CN111777952A - Aerogel and nano hydrotalcite synergistic fireproof sealant and preparation method thereof - Google Patents
Aerogel and nano hydrotalcite synergistic fireproof sealant and preparation method thereof Download PDFInfo
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- CN111777952A CN111777952A CN202010535536.9A CN202010535536A CN111777952A CN 111777952 A CN111777952 A CN 111777952A CN 202010535536 A CN202010535536 A CN 202010535536A CN 111777952 A CN111777952 A CN 111777952A
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- aerogel
- hydrotalcite
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- 239000004964 aerogel Substances 0.000 title claims abstract description 77
- 229960001545 hydrotalcite Drugs 0.000 title claims abstract description 72
- 229910001701 hydrotalcite Inorganic materials 0.000 title claims abstract description 72
- GDVKFRBCXAPAQJ-UHFFFAOYSA-A dialuminum;hexamagnesium;carbonate;hexadecahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Mg+2].[Al+3].[Al+3].[O-]C([O-])=O GDVKFRBCXAPAQJ-UHFFFAOYSA-A 0.000 title claims abstract description 63
- 239000000565 sealant Substances 0.000 title claims abstract description 50
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 230000002195 synergetic effect Effects 0.000 title claims description 11
- VTYYLEPIZMXCLO-UHFFFAOYSA-L calcium carbonate Substances [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims abstract description 37
- QCWXUUIWCKQGHC-UHFFFAOYSA-N Zirconium Chemical compound [Zr] QCWXUUIWCKQGHC-UHFFFAOYSA-N 0.000 claims abstract description 31
- 229910052726 zirconium Inorganic materials 0.000 claims abstract description 31
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 28
- 239000010703 silicon Substances 0.000 claims abstract description 28
- 239000000347 magnesium hydroxide Substances 0.000 claims abstract description 22
- 229910001862 magnesium hydroxide Inorganic materials 0.000 claims abstract description 22
- 239000000463 material Substances 0.000 claims abstract description 22
- 229920002367 Polyisobutene Polymers 0.000 claims abstract description 20
- 239000004115 Sodium Silicate Substances 0.000 claims abstract description 20
- 229910000019 calcium carbonate Inorganic materials 0.000 claims abstract description 20
- 239000007822 coupling agent Substances 0.000 claims abstract description 20
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims abstract description 20
- 229910052911 sodium silicate Inorganic materials 0.000 claims abstract description 20
- 239000003063 flame retardant Substances 0.000 claims abstract description 12
- 239000011159 matrix material Substances 0.000 claims abstract description 11
- 229920000642 polymer Polymers 0.000 claims abstract description 10
- 230000004048 modification Effects 0.000 claims abstract description 9
- 238000012986 modification Methods 0.000 claims abstract description 9
- 239000002131 composite material Substances 0.000 claims abstract description 8
- LDMOEFOXLIZJOW-UHFFFAOYSA-N 1-dodecanesulfonic acid Chemical group CCCCCCCCCCCCS(O)(=O)=O LDMOEFOXLIZJOW-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000000178 monomer Substances 0.000 claims abstract description 5
- 238000006116 polymerization reaction Methods 0.000 claims abstract description 5
- 239000000853 adhesive Substances 0.000 claims abstract description 4
- 230000001070 adhesive effect Effects 0.000 claims abstract description 4
- 239000000945 filler Substances 0.000 claims abstract description 4
- 238000011065 in-situ storage Methods 0.000 claims abstract description 4
- 239000012747 synergistic agent Substances 0.000 claims abstract description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 61
- 238000002156 mixing Methods 0.000 claims description 48
- 238000006243 chemical reaction Methods 0.000 claims description 34
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 27
- 239000011259 mixed solution Substances 0.000 claims description 24
- 238000003756 stirring Methods 0.000 claims description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 22
- 239000011240 wet gel Substances 0.000 claims description 21
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 20
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical compound [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 20
- WNROFYMDJYEPJX-UHFFFAOYSA-K aluminium hydroxide Chemical compound [OH-].[OH-].[OH-].[Al+3] WNROFYMDJYEPJX-UHFFFAOYSA-K 0.000 claims description 19
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 claims description 19
- 235000019441 ethanol Nutrition 0.000 claims description 17
- 239000000499 gel Substances 0.000 claims description 17
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 16
- 238000001816 cooling Methods 0.000 claims description 16
- 238000001914 filtration Methods 0.000 claims description 16
- 239000000243 solution Substances 0.000 claims description 16
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 12
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims description 11
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 10
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 10
- HRPVXLWXLXDGHG-UHFFFAOYSA-N Acrylamide Chemical compound NC(=O)C=C HRPVXLWXLXDGHG-UHFFFAOYSA-N 0.000 claims description 10
- 239000011837 N,N-methylenebisacrylamide Substances 0.000 claims description 10
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 claims description 10
- QANIADJLTJYOFI-UHFFFAOYSA-K aluminum;magnesium;carbonate;hydroxide;hydrate Chemical compound O.[OH-].[Mg+2].[Al+3].[O-]C([O-])=O QANIADJLTJYOFI-UHFFFAOYSA-K 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- ZIUHHBKFKCYYJD-UHFFFAOYSA-N n,n'-methylenebisacrylamide Chemical compound C=CC(=O)NCNC(=O)C=C ZIUHHBKFKCYYJD-UHFFFAOYSA-N 0.000 claims description 10
- 230000032683 aging Effects 0.000 claims description 9
- 239000003999 initiator Substances 0.000 claims description 9
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 8
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical group CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 8
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 8
- 239000007864 aqueous solution Substances 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- 238000000227 grinding Methods 0.000 claims description 8
- 238000004898 kneading Methods 0.000 claims description 8
- ZGSOBQAJAUGRBK-UHFFFAOYSA-N propan-2-olate;zirconium(4+) Chemical group [Zr+4].CC(C)[O-].CC(C)[O-].CC(C)[O-].CC(C)[O-] ZGSOBQAJAUGRBK-UHFFFAOYSA-N 0.000 claims description 8
- 238000002791 soaking Methods 0.000 claims description 8
- 239000007787 solid Substances 0.000 claims description 8
- 238000000352 supercritical drying Methods 0.000 claims description 8
- 238000009210 therapy by ultrasound Methods 0.000 claims description 8
- 238000004132 cross linking Methods 0.000 claims description 3
- 238000007789 sealing Methods 0.000 abstract description 4
- 239000011162 core material Substances 0.000 abstract 1
- 239000002245 particle Substances 0.000 abstract 1
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 description 7
- 230000000694 effects Effects 0.000 description 4
- 239000010410 layer Substances 0.000 description 4
- 230000009044 synergistic interaction Effects 0.000 description 3
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- 239000010936 titanium Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009435 building construction Methods 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000002309 gasification Methods 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 239000004926 polymethyl methacrylate Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000003566 sealing material Substances 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 150000003608 titanium Chemical class 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J1/00—Adhesives based on inorganic constituents
- C09J1/02—Adhesives based on inorganic constituents containing water-soluble alkali silicates
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J123/00—Adhesives based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Adhesives based on derivatives of such polymers
- C09J123/02—Adhesives based on homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Adhesives based on derivatives of such polymers not modified by chemical after-treatment
- C09J123/18—Homopolymers or copolymers of hydrocarbons having four or more carbon atoms
- C09J123/20—Homopolymers or copolymers of hydrocarbons having four or more carbon atoms having four to nine carbon atoms
- C09J123/22—Copolymers of isobutene; Butyl rubber ; Homo- or copolymers of other iso-olefines
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2217—Oxides; Hydroxides of metals of magnesium
- C08K2003/2224—Magnesium hydroxide
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2227—Oxides; Hydroxides of metals of aluminium
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/24—Acids; Salts thereof
- C08K3/26—Carbonates; Bicarbonates
- C08K2003/265—Calcium, strontium or barium carbonate
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/014—Additives containing two or more different additives of the same subgroup in C08K
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Sealing Material Composition (AREA)
- Polymerisation Methods In General (AREA)
Abstract
The invention discloses a fire-proof sealant based on synergy of aerogel and nano-hydrotalcite, which takes sodium silicate and polyisobutylene as matrix adhesives, nano-aluminum hydroxide and nano-magnesium hydroxide as composite flame retardants, nano-calcium carbonate as fillers, modified aerogel and modified nano-hydrotalcite as synergistic agents, and a coupling agent is added; the modified aerogel is prepared by taking silicon/zirconium composite aerogel particles as a core material and taking a polymer as a wall material; the modified nano hydrotalcite is prepared by inserting dodecyl sulfonate groups between nano hydrotalcite layers and adding a polymer monomer solution for in-situ polymerization modification. The invention also discloses a preparation method of the fireproof sealant; the fireproof sealant provided by the invention has good sealing performance, fireproof performance and mechanical performance, and is simple to prepare.
Description
The technical field is as follows:
the invention relates to the field of high polymer materials, in particular to a fire-proof sealant based on synergistic interaction of aerogel and nano-hydrotalcite and a preparation method thereof.
Background art:
in building construction, a large number of mechanical and electrical pipes are criss-crossed between the floor and the wall due to the required functions and structures. Thus, it results in many voids between the floor and the duct, or between the wall and the duct. These pores should be sealed, so that smoke will spread rapidly and expand rapidly in case of building fire. The fireproof sealant is a sealing material for plugging and has double performances of sealing and fire prevention. The existing fireproof sealant is a lot, but the sealant with both excellent fireproof performance and excellent mechanical performance is difficult to meet the requirements of users. Therefore, the development of high-performance sealant is imminent.
The invention content is as follows:
the technical problem to be solved by the invention is to provide a fire-proof sealant based on synergy of aerogel and nano-hydrotalcite aiming at the defects of the prior art; according to the invention, the modified aerogel and the modified nano hydrotalcite are used as the synergistic agent of the flame retardant, and the prepared sealant has good sealing performance, fire resistance and mechanical property.
The invention also discloses a preparation method of the aerogel and nano-hydrotalcite synergistic fireproof sealant, which is simple to operate and low in preparation cost.
In order to better solve the technical problems, the invention adopts the following technical scheme:
the fire-proof sealant based on synergy of aerogel and nano-hydrotalcite takes sodium silicate and polyisobutylene as matrix adhesives, nano-aluminum hydroxide and nano-magnesium hydroxide as composite flame retardants, nano-calcium carbonate as fillers, modified aerogel and modified nano-hydrotalcite as synergistic agents, and a coupling agent is added; the modified aerogel is prepared by taking silicon/zirconium composite aerogel as a matrix and adding a polymer for crosslinking modification; the modified nano hydrotalcite is prepared by inserting dodecyl sulfonate groups between nano hydrotalcite layers and adding a polymer monomer solution for in-situ polymerization modification.
Preferably, in the technical scheme, the fireproof sealant comprises the following components in parts by weight: 35-45 parts of sodium silicate, 15-20 parts of polyisobutylene, 3-5 parts of nano aluminum hydroxide, 3-5 parts of nano magnesium hydroxide, 20-30 parts of nano calcium carbonate, 1-3 parts of modified aerogel, 2-3 parts of modified nano hydrotalcite and 0.5-1 part of coupling agent.
As a preferred aspect of the above technical solution, the preparation method of the modified aerogel specifically comprises: firstly, adding a silicon source and a zirconium source into a mixed solution of absolute ethyl alcohol and isopropanol, then dropwise adding deionized water for mixing, dropwise adding hydrochloric acid into the mixed solution after uniformly mixing, and adjusting the pH value of the mixed solution to 1-2; stirring and reacting for 1.5-3.5 h at normal temperature, and slowly dropwise adding ammonia water into the reaction system after the reaction is finished to prepare wet gel containing silicon/zirconium; aging the silicon/zirconium-containing wet gel in a water bath at 50-60 ℃, placing the gel in ethanol of a silane coupling agent for standing for 1-4 h, taking out the gel, performing supercritical drying, adding the dried aerogel into an aqueous solution of methyl methacrylate, performing soaking treatment for 2-4 h, adding potassium persulfate, reacting for 2-3 h at 60-70 ℃, and naturally cooling to room temperature after the reaction is finished to obtain the modified aerogel.
Preferably, in the above technical solution, the silicon source is tetraethyl silicate; the zirconium source is zirconium isopropoxide.
Preferably, in the technical scheme, the molar ratio of the silicon source to the zirconium source to the absolute ethyl alcohol to the isopropanol to the deionized water is 1:1:5:5: 7.
Preferably, in the above technical solution, the mass ratio of the silicon/zirconium-containing wet gel to the methyl methacrylate to the silane coupling agent to the potassium persulfate is 1: (0.2-0.3): (0.01-0.02): 0.001.
preferably, the preparation method of the modified nano hydrotalcite comprises the following steps: adding nano hydrotalcite powder into an ethanol solution of sodium dodecyl sulfate, carrying out ultrasonic treatment, then adding acrylic acid, acrylamide and N, N-methylene bisacrylamide, stirring and mixing, then continuously adding potassium persulfate serving as an initiator, reacting for 2-4 hours at the temperature of 60-80 ℃, and cooling to room temperature after the reaction is finished; filtering, drying the solid obtained by filtering, and grinding to obtain the modified nano hydrotalcite.
Preferably, in the technical scheme, the mass ratio of the nano hydrotalcite powder, the sodium dodecyl sulfate, the acrylic acid, the acrylamide, the N, N-methylene bisacrylamide and the potassium persulfate is 5: 0.001: (0.8-1.2): 0.5:0.001: (0.001-0.003).
In order to better solve the technical problems, the technical scheme adopted by the invention is as follows:
a preparation method of a fire-proof sealant based on synergy of aerogel and nano-hydrotalcite comprises the following steps:
(1) adding sodium silicate and polyisobutylene into a kneading machine for mixing treatment; then adding a coupling agent, nano aluminum hydroxide, nano magnesium hydroxide and nano calcium carbonate, and continuously mixing to prepare a mixed material;
(2) and continuously adding the modified aerogel and the modified nano hydrotalcite into the mixed material, and uniformly stirring and mixing to obtain the fireproof sealant.
Due to the adoption of the technical scheme, the invention has the following beneficial effects:
the invention provides a fire-proof sealant based on aerogel and nano-hydrotalcite synergistic interaction, which takes sodium silicate and polyisobutylene as matrix adhesives, nano-aluminum hydroxide and nano-magnesium hydroxide as composite flame retardants, nano-calcium carbonate as fillers, modified aerogel and modified nano-hydrotalcite as synergistic interaction agents, and a coupling agent is added; the modified aerogel is prepared by taking silicon/zirconium composite aerogel as a matrix and adding a polymer for crosslinking modification; the modified nano hydrotalcite is prepared by inserting dodecyl sulfonate groups between nano hydrotalcite layers and adding a polymer monomer solution for in-situ polymerization modification. The nano magnesium hydroxide and the nano aluminum hydroxide are used as flame retardants, can release crystal water after being heated, and can effectively absorb ambient heat for gasification, so that the combustible gas is diluted, and the flame retardant effect is achieved; and the activity is high, a compact carbonized film can be formed on the surface of the flame retardant, and the flame retardant is further realized. The aerogel has good adsorptivity, high activity and good heat-insulating property; and the porous structure of the aerogel can adsorb crystal water released by heating nano magnesium hydroxide and nano aluminum hydroxide, and promote the generation of metal oxide, thereby promoting the formation of a carbonized film on the surface of a flame-retardant object. The nano hydrotalcite material has high activity, interlayer water can be removed when the nano hydrotalcite material is heated, and a large amount of heat is absorbed, so that water vapor is released to dilute combustible gas, and the formation of a carbonized film on the surface of a flame-retardant object is promoted; the fireproof and flame-retardant performance of the sealant is improved.
In the process of preparing the fireproof sealant, firstly, preparing titanium/zirconium-containing wet gel, then, aging the wet gel, and adding the aged wet gel into an ethanol solution of a silane coupling agent for reaction; the titanium/zirconium gel network structure contains a large number of active groups which can be effectively combined with a silane coupling agent, then methyl methacrylate is added, and an initiator is added for reaction, so as to prepare the polymethyl methacrylate modified titanium/zirconium aerogel; the dispersion is good, and the mechanical property is excellent. Although the nano hydrotalcite material has excellent performance, the compatibility of the nano hydrotalcite material and matrix glue is poor; according to the invention, dodecyl sulfonate is inserted between layers of the nano hydrotalcite to increase the distance between the layers, and then the nano hydrotalcite is added into a polymer monomer solution, and the nano hydrotalcite is stripped in the process of polymer polymerization, so that the prepared modified hydrotalcite material has good dispersibility and good compatibility with a matrix. The sealant prepared by the invention has good sealing performance, fire resistance and mechanical property.
The specific implementation mode is as follows:
the present invention is further illustrated by the following examples, which are provided for the purpose of illustration only and are not intended to be limiting.
Example 1
A fire-proof sealant based on synergy of aerogel and nano hydrotalcite comprises the following components in parts by weight: 35 parts of sodium silicate, 15 parts of polyisobutylene, 3 parts of nano aluminum hydroxide, 3 parts of nano magnesium hydroxide, 20 parts of nano calcium carbonate, 1 part of modified aerogel, 2 parts of modified nano hydrotalcite and 0.5 part of coupling agent;
the preparation method comprises the following steps:
(1) firstly, adding 1mol of tetraethyl silicate and 1mol of zirconium isopropoxide into a mixed solution of 5mol of absolute ethyl alcohol and 5mol of isopropanol, then dropwise adding 7mol of deionized water for mixing, dropwise adding hydrochloric acid into the mixed solution after uniform mixing, and adjusting the pH value of the mixed solution to 1-2; stirring and reacting for 1.5h at normal temperature, and slowly dripping ammonia water into a reaction system after the reaction is finished to prepare wet gel containing silicon/zirconium; aging a silicon/zirconium-containing wet gel in a water bath at 50 ℃, placing 10g of the aged gel in ethanol containing 0.1g of silane coupling agent for standing treatment for 1h, taking out the gel and then performing supercritical drying, adding the dried aerogel into an aqueous solution containing 2g of methyl methacrylate, soaking for 2h, adding 0.01g of potassium persulfate, reacting for 2h at 60 ℃, and naturally cooling to room temperature after the reaction is finished to obtain the modified aerogel;
(2) adding 5g of nano hydrotalcite powder into an ethanol solution containing 0.001g of sodium dodecyl sulfate, carrying out ultrasonic treatment, then adding 0.8g of acrylic acid, 0.5g of acrylamide and 0.001g of N, N-methylene bisacrylamide, stirring and mixing, then continuously adding 0.001g of potassium persulfate serving as an initiator, reacting for 2 hours at the temperature of 60 ℃, and cooling to room temperature after the reaction is finished; filtering, drying the solid obtained by filtering, and then grinding to obtain modified nano hydrotalcite;
(3) adding sodium silicate and polyisobutylene into a kneading machine for mixing treatment; then adding a coupling agent, nano aluminum hydroxide, nano magnesium hydroxide and nano calcium carbonate, and continuously mixing to prepare a mixed material; and continuously adding the modified aerogel and the modified nano hydrotalcite into the mixed material, and uniformly stirring and mixing to obtain the fireproof sealant.
Example 2
A fire-proof sealant based on synergy of aerogel and nano hydrotalcite comprises the following components in parts by weight: 45 parts of sodium silicate, 20 parts of polyisobutylene, 5 parts of nano aluminum hydroxide, 5 parts of nano magnesium hydroxide, 30 parts of nano calcium carbonate, 3 parts of modified aerogel, 3 parts of modified nano hydrotalcite and 1 part of coupling agent;
the preparation method comprises the following steps:
(1) firstly, adding 1mol of tetraethyl silicate and 1mol of zirconium isopropoxide into a mixed solution of 5mol of absolute ethyl alcohol and 5mol of isopropanol, then dropwise adding 7mol of deionized water for mixing, dropwise adding hydrochloric acid into the mixed solution after uniform mixing, and adjusting the pH value of the mixed solution to 1-2; stirring and reacting for 3.5h at normal temperature, and slowly dripping ammonia water into a reaction system after the reaction is finished to prepare wet gel containing silicon/zirconium; aging a silicon/zirconium-containing wet gel in a water bath at 60 ℃, placing 10g of the aged gel in ethanol containing 0.2g of silane coupling agent for standing treatment for 4h, taking out the gel, performing supercritical drying, adding the dried aerogel into an aqueous solution containing 3g of methyl methacrylate, soaking for 4h, adding 0.01g of potassium persulfate, reacting for 3h at 70 ℃, and naturally cooling to room temperature after the reaction is finished to obtain the modified aerogel;
(2) adding 5g of nano hydrotalcite powder into an ethanol solution containing 0.001g of sodium dodecyl sulfate, carrying out ultrasonic treatment, then adding 1.2g of acrylic acid, 0.5g of acrylamide and 0.001g of N, N-methylene bisacrylamide, stirring and mixing, then continuously adding 0.003g of potassium persulfate as an initiator, reacting for 4 hours at 80 ℃, and cooling to room temperature after the reaction is finished; filtering, drying the solid obtained by filtering, and then grinding to obtain modified nano hydrotalcite;
(3) adding sodium silicate and polyisobutylene into a kneading machine for mixing treatment; then adding a coupling agent, nano aluminum hydroxide, nano magnesium hydroxide and nano calcium carbonate, and continuously mixing to prepare a mixed material; and continuously adding the modified aerogel and the modified nano hydrotalcite into the mixed material, and uniformly stirring and mixing to obtain the fireproof sealant.
Example 3
A fire-proof sealant based on synergy of aerogel and nano hydrotalcite comprises the following components in parts by weight: 37 parts of sodium silicate, 16 parts of polyisobutylene, 3.5 parts of nano aluminum hydroxide, 3.5 parts of nano magnesium hydroxide, 22 parts of nano calcium carbonate, 1.5 parts of modified aerogel, 2.5 parts of modified nano hydrotalcite and 0.6 part of coupling agent;
the preparation method comprises the following steps:
(1) firstly, adding 1mol of tetraethyl silicate and 1mol of zirconium isopropoxide into a mixed solution of 5mol of absolute ethyl alcohol and 5mol of isopropanol, then dropwise adding 7mol of deionized water for mixing, dropwise adding hydrochloric acid into the mixed solution after uniform mixing, and adjusting the pH value of the mixed solution to 1-2; stirring and reacting for 2h at normal temperature, and slowly dripping ammonia water into a reaction system after the reaction is finished to prepare wet gel containing silicon/zirconium; aging a silicon/zirconium-containing wet gel in a water bath at 50 ℃, placing 10g of the aged gel in ethanol containing 0.12g of silane coupling agent for standing treatment for 2 hours, taking out the gel and then performing supercritical drying, adding the dried aerogel into an aqueous solution containing 2.5g of methyl methacrylate, soaking for 2.5 hours, adding 0.01g of potassium persulfate, reacting for 2.5 hours at 60 ℃, and naturally cooling to room temperature after the reaction is finished to obtain the modified aerogel;
(2) adding 5g of nano hydrotalcite powder into an ethanol solution containing 0.001g of sodium dodecyl sulfate, carrying out ultrasonic treatment, then adding 0.9g of acrylic acid, 0.5g of acrylamide and 0.001g of N, N-methylene bisacrylamide, stirring and mixing, then continuously adding 0.0015g of potassium persulfate as an initiator, reacting for 2.5h at 65 ℃, and cooling to room temperature after the reaction is finished; filtering, drying the solid obtained by filtering, and then grinding to obtain modified nano hydrotalcite;
(3) adding sodium silicate and polyisobutylene into a kneading machine for mixing treatment; then adding a coupling agent, nano aluminum hydroxide, nano magnesium hydroxide and nano calcium carbonate, and continuously mixing to prepare a mixed material; and continuously adding the modified aerogel and the modified nano hydrotalcite into the mixed material, and uniformly stirring and mixing to obtain the fireproof sealant.
Example 4
A fire-proof sealant based on synergy of aerogel and nano hydrotalcite comprises the following components in parts by weight: 40 parts of sodium silicate, 17 parts of polyisobutylene, 4 parts of nano aluminum hydroxide, 4 parts of nano magnesium hydroxide, 24 parts of nano calcium carbonate, 2 parts of modified aerogel, 3 parts of modified nano hydrotalcite and 0.7 part of coupling agent;
the preparation method comprises the following steps:
(1) firstly, adding 1mol of tetraethyl silicate and 1mol of zirconium isopropoxide into a mixed solution of 5mol of absolute ethyl alcohol and 5mol of isopropanol, then dropwise adding 7mol of deionized water for mixing, dropwise adding hydrochloric acid into the mixed solution after uniform mixing, and adjusting the pH value of the mixed solution to 1-2; stirring and reacting for 2.5h at normal temperature, and slowly dripping ammonia water into a reaction system after the reaction is finished to prepare wet gel containing silicon/zirconium; aging a silicon/zirconium-containing wet gel in a water bath at 60 ℃, placing 10g of the aged gel in ethanol containing 0.14g of silane coupling agent for standing treatment for 2h, taking out the gel and then performing supercritical drying, adding the dried aerogel into an aqueous solution containing 2g of methyl methacrylate, soaking for 3h, adding 0.01g of potassium persulfate, reacting for 2h at 60 ℃, and naturally cooling to room temperature after the reaction is finished to obtain the modified aerogel;
(2) adding 5g of nano hydrotalcite powder into an ethanol solution containing 0.001g of sodium dodecyl sulfate, carrying out ultrasonic treatment, then adding 1g of acrylic acid, 0.5g of acrylamide and 0.001g of N, N-methylene bisacrylamide, stirring and mixing, continuously adding 0.002g of potassium persulfate serving as an initiator, reacting for 3 hours at 70 ℃, and cooling to room temperature after the reaction is finished; filtering, drying the solid obtained by filtering, and then grinding to obtain modified nano hydrotalcite;
(3) adding sodium silicate and polyisobutylene into a kneading machine for mixing treatment; then adding a coupling agent, nano aluminum hydroxide, nano magnesium hydroxide and nano calcium carbonate, and continuously mixing to prepare a mixed material; and continuously adding the modified aerogel and the modified nano hydrotalcite into the mixed material, and uniformly stirring and mixing to obtain the fireproof sealant.
Example 5
A fire-proof sealant based on synergy of aerogel and nano hydrotalcite comprises the following components in parts by weight: 41 parts of sodium silicate, 18 parts of polyisobutylene, 4.5 parts of nano aluminum hydroxide, 4.5 parts of nano magnesium hydroxide, 26 parts of nano calcium carbonate, 2 parts of modified aerogel, 2 parts of modified nano hydrotalcite and 0.5 part of coupling agent;
the preparation method comprises the following steps:
(1) firstly, adding 1mol of tetraethyl silicate and 1mol of zirconium isopropoxide into a mixed solution of 5mol of absolute ethyl alcohol and 5mol of isopropanol, then dropwise adding 7mol of deionized water for mixing, dropwise adding hydrochloric acid into the mixed solution after uniform mixing, and adjusting the pH value of the mixed solution to 1-2; stirring and reacting for 2h at normal temperature, and slowly dripping ammonia water into a reaction system after the reaction is finished to prepare wet gel containing silicon/zirconium; aging a silicon/zirconium-containing wet gel in a water bath at 60 ℃, placing 10g of the aged gel in ethanol containing 0.16g of silane coupling agent for standing treatment for 3.5h, taking out the gel, performing supercritical drying, adding the dried aerogel into an aqueous solution containing 3g of methyl methacrylate, soaking for 3.5h, adding 0.01g of potassium persulfate, reacting for 2h at 70 ℃, and naturally cooling to room temperature after the reaction is finished to obtain the modified aerogel;
(2) adding 5g of nano hydrotalcite powder into an ethanol solution containing 0.001g of sodium dodecyl sulfate, carrying out ultrasonic treatment, then adding 1g of acrylic acid, 0.5g of acrylamide and 0.001g of N, N-methylene bisacrylamide, stirring and mixing, continuously adding 0.0025g of potassium persulfate serving as an initiator, reacting for 3.5 hours at 75 ℃, and cooling to room temperature after the reaction is finished; filtering, drying the solid obtained by filtering, and then grinding to obtain modified nano hydrotalcite;
(3) adding sodium silicate and polyisobutylene into a kneading machine for mixing treatment; then adding a coupling agent, nano aluminum hydroxide, nano magnesium hydroxide and nano calcium carbonate, and continuously mixing to prepare a mixed material; and continuously adding the modified aerogel and the modified nano hydrotalcite into the mixed material, and uniformly stirring and mixing to obtain the fireproof sealant.
Example 6
A fire-proof sealant based on synergy of aerogel and nano hydrotalcite comprises the following components in parts by weight: 42 parts of sodium silicate, 19 parts of polyisobutylene, 4 parts of nano aluminum hydroxide, 4 parts of nano magnesium hydroxide, 28 parts of nano calcium carbonate, 3 parts of modified aerogel, 2 parts of modified nano hydrotalcite and 0.5 part of coupling agent;
the preparation method comprises the following steps:
(1) firstly, adding 1mol of tetraethyl silicate and 1mol of zirconium isopropoxide into a mixed solution of 5mol of absolute ethyl alcohol and 5mol of isopropanol, then dropwise adding 7mol of deionized water for mixing, dropwise adding hydrochloric acid into the mixed solution after uniform mixing, and adjusting the pH value of the mixed solution to 1-2; stirring and reacting for 3h at normal temperature, and slowly dripping ammonia water into a reaction system after the reaction is finished to prepare wet gel containing silicon/zirconium; aging a silicon/zirconium-containing wet gel in a water bath at 60 ℃, placing 10g of the aged gel in ethanol containing 0.1g of silane coupling agent for standing treatment for 4 hours, taking out the gel, performing supercritical drying, adding the dried aerogel into an aqueous solution containing 3g of methyl methacrylate, soaking for 2 hours, adding 0.01g of potassium persulfate, reacting for 3 hours at 70 ℃, and naturally cooling to room temperature after the reaction is finished to obtain the modified aerogel;
(2) adding 5g of nano hydrotalcite powder into an ethanol solution containing 0.001g of sodium dodecyl sulfate, carrying out ultrasonic treatment, then adding 1g of acrylic acid, 0.5g of acrylamide and 0.001g of N, N-methylene bisacrylamide, stirring and mixing, continuously adding 0.002g of potassium persulfate serving as an initiator, reacting for 3 hours at 80 ℃, and cooling to room temperature after the reaction is finished; filtering, drying the solid obtained by filtering, and then grinding to obtain modified nano hydrotalcite;
(3) adding sodium silicate and polyisobutylene into a kneading machine for mixing treatment; then adding a coupling agent, nano aluminum hydroxide, nano magnesium hydroxide and nano calcium carbonate, and continuously mixing to prepare a mixed material; and continuously adding the modified aerogel and the modified nano hydrotalcite into the mixed material, and uniformly stirring and mixing to obtain the fireproof sealant.
Comparative example 1
The aerogel and the nano hydrotalcite added into the fireproof sealant are not modified, and other preparation conditions are the same as those in the example 6.
Comparative example 2
The modified aerogel and the modified hydrotalcite are not added into the sealant, and other preparation conditions are the same as those in the example 6.
The performance of the prepared fire-proof sealant is tested as follows, and the test results are shown in table 1:
TABLE 1
From the test results, the modified aerogel and the modified nano hydrotalcite are added into the sealant, so that the fireproof performance of the sealant can be effectively improved under the condition that the mechanical property of the matrix is not influenced, and the mechanical property of the matrix is also effectively improved.
Although specific embodiments of the invention have been described, many other forms and modifications of the invention will be apparent to those skilled in the art. It is to be understood that the appended claims and this invention generally cover all such obvious forms and modifications which are within the true spirit and scope of the present invention.
Claims (9)
1. A fire-proof sealant based on synergy of aerogel and nano-hydrotalcite is characterized in that: the fireproof sealant takes sodium silicate and polyisobutylene as matrix adhesives, nano aluminum hydroxide and nano magnesium hydroxide as composite flame retardants, nano calcium carbonate as a filler, modified aerogel and modified nano hydrotalcite as synergistic agents, and a coupling agent is added; the modified aerogel is prepared by taking silicon/zirconium composite aerogel as a matrix and adding a polymer for crosslinking modification; the modified nano hydrotalcite is prepared by inserting dodecyl sulfonate groups between nano hydrotalcite layers and adding a polymer monomer solution for in-situ polymerization modification.
2. The aerogel and nano hydrotalcite synergistic fireproof sealant as claimed in claim 1, which is characterized in that: the fireproof sealant comprises the following components in parts by weight: 35-45 parts of sodium silicate, 15-20 parts of polyisobutylene, 3-5 parts of nano aluminum hydroxide, 3-5 parts of nano magnesium hydroxide, 20-30 parts of nano calcium carbonate, 1-3 parts of modified aerogel, 2-3 parts of modified nano hydrotalcite and 0.5-1 part of coupling agent.
3. The aerogel and nano hydrotalcite synergistic fireproof sealant as claimed in claim 1, which is characterized in that: the preparation method of the modified aerogel comprises the following steps: firstly, adding a silicon source and a zirconium source into a mixed solution of absolute ethyl alcohol and isopropanol, then dropwise adding deionized water for mixing, dropwise adding hydrochloric acid into the mixed solution after uniformly mixing, and adjusting the pH value of the mixed solution to 1-2; stirring and reacting for 1.5-3.5 h at normal temperature, and slowly dropwise adding ammonia water into the reaction system after the reaction is finished to prepare wet gel containing silicon/zirconium; aging the silicon/zirconium-containing wet gel in a water bath at 50-60 ℃, placing the gel in ethanol of a silane coupling agent for standing for 1-4 h, taking out the gel, performing supercritical drying, adding the dried aerogel into an aqueous solution of methyl methacrylate, performing soaking treatment for 2-4 h, adding potassium persulfate, reacting for 2-3 h at 60-70 ℃, and naturally cooling to room temperature after the reaction is finished to obtain the modified aerogel.
4. The aerogel and nano hydrotalcite synergistic fireproof sealant as claimed in claim 3, characterized in that: the silicon source is tetraethyl silicate; the zirconium source is zirconium isopropoxide.
5. The aerogel and nano hydrotalcite synergistic fireproof sealant as claimed in claim 3, characterized in that: the molar ratio of the silicon source to the zirconium source to the absolute ethyl alcohol to the isopropanol to the deionized water is 1:1:5:5: 7.
6. The aerogel and nano hydrotalcite synergistic fireproof sealant as claimed in claim 3, characterized in that: the mass ratio of the silicon/zirconium-containing wet gel to the methyl methacrylate to the silane coupling agent to the potassium persulfate is 1: (0.2-0.3): (0.01-0.02): 0.001.
7. the aerogel and nano hydrotalcite synergistic fireproof sealant as claimed in claim 1, which is characterized in that: the preparation method of the modified nano hydrotalcite comprises the following steps: adding nano hydrotalcite powder into an ethanol solution of sodium dodecyl sulfate, carrying out ultrasonic treatment, then adding acrylic acid, acrylamide and N, N-methylene bisacrylamide, stirring and mixing, then continuously adding potassium persulfate serving as an initiator, reacting for 2-4 hours at the temperature of 60-80 ℃, and cooling to room temperature after the reaction is finished; filtering, drying the solid obtained by filtering, and grinding to obtain the modified nano hydrotalcite.
8. The aerogel and nano hydrotalcite synergistic fireproof sealant as claimed in claim 7, wherein: the mass ratio of the nano hydrotalcite powder, sodium dodecyl sulfate, acrylic acid, acrylamide, N, N-methylene bisacrylamide and potassium persulfate is 5: 0.001: (0.8-1.2): 0.5:0.001: (0.001-0.003).
9. The preparation method of the aerogel and nano hydrotalcite synergistic fireproof sealant according to any one of claims 1 to 8, which is characterized by comprising the following steps:
(1) adding sodium silicate and polyisobutylene into a kneading machine for mixing treatment; then adding a coupling agent, nano aluminum hydroxide, nano magnesium hydroxide and nano calcium carbonate, and continuously mixing to prepare a mixed material;
(2) and continuously adding the modified aerogel and the modified nano hydrotalcite into the mixed material, and uniformly stirring and mixing to obtain the fireproof sealant.
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