CN107022080A - A kind of preparation method of novel silicon alkanes plural gel waterproof material - Google Patents
A kind of preparation method of novel silicon alkanes plural gel waterproof material Download PDFInfo
- Publication number
- CN107022080A CN107022080A CN201710291399.7A CN201710291399A CN107022080A CN 107022080 A CN107022080 A CN 107022080A CN 201710291399 A CN201710291399 A CN 201710291399A CN 107022080 A CN107022080 A CN 107022080A
- Authority
- CN
- China
- Prior art keywords
- plural gel
- preparation
- waterproof material
- oil phase
- aqueous phase
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000000463 material Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 23
- -1 silicon alkanes Chemical class 0.000 title claims abstract description 22
- 229910052710 silicon Inorganic materials 0.000 title claims abstract description 16
- 239000010703 silicon Substances 0.000 title claims abstract description 16
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 50
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000012071 phase Substances 0.000 claims abstract description 33
- 229910000077 silane Inorganic materials 0.000 claims abstract description 33
- 239000003921 oil Substances 0.000 claims abstract description 32
- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical compound [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 claims abstract description 31
- 239000008346 aqueous phase Substances 0.000 claims abstract description 30
- NWGKJDSIEKMTRX-AAZCQSIUSA-N Sorbitan monooleate Chemical compound CCCCCCCC\C=C/CCCCCCCC(=O)OC[C@@H](O)[C@H]1OC[C@H](O)[C@H]1O NWGKJDSIEKMTRX-AAZCQSIUSA-N 0.000 claims abstract description 19
- 239000000178 monomer Substances 0.000 claims abstract description 18
- 239000012153 distilled water Substances 0.000 claims abstract description 13
- 238000002156 mixing Methods 0.000 claims abstract description 10
- 150000004756 silanes Chemical class 0.000 claims abstract description 9
- 238000001704 evaporation Methods 0.000 claims abstract description 7
- 230000008020 evaporation Effects 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims abstract description 7
- 239000012298 atmosphere Substances 0.000 claims abstract description 3
- ALVYUZIFSCKIFP-UHFFFAOYSA-N triethoxy(2-methylpropyl)silane Chemical compound CCO[Si](CC(C)C)(OCC)OCC ALVYUZIFSCKIFP-UHFFFAOYSA-N 0.000 claims description 10
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 claims description 4
- 238000002454 metastable transfer emission spectrometry Methods 0.000 claims description 4
- MSRJTTSHWYDFIU-UHFFFAOYSA-N octyltriethoxysilane Chemical compound CCCCCCCC[Si](OCC)(OCC)OCC MSRJTTSHWYDFIU-UHFFFAOYSA-N 0.000 claims description 4
- 229960003493 octyltriethoxysilane Drugs 0.000 claims description 4
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical group CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 claims description 4
- 230000007797 corrosion Effects 0.000 abstract description 6
- 238000005260 corrosion Methods 0.000 abstract description 6
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 abstract description 2
- 229910000831 Steel Inorganic materials 0.000 abstract description 2
- 239000011365 complex material Substances 0.000 abstract description 2
- 239000010959 steel Substances 0.000 abstract description 2
- 230000001629 suppression Effects 0.000 abstract 1
- 238000012360 testing method Methods 0.000 description 36
- 230000009102 absorption Effects 0.000 description 27
- 238000010521 absorption reaction Methods 0.000 description 27
- 239000011248 coating agent Substances 0.000 description 14
- 238000000576 coating method Methods 0.000 description 14
- 239000000839 emulsion Substances 0.000 description 11
- 238000002474 experimental method Methods 0.000 description 11
- 238000012545 processing Methods 0.000 description 10
- 230000000694 effects Effects 0.000 description 9
- 238000005516 engineering process Methods 0.000 description 6
- 239000011253 protective coating Substances 0.000 description 6
- 238000010276 construction Methods 0.000 description 5
- 238000010348 incorporation Methods 0.000 description 5
- 239000002904 solvent Substances 0.000 description 5
- 230000009286 beneficial effect Effects 0.000 description 4
- 230000033228 biological regulation Effects 0.000 description 4
- 239000002270 dispersing agent Substances 0.000 description 4
- 239000003995 emulsifying agent Substances 0.000 description 4
- 239000000758 substrate Substances 0.000 description 4
- LFQCEHFDDXELDD-UHFFFAOYSA-N tetramethyl orthosilicate Chemical group CO[Si](OC)(OC)OC LFQCEHFDDXELDD-UHFFFAOYSA-N 0.000 description 4
- 239000002585 base Substances 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 230000002209 hydrophobic effect Effects 0.000 description 3
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000015271 coagulation Effects 0.000 description 2
- 238000005345 coagulation Methods 0.000 description 2
- 238000001035 drying Methods 0.000 description 2
- 230000005661 hydrophobic surface Effects 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 239000003973 paint Substances 0.000 description 2
- 229920001296 polysiloxane Polymers 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 229920002545 silicone oil Polymers 0.000 description 2
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 1
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 description 1
- VAJVDSVGBWFCLW-UHFFFAOYSA-N 3-Phenyl-1-propanol Chemical compound OCCCC1=CC=CC=C1 VAJVDSVGBWFCLW-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- 241000370738 Chlorion Species 0.000 description 1
- 206010023126 Jaundice Diseases 0.000 description 1
- DYUQAZSOFZSPHD-UHFFFAOYSA-N Phenylpropyl alcohol Natural products CCC(O)C1=CC=CC=C1 DYUQAZSOFZSPHD-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000004568 cement Substances 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000000460 chlorine Substances 0.000 description 1
- 229910052801 chlorine Inorganic materials 0.000 description 1
- 238000010835 comparative analysis Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000006482 condensation reaction Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000000280 densification Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- KPUWHANPEXNPJT-UHFFFAOYSA-N disiloxane Chemical class [SiH3]O[SiH3] KPUWHANPEXNPJT-UHFFFAOYSA-N 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000002706 hydrostatic effect Effects 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 239000012188 paraffin wax Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 239000003223 protective agent Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 239000005871 repellent Substances 0.000 description 1
- 239000013049 sediment Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 229920002379 silicone rubber Polymers 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 238000007711 solidification Methods 0.000 description 1
- 230000008023 solidification Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/06—Preparatory processes
-
- 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
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/009—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone characterised by the material treated
-
- 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
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/46—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements with organic materials
- C04B41/49—Compounds having one or more carbon-to-metal or carbon-to-silicon linkages ; Organo-clay compounds; Organo-silicates, i.e. ortho- or polysilicic acid esters ; Organo-phosphorus compounds; Organo-inorganic complexes
- C04B41/4905—Compounds having one or more carbon-to-metal or carbon-to-silicon linkages ; Organo-clay compounds; Organo-silicates, i.e. ortho- or polysilicic acid esters ; Organo-phosphorus compounds; Organo-inorganic complexes containing silicon
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/20—Polysiloxanes containing silicon bound to unsaturated aliphatic groups
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
- C09D183/04—Polysiloxanes
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/08—Anti-corrosive paints
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Ceramic Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Health & Medical Sciences (AREA)
- Structural Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The present invention relates to a kind of preparation method of gel complex material, and in particular to a kind of preparation method of novel silicon alkanes plural gel waterproof material.Comprise the following steps：(1) oil phase and aqueous phase are prepared：Span 80 and silane monomer are taken, is sufficiently stirred in homogenizer, uniform oil phase is prepared；Take PPG O and distilled water to be uniformly dispersed in homogenizer, prepare uniform aqueous phase；(2) oil phase and aqueous phase are uniformly mixed：Aqueous phase is poured into flask, oil phase and PEG 2000, high-speed stirred are slowly added to while stirring；(3) TEOS is added：TEOS is slowly added to, addition continues high-speed stirred under constant temperature after finishing；(4) plural gel is made：Improve mixing temperature and opening is exposed in atmosphere, by moisture evaporation, so as to obtain silanes plural gel.Silanes plural gel obtained by the present invention has the generation of excellent waterproof ability and corrosion resistance of chloride ion ability, effectively suppression steel bar corrosion and concrete corrosion.
Description
Technical field
The present invention relates to a kind of preparation method of gel complex material, and in particular to a kind of novel silicon alkanes plural gel is prevented
The preparation method of water material.
Background technology
Harbour concrete structure need to often take some special measures to improve the durability of structure.In recent years, laboratory is ground
The durability that study carefully result fully proves to improve concrete structure using silane hydrophobic surface treatment technology is reliable, and should
Technology is more and more applied in Practical Project.In Practical Project, due to the limitation of field condition, construction quality
Validity on above-mentioned concrete surface safeguard procedures can make a significant impact.Therefore, the live silane hydrophobic surface of scientific evaluation
Before the construction effect of guard technology is reasonable prediction using the durability and service life of the harbour concrete structure of the technology
Carry.
Permselective silane material forms the hydrophobic film waterproof construction of densification in concrete surface and pore inwall, can make coagulation
Humidity inside soil is gradually reduced, so as to prevent or reduce the infringement that alkali-aggregate reaction is caused to concrete structure.Permselective silane
The waterproof construction of material formation, makes inside concrete isolate with wet environment, so as to prevent that inside concrete formation saturation is watery
State, mitigates freeze-thaw damage.
Common silane waterproof material has following classification：
(1) aqueous silane protective coating
The protective agent chief component is methyl silicate., can be with base material top layer, air after substrate surface is coated in
In CO2Reacted with water, further polymerization generation polymethyl siloxane film, the film has very strong hydrophobicity performance.
This one type of silane water-repellent paint low cost, construction technology is easy, easy to operate.However, its shortcoming is it is also obvious that main
In terms of being embodied in three below：First, methyl silicate with CO2When being reacted, speed is more slow, and it is firm to want to reach
Solidification effect need long time；Second, methyl silicate reacts not complete enough in the preliminary stage of coating, and part is also
It is to be in water soluble state, once there are the weather such as rainwater and frost, the unreacted or incomplete coating of reaction will be very
Readily depart from substrate surface, weaken hydrophobic effect；3rd, there is portion in the reaction product of methyl silicate and cement-based material
Divide alkali carbonate, more obvious sediment occurs in substrate surface, the situation of jaundice, appearance are had when serious
It is poor.
(2) solvent-borne type silane protective coating
Solvent-borne type silane protective coating medium is based on organic solvent, and it is mainly by methyl alkoxy (or chlorine) silane, carbon
The raw materials such as chain alkyl alkoxy silane, the octyltri-ethoxysilane of number >=8 coordinate synthesized by different types of modified silane,
It can be used alone, but in order to reach better protection effect, can add in right amount when in use organic molten in application aspect
Agent, is effectively combined in this, as carrier.
In practical engineering application, when being applied over substrate surface, solvent will quickly volatilize, in concrete surface or hair
One layer of very thin colorless and transparent film is deposited on pore, the natural look on concrete influences very little.Because it is by external environment
Influence is smaller, thus it is wider using scope, but the volatilization of organic solvent, easily cause environmental pollution.
(3) emulsion-type silane protective coating
Emulsion-type silane protective coating is by organic polymer emulsion (such as acrylic acid, acid third, phenylpropyl alcohol polymer emulsion)
With a class NEW PAINT SYSTEMS FOR BUILDINGS of reactive silane emulsion (reactive silicon rubber or active silicone oil) synthesis.
The base material treated using emulsion-type silane protective coating can not only ensure the good breathable properties of wall, moreover it is possible to
Effectively suppress the intrusion of moisture, reach excellent hydrophobic effect.What application was more at present is Methyl Hydrogen Polysiloxane Fluid emulsion, hydroxyl
Silicone oil emulsion and alkylalkoxy silane emulsion etc..
The content of the invention
To solve the above-mentioned problems in the prior art, the present invention provides a kind of novel silicon alkanes plural gel waterproof material
The preparation method of material.
The technical solution adopted by the present invention is as follows：
A kind of preparation method of novel silicon alkanes plural gel waterproof material, comprises the following steps：
Step one, oil phase and aqueous phase are prepared
Span 80 and silane monomer are taken, is sufficiently stirred in homogenizer, uniform oil phase is prepared；Take PPG O and distillation
Water is uniformly dispersed in homogenizer, prepares uniform aqueous phase；
Step 2, oil phase and aqueous phase are uniformly mixed
Aqueous phase is poured into flask, oil phase and PEG 2000, high-speed stirred are slowly added to while stirring；
Step 3, adds TEOS
TEOS is slowly added to, addition continues high-speed stirred under constant temperature after finishing；
Step 4, is made plural gel
Improve mixing temperature and opening is exposed in atmosphere, by moisture evaporation, so as to obtain silanes plural gel.
Further, the mass fraction of the TEOS described in step 3 is 30%~50%.
Further, the silane monomer described in step one be MTES, it is VTES, pungent
Ethyl triethoxy silicane alkane or isobutyl triethoxy silane.
Further, the mass fraction of the Span 80 described in step one is for 2%~10%, PPG O mass fraction
2%~10%, Span 80 and PPG O ratio are 1:1~1:2.
Further, the mass fraction of the silane monomer described in step one is 20%~60%, the mass fraction of distilled water
For 30%~40%.
Further, the mass fraction of the PEG 2000 described in step 2 is 0.1%~0.5%.
Further, the speed of agitator for preparing oil phase described in step one is 18000~20000r/min, prepares aqueous phase
Mixing speed is 15000~18000r/min.
Further, the add oil phase and the temperature of PEG 2000 and high-speed stirred described in step 2 are 30~50 DEG C, are stirred
The time is mixed for 1~2h.
Further, the temperature of the high-speed stirred described in step 3 is 30~50 DEG C, and mixing time is 3~10h.
Further, the temperature of the mixing described in step 4 is 50~80 DEG C.
Compared with prior art, the present invention has following excellent technique effect：
(1) the silanes plural gel obtained by technical solution of the present invention has excellent waterproof ability.
Condensation reaction further occurs between the hydroxyl in concrete surface and capillary channel and generates netted organosilicon tree
Fat, by stable silica chemical bond, silicone molecules is securely attached in concrete surface and capillary channel, make to drop in
Water above it turns into droplet, it is impossible to penetrate into inside base material, so that the nuisance effectively entrained by stop moisture and moisture
Matter penetrates into inside concrete.
(2) the silanes plural gel obtained by technical solution of the present invention has excellent corrosion resistance of chloride ion ability.
By suppressing the intrusion of moisture, and then suppress the entrance of the harmful ions such as chlorion, effectively suppress steel bar corrosion and
The generation of concrete corrosion.
Brief description of the drawings
Fig. 1 is that capillary water absorption tests schematic diagram；
Fig. 2 is C40 concrete test block 48h water absorption fitted figures in table 1；
Fig. 3 is C50 concrete test block 48h water absorption fitted figures in table 1；
Fig. 4 is C40 concrete test block the coefficient of capillary suction fitted figures in table 2；
Fig. 5 is C50 concrete test block the coefficient of capillary suction fitted figures in table 2；
Fig. 6 is the concrete capillary water absorption amount curve of different TEOS incorporations.
Embodiment
The present invention is further explained with reference to embodiments：
Embodiment 1
Experiment material：
Silane monomer (isobutyl triethoxy silane, TEOS), emulsifying agent (Span 80, PPG O), dispersant (PEG
2000), solvent (distilled water).
Preparation process：
Step one, oil phase and aqueous phase are prepared
3% Span 80 and 35% isobutyl triethoxy silane monomer is taken, is sufficiently stirred in homogenizer, rotating speed
For 19000r/min, uniform oil phase is prepared；Take 3% PPG O and 30% distilled water to be uniformly dispersed in homogenizer, turn
Speed is 17500r/min, prepares uniform aqueous phase, it is ensured that Span 80 and PPG O ratio are 1:1.
Step 2, oil phase and aqueous phase are uniformly mixed
Aqueous phase is poured into three-neck flask, regulation temperature is 40 DEG C, and oil phase and 0.2% PEG are slowly added to while stirring
2000, high-speed stirred 1h.
Step 3, adds TEOS
35% TEOS is slowly added to, addition continues the high-speed stirred 4h under 40 DEG C of constant temperature after finishing.
Step 4, is made plural gel
Whipping temp rise is for 60 DEG C and open in air, beneficial to the evaporation of moisture, so as to obtain new multiple
Close silane gel.
Embodiment 2
Experiment material：
Silane monomer (MTES, TEOS), emulsifying agent (Span 80, PPG O), dispersant (PEG
2000), solvent (distilled water).
Preparation process：
Step one, oil phase and aqueous phase are prepared
3% Span 80 and 35% MTES monomer is taken, is sufficiently stirred in homogenizer, rotating speed is
19000r/min, prepares uniform oil phase；3% PPG O and 30% distilled water is taken to be uniformly dispersed in homogenizer, rotating speed
For 17500r/min, uniform aqueous phase is prepared, it is ensured that Span 80 and PPG O ratio are 1:1.
Step 2, oil phase and aqueous phase are uniformly mixed
Aqueous phase is poured into three-neck flask, regulation temperature is 40 DEG C, and oil phase and 0.2% PEG are slowly added to while stirring
2000, high-speed stirred 1h.
Step 3, adds TEOS
35% TEOS is slowly added to, addition continues the high-speed stirred 4h under 40 DEG C of constant temperature after finishing.
Step 4, is made plural gel
Whipping temp rise is for 60 DEG C and open in air, beneficial to the evaporation of moisture, so as to obtain new multiple
Close silane gel.
Embodiment 3
Experiment material：
Silane monomer (VTES, TEOS), emulsifying agent (Span 80, PPG O), dispersant (PEG
2000), solvent (distilled water).
Preparation process：
Step one, oil phase and aqueous phase are prepared
3% Span 80 and 35% VTES monomer is taken, is sufficiently stirred in homogenizer, rotating speed
For 19000r/min, uniform oil phase is prepared；Take 3% PPG O and 30% distilled water to be uniformly dispersed in homogenizer, turn
Speed is 17500r/min, prepares uniform aqueous phase, it is ensured that Span 80 and PPG O ratio are 1:1.
Step 2, oil phase and aqueous phase are uniformly mixed
Aqueous phase is poured into three-neck flask, regulation temperature is 40 DEG C, and oil phase and 0.2% PEG are slowly added to while stirring
2000, high-speed stirred 1h.
Step 3, adds TEOS
35% TEOS is slowly added to, addition continues the high-speed stirred 4h under 40 DEG C of constant temperature after finishing.
Step 4, is made plural gel
Whipping temp rise is for 60 DEG C and open in air, beneficial to the evaporation of moisture, so as to obtain new multiple
Close silane gel.
Embodiment 4
Experiment material：
Silane monomer (octyltri-ethoxysilane, TEOS), emulsifying agent (Span 80, PPG O), dispersant (PEG
2000), solvent (distilled water).
Preparation process：
Step one, oil phase and aqueous phase are prepared
3% Span 80 and 35% octyltri-ethoxysilane monomer is taken, is sufficiently stirred in homogenizer, rotating speed is
19000r/min, prepares uniform oil phase；3% PPG O and 30% distilled water is taken to be uniformly dispersed in homogenizer, rotating speed
For 17500r/min, uniform aqueous phase is prepared, it is ensured that Span 80 and PPG O ratio are 1:1.
Step 2, oil phase and aqueous phase are uniformly mixed
Aqueous phase is poured into three-neck flask, regulation temperature is 40 DEG C, and oil phase and 0.2% PEG are slowly added to while stirring
2000, high-speed stirred 1h.
Step 3, adds TEOS
35% TEOS is slowly added to, addition continues the high-speed stirred 4h under 40 DEG C of constant temperature after finishing.
Step 4, is made plural gel
Whipping temp rise is for 60 DEG C and open in air, beneficial to the evaporation of moisture, so as to obtain new multiple
Close silane gel.
Experimental example：Capillary water absorption experiment under hydrostatic pressure after concrete coating plural gel
As shown in figure 1, taking out the concrete test block (strength grade is respectively C40, C50) conserved, hung down along unshaped face
Vertical cut is opened, and test block size is changed into 100mm × 100mm × 50mm.Drying and processing is carried out to concrete test block, chosen after the completion of drying
One forming face of test block, completes application job, and other faces are sealed with paraffin, so as to ensure that capillary water absorption experiment is inhaled to be one-dimensional
Water.
Applicator surface is lowered into the tank equipped with distilled water, concrete test block is supported with support, it is ensured that the water surface is high
Go out 5 ± 1mm of applicator surface.Weigh test block after water suction experiment starts 0,1,2,4,6,8,12,24,36,48h quality, obtain
The concrete test block capillary water absorption amount change of difference coating processing, and according to time evolution law, calculate the hair of every group of test block
Thin absorption coerfficient.
In formula：A --- the coefficient of capillary suction (gm-2·h-1/2)
Δ W --- water absorption (gm in the test block t times-2)
T --- capillary water absorbing time (h)
Table 1 is the concrete test block (strength grade is respectively C40, C50) of varying strength through different silanes waterproof materials
Capillary water absorption result after processing.Wherein, experimental group 1 is the concrete test block of space management, and experimental group 2 is only coating TEOS's
Concrete test block, experimental group 3 for coating isobutyl triethoxy silane emulsion (be added without TEOS, remaining with the phase of embodiment 1
Concrete test block together), experimental group 4 is the concrete test block of the coating gained plural gel of embodiment 1.
As can be seen that experimental group 2,3,4 is compared with experimental group 1 from table 1, Fig. 2 and Fig. 3, the coagulation of coated processing
Water absorption of the native test block in 48h has obvious reduction.When strength grade of concrete is C40, because concrete itself is closely knit
Degree is relatively low, and blank group capillary water absorption result is very notable, and gap is pulled open in the test block with coated with water blocking material, in capillary water absorption
After 48h, blank group (experimental group 1) water absorption reaches 1389gm-2, and through TEOS, isobutyl triethoxy silane emulsion, compound
The concrete (experimental group 2,3,4) of gel coating processing, 48h water absorption only respectively reaches 359gm-2、299g·m-2、
251g·m-2.As the ratio of mud is reduced, concrete strength is in C50, and each group test block water absorption decreases, and proceeds in experiment
During 48h, blank group test block (experimental group 1) water absorption reaches 687gm-2, through TEOS, isobutyl triethoxy silane emulsion, answer
The concrete (experimental group 2,3,4) of gel coating processing is closed, 48h water absorption only respectively reaches 234gm-2、144g·m-2、
118g·m-2.In three kinds of waterproof materials, plural gel waterproof effect is fitst water, and after the experiment of 48h capillary water absorptions, water demand ratio is not
The blank test block reduction by 81.9% and 82.8% of processing.
The concrete test block 1h and 48h water absorption (gm of the different coating processings of table 1-2)
Data result in 0~12h of fitting concrete test block capillary water absorption, obtained slope as the coefficient of capillary suction,
It is capable of the waterproof effect of the more effective different waterproof material of comparative analysis.Table 2 is the hair of the concrete test block of different coating processings
Thin absorption coerfficient.As can be seen that for C40 concrete, blank test block (experimental group 1) capillary water absorption system from table 2, Fig. 4 and Fig. 5
Number is 240gm-2·h-1/2, coating TEOS, isobutyl triethoxy silane emulsion, the concrete test block (experiment of plural gel
Group 2,3,4) the coefficient of capillary suction reduce 75.8%, 80% and 84.1% than blank group respectively；For C50 concrete, blank
Test block (experimental group 1) the coefficient of capillary suction is 118gm-2·h-1/2, coat TEOS, isobutyl triethoxy silane emulsion, answer
Concrete test block (experimental group 4) the coefficient of capillary suction for closing gel reduces 69.5%, 78.8% and than blank group respectively
83.1%.
The coefficient of capillary suction (the gm of the concrete test block of the different coating processings of table 2-2·h-1/2)
The data result of experimental group 3 and experimental group 4 from table 1 and table 2 can show that TEOS addition is to multiple in step 3
Closing the waterproof effect of gel has important influence, therefore is also studied for TEOS addition.Table 3 is different TEOS
The plural gel coating concrete test block capillary water absorption result of incorporation.The plural gel TEOS incorporations point of experimental group 5~13
Not Wei 20%, 25%, 30%, 35%, 40%, 45%, 50%, 55%, 60% (only TEOS incorporations are different, remaining with reality
Apply example 1 identical).
The concrete test block 1h and 48h water absorption (gm of the difference TEOS incorporations of table 3-2)
From table 3 and Fig. 3 it will be evident that by the control of TEOS volumes between 35%~40%, the waterproof effect reached
Most preferably.
Table 4 coats concrete test block capillary water absorption result for the plural gel of different silane monomers.From table 4, selection
Plural gel prepared by isobutyl triethoxy silane monomer, the waterproof effect that it reaches is optimal.
The concrete test block 1h and 48h water absorption (gm of the different silane monomers of table 4-2)
By multiple orthogonal experiment, the silanes plural gel waterproof material of the concrete durability application finally given
Optimal preparation method and optimal proportion are as described in Example 1.
Claims (10)
1. a kind of preparation method of novel silicon alkanes plural gel waterproof material, it is characterised in that comprise the following steps：
Step one, oil phase and aqueous phase are prepared
Span 80 and silane monomer are taken, is sufficiently stirred in homogenizer, uniform oil phase is prepared；PPG O and distilled water is taken to exist
It is uniformly dispersed in homogenizer, prepares uniform aqueous phase；
Step 2, oil phase and aqueous phase are uniformly mixed
Aqueous phase is poured into flask, oil phase and PEG 2000, high-speed stirred are slowly added to while stirring；
Step 3, adds TEOS
TEOS is slowly added to, addition continues high-speed stirred under constant temperature after finishing；
Step 4, is made plural gel
Improve mixing temperature and opening is exposed in atmosphere, by moisture evaporation, so as to obtain silanes plural gel.
2. the preparation method of novel silicon alkanes plural gel waterproof material according to claim 1, it is characterised in that step
The mass fraction of TEOS described in three is 30%~50%.
3. the preparation method of novel silicon alkanes plural gel waterproof material according to claim 1 or 2, it is characterised in that
Silane monomer described in step one is MTES, VTES, octyltri-ethoxysilane or
Isobutyl triethoxy silane.
4. the preparation method of novel silicon alkanes plural gel waterproof material according to claim 1 or 2, it is characterised in that
The mass fraction that the mass fraction of Span 80 described in step one is 2%~10%, PPG O is the Hes of 2%~10%, Span 80
PPG O ratio is 1:1~1:2.
5. the preparation method of novel silicon alkanes plural gel waterproof material according to claim 4, it is characterised in that step
The mass fraction of silane monomer described in one is 20%~60%, and the mass fraction of distilled water is 30%~40%.
6. the preparation method of novel silicon alkanes plural gel waterproof material according to claim 1 or 2, it is characterised in that
The mass fraction of PEG 2000 described in step 2 is 0.1%~0.5%.
7. the preparation method of novel silicon alkanes plural gel waterproof material according to claim 1 or 2, it is characterised in that
The speed of agitator for preparing oil phase described in step one is 18000~20000r/min, prepare the mixing speed of aqueous phase for 15000~
18000r/min。
8. the preparation method of novel silicon alkanes plural gel waterproof material according to claim 1 or 2, it is characterised in that
Add oil phase and the temperature of PEG 2000 and high-speed stirred described in step 2 are 30~50 DEG C, and mixing time is 1~2h.
9. the preparation method of novel silicon alkanes plural gel waterproof material according to claim 1 or 2, it is characterised in that
The temperature of high-speed stirred described in step 3 is 30~50 DEG C, and mixing time is 3~10h.
10. the preparation method of novel silicon alkanes plural gel waterproof material according to claim 9, it is characterised in that step
The temperature of mixing described in rapid four is 50~80 DEG C.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710291399.7A CN107022080A (en) | 2017-04-28 | 2017-04-28 | A kind of preparation method of novel silicon alkanes plural gel waterproof material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710291399.7A CN107022080A (en) | 2017-04-28 | 2017-04-28 | A kind of preparation method of novel silicon alkanes plural gel waterproof material |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN107022080A true CN107022080A (en) | 2017-08-08 |
Family
ID=59528295
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201710291399.7A Pending CN107022080A (en) | 2017-04-28 | 2017-04-28 | A kind of preparation method of novel silicon alkanes plural gel waterproof material |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN107022080A (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107699130A (en) * | 2017-11-10 | 2018-02-16 | 青岛理工大学 | A kind of silane graphene waterproof composite material and preparation method thereof |
| CN108002741A (en) * | 2017-12-06 | 2018-05-08 | 马鞍山拓锐金属表面技术有限公司 | A kind of preparation method of silane microcapsules solid powder waterproofing agent |
| CN110183963A (en) * | 2019-06-06 | 2019-08-30 | 青岛理工大学 | A kind of graphene oxide-TEOS/ silane composite gel material and its preparation method and application |
| CN110204244A (en) * | 2019-06-06 | 2019-09-06 | 青岛理工大学 | A kind of preparation method and application of graphene oxide-TEOS/ silane composite nano materials |
| GB2595009A (en) * | 2019-06-06 | 2021-11-17 | Univ Qingdao Technology | Graphene oxide-TEOS/silane composite gel material, preparation method therefor and use thereof |
| WO2023272846A1 (en) * | 2021-06-28 | 2023-01-05 | 青岛理工大学 | Use of silane composite emulsion as anti-cracking reinforcing agent |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070098911A1 (en) * | 2005-10-31 | 2007-05-03 | Korea Electronic Power Corporation | Penetration reinforcing agent for preventing aging of concrete and process for preparing the same |
| CN106277911A (en) * | 2016-07-19 | 2017-01-04 | 无锡鸿孚硅业科技有限公司 | A kind of preparation method of silane emulsion waterproof agent for building |
-
2017
- 2017-04-28 CN CN201710291399.7A patent/CN107022080A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070098911A1 (en) * | 2005-10-31 | 2007-05-03 | Korea Electronic Power Corporation | Penetration reinforcing agent for preventing aging of concrete and process for preparing the same |
| CN106277911A (en) * | 2016-07-19 | 2017-01-04 | 无锡鸿孚硅业科技有限公司 | A kind of preparation method of silane emulsion waterproof agent for building |
Non-Patent Citations (1)
| Title |
|---|
| 陈旭 等: "《TEOS/异丁基三乙氧基硅烷复合乳液对混凝土抗氯离子渗透性能的影响》", 《涂料工业》 * |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107699130A (en) * | 2017-11-10 | 2018-02-16 | 青岛理工大学 | A kind of silane graphene waterproof composite material and preparation method thereof |
| CN108002741A (en) * | 2017-12-06 | 2018-05-08 | 马鞍山拓锐金属表面技术有限公司 | A kind of preparation method of silane microcapsules solid powder waterproofing agent |
| CN110183963A (en) * | 2019-06-06 | 2019-08-30 | 青岛理工大学 | A kind of graphene oxide-TEOS/ silane composite gel material and its preparation method and application |
| CN110204244A (en) * | 2019-06-06 | 2019-09-06 | 青岛理工大学 | A kind of preparation method and application of graphene oxide-TEOS/ silane composite nano materials |
| WO2020244263A1 (en) * | 2019-06-06 | 2020-12-10 | 青岛理工大学 | Graphene oxide-teos/silane composite gel material, preparation method therefor and use thereof |
| GB2595009A (en) * | 2019-06-06 | 2021-11-17 | Univ Qingdao Technology | Graphene oxide-TEOS/silane composite gel material, preparation method therefor and use thereof |
| AU2020227037B2 (en) * | 2019-06-06 | 2021-11-18 | Qingdao university of technology | Graphene oxide-tetraethyl orthosilicate/silane composite gel material, and preparation method and use thereof |
| GB2595009B (en) * | 2019-06-06 | 2023-07-26 | Univ Qingdao Technology | Graphene oxide-tetraethyl orthosilicate/silane composite gel material, and preparation method and use thereof |
| US11879069B2 (en) | 2019-06-06 | 2024-01-23 | Qingdao university of technology | Graphene orthosilicate/silane composite gel material, and preparation method and use thereof |
| WO2023272846A1 (en) * | 2021-06-28 | 2023-01-05 | 青岛理工大学 | Use of silane composite emulsion as anti-cracking reinforcing agent |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN107022080A (en) | A kind of preparation method of novel silicon alkanes plural gel waterproof material | |
| DE60121164T2 (en) | Water-repellent organosilicone composition | |
| US4486476A (en) | Preparation for making inorganic building materials water-repellent | |
| US6403163B1 (en) | Method of treating surfaces with organosilicon water repellent compositions | |
| US5679147A (en) | Water-based organic polysiloxane-containing compositions, processes for their preparation and their use | |
| JP2875917B2 (en) | Method and composition for making a stone building material water repellent | |
| KR101982472B1 (en) | Water repellent for concrete | |
| JPH11199292A (en) | Production of concrete which is made hydrophobic in block state, and concrete mixture obtained by this production and its use | |
| CA2849266C (en) | Process of preparing a siloxane copolymer | |
| US5319049A (en) | Impregnating waterproofing composition | |
| CN108300047A (en) | A kind of indoor anti-pollution water-water coating and preparation method thereof | |
| Roos et al. | Evolution of silicone based water repellents for modern building protection | |
| CN110183246A (en) | A kind of self-crosslinking alkylalkoxy silane impregnating agent | |
| CN103043945A (en) | Application of organic silicone emulsion waterproof agent in outer wall rock wool heat insulating material waterproof agent | |
| JP2748758B2 (en) | Impregnating waterproofing composition | |
| CN101353267A (en) | Aqueous emulsion containing organic silicon compound, preparation and use thereof in surface treatment | |
| CA1103528A (en) | Process for rendering building materials hydrophobic | |
| CN114349390B (en) | Organic silicon/inorganic nano material composite waterproof agent and preparation method thereof | |
| KR100952755B1 (en) | Water Repellent Composition | |
| CN114716690A (en) | Silicone rubber emulsion, preparation method and application | |
| CN108070258A (en) | A kind of long-acting alkylsiloxane oligomeric composition of Thief zone water-in-oil type and preparation method thereof | |
| RU2389734C1 (en) | Method for synthesis of aminooxyalkylene-containing oligoalkoxy siloxane and self-emulsifying composition based on said compound | |
| JP5058999B2 (en) | Method for hydrophobizing construction material and improving the beading effect of the material | |
| US10995255B2 (en) | Method of inhibiting water penetration into oil- and gas-producing formations | |
| CN106397772A (en) | Method for preparing micro-emulsion type waterproof preservatives for reinforced concrete |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| PB01 | Publication | ||
| PB01 | Publication | ||
| SE01 | Entry into force of request for substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20170808 |
|
| RJ01 | Rejection of invention patent application after publication |