CN106380111A - Corrosion inhibitor slow-release microcapsule and preparation method thereof - Google Patents
Corrosion inhibitor slow-release microcapsule and preparation method thereof Download PDFInfo
- Publication number
- CN106380111A CN106380111A CN201610781539.4A CN201610781539A CN106380111A CN 106380111 A CN106380111 A CN 106380111A CN 201610781539 A CN201610781539 A CN 201610781539A CN 106380111 A CN106380111 A CN 106380111A
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- China
- Prior art keywords
- corrosion inhibitor
- release microcapsule
- preparation
- slow
- inhibitor slow
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Classifications
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
- C04B40/0028—Aspects relating to the mixing step of the mortar preparation
- C04B40/0039—Premixtures of ingredients
- C04B40/0046—Premixtures of ingredients characterised by their processing, e.g. sequence of mixing the ingredients when preparing the premixtures
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
- C04B2103/0068—Ingredients with a function or property not provided for elsewhere in C04B2103/00
- C04B2103/0069—Ingredients with a function or property not provided for elsewhere in C04B2103/00 the ingredients being characterised by their physical state
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
- C04B2103/60—Agents for protection against chemical, physical or biological attack
- C04B2103/61—Corrosion inhibitors
Abstract
The invention provides slow-release microcapsule containing a corrosion inhibitor and a preparation method thereof. The technical problem that existing microcapsules have short corrosion inhibition period and the wall material is not suitable for a concrete system is solved. The capsule-core of the corrosion inhibitor slow-release microcapsule is sodium monofluorophosphate. The capsule-wall of the corrosion inhibitor slow-release microcapsule is a composite material of cage-type polysilsesquioxane and polymethylmethacrylate polymer or polystyrene polymer. In comparison with a general polymer wall-material, the wall material of the invention has the following characteristic: as the wall material contains the molecular-level cage-type polysilsesquioxane compound, in the later period of cement concrete hydration, highly-alkaline substance in a cement system is easy to undergo a chemical reaction with silicon oxygen bond in the cage-type polysilsesquioxane compound so as to generate nano-scale micropores on the microcapsule wall-material; and the micropores, in the later use period of cement concrete, continuously release a sodium monofluorophosphate corrosion inhibitor so as to everlastingly protect steel bar in concrete.
Description
Technical field
The invention belongs to pavement material field, it is related to rust-resistant agent for concrete reinforcing bar and in particular to a kind of corrosion inhibitor slow release is micro-
Capsule and preparation method thereof
Background technology
Steel bar corrosion causes concrete structure premature failure, causes huge economic loss, is that the whole world is generally closed
The significant problem of note.Chloride Attack is the major reason causing steel bar corrosion.Under high alkalinity environment, rebar surface can be spontaneous
Generate one layer of fine and close oxide-film, make reinforcing bar be in passive state and from corrosion, but when there is a large amount of chloride ion in environment,
Chloride ion passes through local acidifying and anode unpolarizing constantly makes the passivating film dissolved destruction of rebar surface.Spread ice in a large number
Salt, it is excessively used chloride salt early strength agent, unreasonably all can cause chloride ion that reinforcing bar is invaded using sea sand and sea water intrusion etc.
Erosion.
The technical measures preventing steel bar corrosion have multiple, such as electrochemical protection, concrete surface coating, coated reinforcement etc.,
And mix corrosion inhibitor in armored concrete to change the protective capacities of its own is considered as most economical and capable having
The method of effect.Conventional reinforcing steel bar corrosion inhibitor has nitrite, amido alcohol, fatty acid ester.Sodium monofluorophosphate (MFP) is as one kind relatively
For new corrosion inhibitor, belong to a kind of corrosion inhibitor of water preparation surface penetration type, but MFP is soluble in water, add in concrete easily
Cause the loss of MFP, in addition, MFP is when external coating is constructed, its seepage velocity is gradually lowered, thus reducing its resistance rust effect.
In order to improve the resistance rust effect of sodium monofluorophosphate further, need its resistance to water and internal insertions function are further carried
Rise, existing corrosion inhibitor being placed in capsule-core using microcapsule coated technology improves its resistance to water, but being released in of corrosion inhibitor is short
Shi Fasheng, the microcapsule resistance rust phase is too short.
Content of the invention
In view of the shortcomings of the prior art, it is an object of the invention to, a kind of micro- glue of slow release including corrosion inhibitor is provided
Capsule and preparation method thereof, the solution existing microcapsule resistance rust phase is too short, and its wall material is not suitable for the technical problem of concrete system.
In order to solve above-mentioned technical problem, the present invention adopts the following technical scheme that and is achieved：
A kind of corrosion inhibitor slow-release microcapsule, including capsule-core and cyst wall, capsule-core is sodium monofluorophosphate, and cyst wall is the poly- sesquialter of cage modle
Siloxanes and the composite of poly methyl methacrylate polymer or poly styrene polymer.
Cage modle polysilsesquioxane is that TMS polysilsesquioxane, vinyl polysilsesquioxane or methyl gather
Silsesquioxane.
The preparation method of corrosion inhibitor slow-release microcapsule, comprises the following steps,
Step one, emulsifying agent is dissolved in the solution obtaining continuous phase in organic solvent；
Step 2, cage modle polysilsesquioxane is dissolved in poly methyl methacrylate polymer or poly styrene polymer
In organic solvent dichloromethane, add sodium monofluorophosphate solid matter after stirring and dissolving, obtain dispersion phase；
Step 3, the dispersion that step 2 is obtained is added in the continuous phase solution that step one obtains, and cuts through high speed
Cut, stirring at low speed to organic solvent is volatilized, and obtains suspension；
Step 4, through centrifugation, gained sediment is scrubbed, normal temperature drying obtains for the suspension that step 3 is obtained
Described corrosion inhibitor slow-release microcapsule.
Organic solvent is liquid paraffin, methyl-silicone oil, ethyl silicon oil, dimethicone, any one in phenyl silicone oil
Or numerous compositions.
Emulsifying agent is any one in Span series.The mass concentration of emulsifying agent is 0.5%～2%.
Cage modle polysilsesquioxane, poly methyl methacrylate polymer or poly styrene polymer and sodium monofluorophosphate
Addition is 1～2 in mass ratio:1～4:5～10.
Sodium monofluorophosphate fineness is more than 100 mesh.
The speed of high speed shear is 800r/min～1000r/min, and the time is 15min～30min.
The present invention compared with prior art, has the following technical effect that：
(I) wall material that present invention cladding corrosion inhibitor sodium monofluorophosphate is used is cage modle polysilsesquioxane and poly- methyl-prop
E pioic acid methyl ester polymer or poly styrene polymer composite, compared with generally using polymer wall material, contain due in wall material
There is the cage modle polysilsesquioxane compound of molecular level size (1～3nm), in the cement concrete aquation later stage, system is high-alkali
Property environment it is easy to there is chemical reaction with the siliconoxygen bond in cage modle polysilsesquioxane compound, thus in microcapsule wall material
The nano level micropore of upper generation, these micropores, during the use of cement concrete later stage, constantly discharge sodium monofluorophosphate resistance
Rust agent, will produce lasting protection to the reinforcing bar in concrete.
(II) wall material of the corrosion inhibitor slow-release microcapsule of the present invention is mixed and stirred in cement concrete and is not ruptured with the aquation initial stage,
Therefore do not affect normal hydrated, the trigger action of cage modle polysilsesquioxane material of cement in concrete, can be with concrete
In component reaction generate secondary product, make xoncrete structure more closely knit.
Brief description
Fig. 1 is used for the when m- electric potential relation figure of reinforcing bar in mortar for embodiment of the present invention 1-7.
Fig. 2 is the embodiment of the present invention 1 corrosion inhibitor slow-release microcapsule stereoscan photograph.
With reference to embodiments explanation is further explained in detail to the particular content of the present invention.
Specific embodiment
The specific embodiment of the present invention given below, implements in detail below it should be noted that the invention is not limited in
Example, all equivalents done on the basis of technical scheme each fall within protection scope of the present invention.
Embodiment 1：
The present embodiment provides a kind of corrosion inhibitor slow-release microcapsule, is calculated in mass percent, and emulsifying agent mass concentration is 2%,
The addition of TMS polysilsesquioxane, poly methyl methacrylate polymer and sodium monofluorophosphate is in mass ratio
1:1:5.
Based on the composition of raw materials of the present embodiment, the following institute of concrete preparation process of the present embodiment corrosion inhibitor slow-release microcapsule
State：
Step one, weighs 4g Span 80 and is dissolved in 200ml liquid paraffin, obtain emulsifying agent mass concentration be 2% continuous
Phase；
Step 2, weighs 2g TMS polysilsesquioxane respectively and 2g poly methyl methacrylate polymer is molten
In 20ml organic solvent dichloromethane, stirring is allowed to dissolving completely, and is added thereto to single fluorine phosphorus that 10g fineness is 200 mesh
Sour sodium powder end, stirs, and the solution of formation is dispersion phase；
Step 3, oil phase is slowly added in continuous phase solution, and through high speed shearing emulsification, high speed shear speed is
1000r/min, shear time is 15min, and then at normal temperatures, rotating speed is waved to organic solvent completely for 300r/min stirring 6h
Send out, obtain the suspension containing slow-release microcapsule；
Step 4, by the suspension obtaining through centrifugation, the precipitation obtaining is washed using petroleum ether, and normal temperature drying obtains
Arrive the microcapsule containing corrosion inhibitor sodium monofluorophosphate.
Embodiment 2：
The present embodiment provides a kind of corrosion inhibitor slow-release microcapsule, is calculated in mass percent, and emulsifying agent mass concentration is
0.5%, the addition of vinyl polysilsesquioxane, poly methyl methacrylate polymer and sodium monofluorophosphate is in mass ratio
2:1:10.
In the present embodiment, the preparation method of the requirement to raw material and corrosion inhibitor slow-release microcapsule is all same as Example 1, institute
Except for the difference that, it is Span 60 using emulsifying agent, sodium monofluorophosphate fineness of powder is 100 mesh, high speed shear speed is 800r/min,
Shear time is 30min.
Embodiment 3：
The present embodiment provides a kind of corrosion inhibitor slow-release microcapsule, is calculated in mass percent, and emulsifying agent mass concentration is 1%,
The addition of methyl sesquisiloxane, poly styrene polymer and sodium monofluorophosphate is 1 in mass ratio:2:6.
In the present embodiment, the preparation method of the requirement to raw material and corrosion inhibitor slow-release microcapsule is all same as Example 1, institute
Except for the difference that, it is Span 40 using emulsifying agent, sodium monofluorophosphate fineness of powder is 300 mesh, high speed shear speed is 1000r/
Min, shear time is 15min.
Embodiment 4：
The present embodiment provides a kind of corrosion inhibitor slow-release microcapsule, is calculated in mass percent, and emulsifying agent mass concentration is 2%,
The addition of TMS polysilsesquioxane, poly methyl methacrylate polymer and sodium monofluorophosphate is in mass ratio
1:1:10.
In the present embodiment, the preparation method of the requirement to raw material and corrosion inhibitor slow-release microcapsule is all same as Example 1, institute
Except for the difference that, it is Span 40 using emulsifying agent, sodium monofluorophosphate fineness of powder is 200 mesh, high speed shear speed is 900r/min,
Shear time is 25min.
Embodiment 5：
The present embodiment provides a kind of corrosion inhibitor slow-release microcapsule, is calculated in mass percent, and emulsifying agent mass concentration is 2%,
The addition of methyl sesquisiloxane, poly styrene polymer and sodium monofluorophosphate is 1 in mass ratio:1:6.
In the present embodiment, the preparation method of the requirement to raw material and corrosion inhibitor slow-release microcapsule is all same as Example 1, institute
Except for the difference that, it is Span 85 using emulsifying agent, sodium monofluorophosphate fineness of powder is 150 mesh, high speed shear speed is 800r/min,
Shear time is 30min.
Embodiment 6：
The present embodiment provides a kind of corrosion inhibitor slow-release microcapsule, is calculated in mass percent, and emulsifying agent mass concentration is
1.5%, the addition of vinyl polysilsesquioxane, poly methyl methacrylate polymer and sodium monofluorophosphate is in mass ratio
1:4:9.
In the present embodiment, the preparation method of the requirement to raw material and corrosion inhibitor slow-release microcapsule is all same as Example 1, institute
Except for the difference that, it is Span 80 using emulsifying agent, sodium monofluorophosphate fineness of powder is 200 mesh, high speed shear speed is 800r/min,
Shear time is 30min.
Embodiment 7：
The present embodiment provides a kind of corrosion inhibitor slow-release microcapsule, is calculated in mass percent, and emulsifying agent mass concentration is 1%,
The addition of TMS polysilsesquioxane, poly styrene polymer and sodium monofluorophosphate is 1 in mass ratio:1:5.
In the present embodiment, the preparation method of the requirement to raw material and corrosion inhibitor slow-release microcapsule is all same as Example 1, institute
Except for the difference that, it is Span 85 using emulsifying agent, sodium monofluorophosphate fineness of powder is 200 mesh, high speed shear speed is 900r/min,
Shear time is 25min.
Comparative example 1：
This comparative example provides a kind of corrosion inhibitor microcapsule, is calculated in mass percent, and emulsifying agent mass concentration is 2%, poly- first
The addition of base methacrylate polymer and sodium monofluorophosphate is 1 in mass ratio:5.
In this comparative example, the preparation method of the requirement to raw material and corrosion inhibitor microcapsule is all same as Example 1, and institute is different
, corrosion inhibitor microcapsule capsule wall material do not add TMS polysilsesquioxane.
Comparative example 2：
This comparative example provides a kind of cement concrete, is joined with m (water): m (cement): m (normal sand)=135: 300: 750
Preparation method according to national standard portland cement concrete prepares ratio.
Effect analyses：
The corrosion inhibitor microcapsule being obtained with the corrosion inhibitor slow-release microcapsule that obtains in embodiment 1-7 and comparative example 2 is by 2%
Mass ratio is incorporated in cement, with m (water): m (cement): m (normal sand)=135: 300: 750 proportioning, according to GB 8076
1997《Concrete admixture》Hardened sand slurry processes in steel bar corrosion accelerated test procedures are tested, by the hardened sand handled well
Slurry electrode is placed in saturated calcium hydroxide solution, after soaking a few hours, is tested with PS-6 steel bar corrosion measuring instrument, chlorination
The concentration of sodium water solution is 3.5%, record 5,10,15,20,25,30min when be embedded with the mortar electrode anode polarization potential of reinforcing bar
Value experiment, result is as shown in Figure 1.
Test result indicate that：In cement concrete, do not add any corrosion inhibitor, it is (right that the reinforcing bar in sample cannot protect
Ratio 2), and add in cement concrete and do not add cage modle polysilsesquioxane cladding sodium monofluorophosphate microcapsule, because it is micro-
Capsule surface does not have infiltration lane, and sodium monofluorophosphate cannot form from surface of microcapsule and diffuse into cement so that single fluorine phosphorus
Sour sodium cannot be protected effectively to reinforcing bar.And with the addition of the microcapsule that cage modle polysilsesquioxane coats sodium monofluorophosphate,
Under high alkalinity environment, the siliconoxygen bond in cage modle polysilsesquioxane compound in cyst wall and alkali react so that micro- glue
The micropore of nanoscale size is produced on cyst wall, and sodium monofluorophosphate occurs diffusion from these nanometer level microporous surfaces, constantly
Release corrosion inhibitor is so that reinforcing bar obtains permanent protection.It will be seen from figure 1 that after reaction 30min, added with 7 of microcapsule
The anode polarization current potential of the reinforcing bar of sample (embodiment 1-7) will be high compared with the sample of comparative example 1, comparative example 2, and result shows cement
The middle corrosion inhibitor slow-release microcapsule mixing present invention preparation has fairly obvious resistance rust effect for reinforcing bar.
Claims (9)
1. a kind of corrosion inhibitor slow-release microcapsule, described corrosion inhibitor slow-release microcapsule includes capsule-core and cyst wall, and described capsule-core is single fluorine
Sodium phosphate is it is characterised in that described corrosion inhibitor slow-release microcapsule cyst wall adopts cage modle polysilsesquioxane and polymethylacrylic acid
Methacrylate polymer or the composite of poly styrene polymer.
2. corrosion inhibitor slow-release microcapsule as claimed in claim 1 is it is characterised in that described cage modle polysilsesquioxane is trimethyl
Silylation polysilsesquioxane, vinyl polysilsesquioxane or methyl sesquisiloxane.
3. the preparation method of corrosion inhibitor slow-release microcapsule described in claim 1 is it is characterised in that comprise the following steps：
Step one, emulsifying agent is dissolved in the solution obtaining continuous phase in organic solvent；
Step 2, cage modle polysilsesquioxane and poly methyl methacrylate polymer or poly styrene polymer is dissolved in organic
In methylene chloride, add sodium monofluorophosphate solid matter after stirring and dissolving, obtain dispersion phase；
Step 3, the dispersion that step 2 is obtained is added in the continuous phase solution that step one obtains, through high speed shear, low
Speed stirs to organic solvent volatilization, obtains suspension；
Step 4, the suspension that step 3 is obtained through centrifugation, gained sediment is scrubbed, normal temperature drying obtain described
Corrosion inhibitor slow-release microcapsule.
4. the preparation method of corrosion inhibitor slow-release microcapsule as claimed in claim 3 is it is characterised in that described organic solvent is liquid
One or more of paraffin, methyl-silicone oil, ethyl silicon oil, dimethicone and phenyl silicone oil compositionss.
5. the preparation method of corrosion inhibitor slow-release microcapsule as claimed in claim 3 is it is characterised in that described emulsifying agent is Span system
One of row.
6. the preparation method of corrosion inhibitor slow-release microcapsule as claimed in claim 3 is it is characterised in that the quality of described emulsifying agent is dense
Spend for 0.5%～2%.
7. the preparation method of corrosion inhibitor slow-release microcapsule as claimed in claim 3 is it is characterised in that the poly- silsesquioxane of described cage modle
The addition of alkane, poly methyl methacrylate polymer or poly styrene polymer and sodium monofluorophosphate is 1～2 in mass ratio:1
～4:5～10.
8. the preparation method of corrosion inhibitor slow-release microcapsule as claimed in claim 3 is it is characterised in that described sodium monofluorophosphate fineness
More than 100 mesh.
9. the preparation method of corrosion inhibitor slow-release microcapsule as claimed in claim 3 is it is characterised in that the speed of described high speed shear
For 800r/min～1000r/min, the time is 15min～30min.
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| CN201610781539.4A CN106380111B (en) | 2016-08-30 | 2016-08-30 | A kind of corrosion inhibitor slow-release microcapsule and preparation method thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108439852A (en) * | 2018-03-31 | 2018-08-24 | 芜湖扬展新材料科技服务有限公司 | A kind of rust-resistant agent for concrete reinforcing bar |
| CN108531081A (en) * | 2018-04-19 | 2018-09-14 | 中盐金坛盐化有限责任公司 | A kind of freeze proof coating of slow-release environmental protection and preparation method thereof applied to bituminous paving |
| CN109082120A (en) * | 2018-09-28 | 2018-12-25 | 华南协同创新研究院 | A kind of elastic shell microencapsulated phase change material and its preparation method and application |
| CN109369057A (en) * | 2018-11-12 | 2019-02-22 | 武汉理工大学 | A kind of microcapsules chloride ion curing agent and its preparation method and application |
| CN111205745A (en) * | 2020-01-09 | 2020-05-29 | 厦门双瑞船舶涂料有限公司 | Self-repairing anticorrosive coating and preparation method thereof |
| CN115650454A (en) * | 2022-09-27 | 2023-01-31 | 中国海洋大学 | Preparation and application of slow-release fluorescent scale inhibition microspheres |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108439852A (en) * | 2018-03-31 | 2018-08-24 | 芜湖扬展新材料科技服务有限公司 | A kind of rust-resistant agent for concrete reinforcing bar |
| CN108531081A (en) * | 2018-04-19 | 2018-09-14 | 中盐金坛盐化有限责任公司 | A kind of freeze proof coating of slow-release environmental protection and preparation method thereof applied to bituminous paving |
| CN109082120A (en) * | 2018-09-28 | 2018-12-25 | 华南协同创新研究院 | A kind of elastic shell microencapsulated phase change material and its preparation method and application |
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| CN109369057A (en) * | 2018-11-12 | 2019-02-22 | 武汉理工大学 | A kind of microcapsules chloride ion curing agent and its preparation method and application |
| CN111205745A (en) * | 2020-01-09 | 2020-05-29 | 厦门双瑞船舶涂料有限公司 | Self-repairing anticorrosive coating and preparation method thereof |
| CN115650454A (en) * | 2022-09-27 | 2023-01-31 | 中国海洋大学 | Preparation and application of slow-release fluorescent scale inhibition microspheres |
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| CN106380111B (en) | 2019-03-01 |
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