, is stirred evenly；The waterglass that S1 is prepared is molten
Cocurrent is added in reaction kettle simultaneously for liquid and sulfuric acid solution, and cocurrent total time is 60 minutes, and cocurrent temperature is 30 DEG C；After cocurrent
Then calcium ion-exchanged agent, and ion exchange 8 hours at 90 DEG C are added to 7 in the pH value for adjusting mixed solution with sodium hydroxide；
S3. then regulation system pH value is added organic-silicon-modified auxiliary agent, reacts 3 hours to 2.5；
S4. reaction product is filtered washing, then dry, pulverize.
Preferably, the calcium ion-exchanged agent, organic-silicon-modified auxiliary agent mass ratio be 10-13:1.Inventor is continuous
It was found that, when calcium ion-exchanged agent, organic-silicon-modified auxiliary agent mass ratio within the scope of 10-13:1 when, it is ensured that calcium
Ion exchange silica rust resisting pigment can possess good hole, excellent adsorption, and significantly improve silica and resin
Active force between paint film.The hole adsorptivity that will affect silica when organic-silicon-modified auxiliary dosage is excessive, dosage are too small
The active force between silica and resin paint film cannot then be enhanced.
Preferably, the calcium ion-exchanged agent being added in S2 is calcium hydroxide, calcium oxide, clarification limewash, calcium nitrate, chlorine
Change one of calcium or a variety of.
It is further preferred that the calcium ion-exchanged agent being added is calcium hydroxide and calcium nitrate, mass ratio 1:0.5-1.
Silica and solution containing calcium ion react, and the number of the calcium ion in solution directly influences the effect of reaction.
Inventor is continuous it was found that, the solubility due to calcium hydroxide is lower, if only using calcium hydroxide solution, solution
The content of middle calcium ion would not be too high, therefore, suitable calcium nitrate solution is added, and can greatly improve calcium ion in solution
Content, reaction balance can be made mobile to the direction for being conducive to increase calcium ion-exchanged amount.
Preferably, the organic-silicon-modified auxiliary agent being added in S3 be phenyltrimethoxysila,e, phenyl triethoxysilane,
One of aminomethyl phenyl dimethoxysilane, aminomethyl phenyl diethoxy silane are a variety of.
It is further preferred that the organic-silicon-modified auxiliary agent being added in S3 is phenyltrimethoxysila,e and aminomethyl phenyl two
Methoxy silane.
Preferably, S4 is then dry in 100~150 DEG C by filter cake by reaction product filtration washing to 50 μ S/cm of conductivity <
It is dry, it is crushed to 2~4 μm.
Compared with prior art, beneficial effects of the present invention:
The preparation method of calcium ion-exchanged silica rust resisting pigment of the present invention is easy to operate, and equipment requirement is low, production effect
Rate is high.By using special synthesis technology, calcium ion-exchanged agent is added during the reaction and carries out ion exchange, and is being acidified
Stage carries out hydrophobically modified to silica surface with special organic-silicon-modified auxiliary agent, improves silica and resin paint film
Between active force, increase the crosslink density of paint film, reduce infiltration of the moisture content to paint film.
Specific embodiment
In order to make the objectives, technical solutions, and advantages of the present invention clearer, below in conjunction with specific embodiment, to this
Invention be further described, but the present invention claims protection scope be not limited to embodiment.
Embodiment 1:
The preparation (doing five Duplicate Samples) of calcium ion-exchanged silica rust resisting pigment:
Pure water 100g is added into reaction kettle, with sulphur acid for adjusting pH to 1, unlatching is dispersed with stirring uniformly, by 87.5g 90%
Sulfuric acid and 1500g silica concentration be 10% water glass solution be added in reaction kettle simultaneously, the cocurrent time be 30 minutes,
Reaction temperature is 90 DEG C.PH to 6 is adjusted with sodium hydroxide after reaction, adds 30g calcium hydroxide and 30g calcium nitrate,
Temperature is stirred to react 8 hours under the conditions of being 80 DEG C, is added sulphur acid for adjusting pH to 2,3g phenyltrimethoxysila,e is added, the reaction was continued
It 3 hours, by filter cake in 150 DEG C of dryings after washing filtering, then is crushed to 2~4 μm and obtains product.Its physical and chemical performance is as shown in table 1:
Table 1
Embodiment 2:
The preparation (doing five Duplicate Samples) of calcium ion-exchanged silica rust resisting pigment:
Pure water 500g is added into reaction kettle, with sulphur acid for adjusting pH to 1, unlatching is dispersed with stirring uniformly, by 175g's 30%
The water glass solution that sulfuric acid and 1000g silica concentration are 10% is added in reaction kettle simultaneously, and the cocurrent time is 120 minutes,
Reaction temperature is 30 DEG C.PH to 7 is adjusted with sodium hydroxide after reaction, 18g calcium oxide and 12g calcium chloride are added, in temperature
Degree is stirred to react 5 hours under the conditions of being 90 DEG C, is added sulphur acid for adjusting pH to 2.5,3g phenyl triethoxysilane is added, the reaction was continued
It 2 hours, by filter cake in 100 DEG C of dryings after washing filtering, then is crushed to 2~4 μm and obtains product.Its physical and chemical performance is as shown in table 2:
Table 2
Embodiment 3:
The preparation (doing five Duplicate Samples) of calcium ion-exchanged silica rust resisting pigment:
Pure water 700g is added into reaction kettle, with sulphur acid for adjusting pH to 2, unlatching is dispersed with stirring uniformly, by 262.5g 30%
Sulfuric acid and 750g silica concentration be 20% water glass solution be added in reaction kettle simultaneously, the cocurrent time be 60 minutes,
Reaction temperature is 70 DEG C.PH to 8 is adjusted with sodium hydroxide after reaction, adds 300g clarification limewash and 9g calcium oxide,
It is stirred to react 1 hour under the conditions of temperature is 100 DEG C, adds sulphur acid for adjusting pH to 4,3g aminomethyl phenyl dimethoxysilane is added,
The reaction was continued 0.5 hour, by filter cake in 110 DEG C of dryings after washing filtering, then is crushed to 2~4 μm and obtains product.Its physical and chemical performance
It is as shown in table 3:
Table 3
Embodiment 4:
The preparation (doing five Duplicate Samples) of calcium ion-exchanged silica rust resisting pigment:
Pure water 100g is added into reaction kettle, with sulphur acid for adjusting pH to 4, unlatching is dispersed with stirring uniformly, by 262.5g 30%
Sulfuric acid and 1500g silica concentration be 10% water glass solution be added in reaction kettle simultaneously, the cocurrent time be 90 minutes,
Reaction temperature is 50 DEG C.PH to 7 is adjusted with sodium hydroxide after reaction, 15g calcium oxide and 20g calcium nitrate are added, in temperature
Degree is stirred to react 8 hours under the conditions of being 90 DEG C, is added sulphur acid for adjusting pH to 2.5,3g phenyltrimethoxysila,e is added, the reaction was continued
It 2 hours, by filter cake in 110 DEG C of dryings after washing filtering, then is crushed to 2~4 μm and obtains product.Its physical and chemical performance is as shown in table 4:
Table 4
Embodiment 5:
The preparation (doing five Duplicate Samples) of calcium ion-exchanged silica rust resisting pigment:
Pure water 600g is added into reaction kettle, with sulphur acid for adjusting pH to 2, unlatching is dispersed with stirring uniformly, by 175g's 45%
The water glass solution that sulfuric acid and 1000g silica concentration are 15% is added in reaction kettle simultaneously, and the cocurrent time is 60 minutes, instead
Answering temperature is 30 DEG C.PH to 7 is adjusted with sodium hydroxide after reaction, 20g calcium hydroxide and 10g calcium nitrate are added, in temperature
Degree is stirred to react 8 hours under the conditions of being 90 DEG C, adds sulphur acid for adjusting pH to 2.5,3g phenyltrimethoxysila,e and 3g methyl is added
Phenyidimethoxysilane, the reaction was continued 3 hours, by filter cake in 110 DEG C of dryings after washing filtering, then is crushed to 2~4 μm and obtains
Product.Its physical and chemical performance is as shown in table 5:
Table 5
Comparative example 1:
Compared with Example 1, organic-silicon-modified auxiliary agent is not added.
The preparation (doing five Duplicate Samples) of calcium ion-exchanged silica rust resisting pigment:
Pure water 100g is added into reaction kettle, with sulphur acid for adjusting pH to 1, unlatching is dispersed with stirring uniformly, by 87.5g 90%
Sulfuric acid and 1500g silica concentration be 10% water glass solution be added in reaction kettle simultaneously, the cocurrent time be 30 minutes,
Reaction temperature is 90 DEG C.PH to 6 is adjusted with sodium hydroxide after reaction, adds 30g calcium hydroxide and 30g calcium nitrate,
Temperature is stirred to react 8 hours under the conditions of being 80 DEG C, by filter cake in 150 DEG C of dryings after washing filtering, then is crushed to 2~4 μm and is obtained
Product.Its physical and chemical performance is as shown in table 6:
Table 6
Comparative example 2:
Compared with Example 1, selecting dioxide-containing silica is the water glass solution of 5wt%, other operations and 1 phase of embodiment
Together.Five Duplicate Samples are done, the physical and chemical performance for obtaining product is as shown in table 7:
Table 7
Comparative example 3:
The preparation (doing five Duplicate Samples) of calcium ion-exchanged silica rust resisting pigment:
Pure water 100g is added into reaction kettle, with sulphur acid for adjusting pH to 1, unlatching is dispersed with stirring uniformly, by 87.5g 90%
Sulfuric acid and 1500g silica concentration be 10% water glass solution be added in reaction kettle simultaneously, the cocurrent time be 30 minutes,
Reaction temperature is 90 DEG C.PH to 8.5 is adjusted with sodium hydroxide after reaction, adds 30g calcium hydroxide and 30g calcium nitrate,
It is stirred to react 8 hours, adds sulphur acid for adjusting pH to 2,3g phenyltrimethoxysila,e is added, the reaction was continued 3 hours, after washing filtering
By filter cake in 150 DEG C of dryings, then it is crushed to 2~4 μm and obtains product.Its physical and chemical performance is as shown in table 8:
Table 8
The application performance of calcium ion-exchanged silica rust resisting pigment
1, the preparation of epoxy ester undercoat coating
Ca/SiO2Epoxy ester undercoat is with 619 epoxy resin and Ca/SiO2Type rust resisting pigment is primary raw material, and a small amount of iron is added
Red, blanc fixe, ZnO etc. are used as filler.Colored paint is filtered using 80 mesh filter screens, uses dimethylbenzene, butyl ester as diluent
Working viscosity is adjusted, controls fineness in 60um or less.
2, preparation of specimen
The antirusting paint prepared is sprayed at by GB1727-92 method meet GB9271-88 standard common low carbon it is thin
On steel plate, specific size 100mm*150mm, 120 ± 2 DEG C after baking 1 hour, using the waterproof abrasive paper wet-milling of 400 mesh, 50 ± 2
DEG C after baking dry 30 minutes, second paint is sprayed, is finally toasted 1 hour with 120 ± 2 DEG C, control total film thickness is 40 ± 2 μm
(being tested using GB1764 non-destructive method), uses paraffin: rosin=1:1 mixture carries out edge sealing.It is dry to paint film
It is tested after dry 24 hours.
The test of 3 paint film properties
Calcium ion-exchanged silica rust resisting pigment prepared by embodiment 1-5 and comparative example 1-3 carries out correlated performance survey
Examination, acquired results are as shown in table 9.
Table 9
As can be seen from Table 9, the calcium ion-exchanged silica rust resisting pigment of preparation of the embodiment of the present invention is applied to paint film,
The performance of resistance to salt water and resistance to neutral salt spray is superior to comparative example 1-3 and H06-2 iron red epoxy primer.And comparative example 1-3 is at this
On the basis of invention change synthesis technology in dioxide-containing silica, reaction pH value and do not add organic-silicon-modified auxiliary agent,
Obtained calcium ion-exchanged silica rust resisting pigment is applied to rustless property when paint film and declines.
According to the disclosure and teachings of the above specification, those skilled in the art in the invention can also be to above-mentioned embodiment party
Formula is changed and is modified.Therefore, the invention is not limited to the specific embodiments disclosed and described above, to the one of invention
A little modifications and changes should also be as falling into the scope of the claims of the present invention.In addition, although being used in present specification
Some specific terms, these terms are merely for convenience of description, does not limit the present invention in any way.
Claims (10)
1. a kind of preparation method of calcium ion-exchanged silica rust resisting pigment, which comprises the following steps:
S1. ingredient: preparing the water glass solution that dioxide-containing silica is 10~20wt%, and compound concentration is the sulphur of 30~90wt%
Acid solution；
S2. it synthesizes: water being added into reaction kettle, adjustment system pH is 1~4, is stirred evenly；The water glass solution that S1 is prepared
Cocurrent is added in reaction kettle simultaneously with sulfuric acid solution, and cocurrent total time is 30~120 minutes, and cocurrent temperature is 30~90 DEG C；And
The pH value of mixed solution is adjusted after stream to 6~8, and calcium ion-exchanged agent, and the ion exchange at 80~100 DEG C is then added
1~8 hour；
S3. then regulation system pH value is added organic-silicon-modified auxiliary agent, reacts 0.5~3 hour to 2~4；
S4. reaction product is filtered washing, then dry, pulverize.
2. the preparation method of calcium ion-exchanged silica rust resisting pigment according to claim 1, which is characterized in that including
Following steps:
S1. ingredient: preparing the water glass solution that dioxide-containing silica is 15wt%, and compound concentration is the sulfuric acid solution of 45wt%；
S2. it synthesizes: water being added into reaction kettle, adjustment system pH is 2, is stirred evenly；Water glass solution that S1 is prepared and
Cocurrent is added in reaction kettle sulfuric acid solution simultaneously, and cocurrent total time is 60 minutes, and cocurrent temperature is 30 DEG C；Hydrogen is used after cocurrent
Sodium oxide molybdena adjusts the pH value of mixed solution to 7, and calcium ion-exchanged agent, and ion exchange 8 hours at 90 DEG C are then added；
S3. then regulation system pH value is added organic-silicon-modified auxiliary agent, reacts 3 hours to 2.5；
S4. reaction product is filtered washing, then dry, pulverize.
3. the preparation method of calcium ion-exchanged silica rust resisting pigment according to claim 1, which is characterized in that described
Calcium ion-exchanged agent, organic-silicon-modified auxiliary agent mass ratio be 10-13:1.
4. the preparation method of calcium ion-exchanged silica rust resisting pigment according to claim 1, which is characterized in that in S2
The calcium ion-exchanged agent being added is one of calcium hydroxide, calcium oxide, clarification limewash, calcium nitrate, calcium chloride or a variety of.
5. the preparation method of calcium ion-exchanged silica rust resisting pigment according to claim 4, which is characterized in that added
The calcium ion-exchanged agent entered is calcium hydroxide and calcium nitrate, mass ratio 1:0.5-1.
6. the preparation method of calcium ion-exchanged silica rust resisting pigment according to claim 1, which is characterized in that in S3
The organic-silicon-modified auxiliary agent being added is phenyltrimethoxysila,e, phenyl triethoxysilane, aminomethyl phenyl dimethoxy silicon
One of alkane, aminomethyl phenyl diethoxy silane are a variety of.
7. the preparation method of calcium ion-exchanged silica rust resisting pigment according to claim 6, which is characterized in that added
The organic-silicon-modified auxiliary agent entered is phenyltrimethoxysila,e and aminomethyl phenyl dimethoxysilane.
8. the preparation method of calcium ion-exchanged silica rust resisting pigment according to claim 1, which is characterized in that S4 will
Then reaction product filtration washing dry, pulverize filter cake to 2~4 μm in 100~150 DEG C to 50 μ S/cm of conductivity <.
9. a kind of preparation method by any calcium ion-exchanged silica rust resisting pigment of claim 1-8 is prepared
Rust resisting pigment.
10. a kind of antirusting paint comprising rust resisting pigment as claimed in claim 9.
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| CN110607197A (en) * | 2019-08-23 | 2019-12-24 | 广州凌玮科技股份有限公司 | Antirust lubricating oil |
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| CN115637072A (en) * | 2022-10-28 | 2023-01-24 | 瓮福（集团）有限责任公司 | Calcium ion exchange type antirust pigment prepared from fluorine-containing silicon powder and preparation method thereof |
| CN115678336A (en) * | 2022-10-28 | 2023-02-03 | 瓮福（集团）有限责任公司 | Extinction powder prepared from fluorine-containing silicon powder and preparation method thereof |
| CN115637072B (en) * | 2022-10-28 | 2024-03-08 | 瓮福（集团）有限责任公司 | Calcium ion exchange type antirust pigment prepared from fluorine-containing silicon powder and preparation method thereof |
| CN115678336B (en) * | 2022-10-28 | 2024-04-05 | 瓮福（集团）有限责任公司 | Extinction powder prepared from fluorine-containing silicon powder and preparation method thereof |
| CN116715985A (en) * | 2023-07-04 | 2023-09-08 | 连城县佳辉科技有限公司 | Antirust pigment and paint and preparation method thereof |
| CN116715985B (en) * | 2023-07-04 | 2023-12-15 | 连城县佳辉科技有限公司 | Antirust pigment and paint and preparation method thereof |
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| CN109735153B (en) | 2021-05-07 |
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