CN116120007A - Antioxidant cement-based waterproof material and preparation process thereof - Google Patents
Antioxidant cement-based waterproof material and preparation process thereof Download PDFInfo
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- CN116120007A CN116120007A CN202211698291.7A CN202211698291A CN116120007A CN 116120007 A CN116120007 A CN 116120007A CN 202211698291 A CN202211698291 A CN 202211698291A CN 116120007 A CN116120007 A CN 116120007A
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- Prior art keywords
- aluminate
- phthalonitrile
- cement
- mass
- continuously stirring
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- 239000004568 cement Substances 0.000 title claims abstract description 93
- 239000000463 material Substances 0.000 title claims abstract description 78
- 230000003078 antioxidant effect Effects 0.000 title claims abstract description 28
- 239000003963 antioxidant agent Substances 0.000 title claims abstract description 21
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- -1 o-phthalonitrile aluminate Chemical class 0.000 claims abstract description 146
- 229920006391 phthalonitrile polymer Polymers 0.000 claims abstract description 114
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 34
- 238000002156 mixing Methods 0.000 claims abstract description 26
- 235000008733 Citrus aurantifolia Nutrition 0.000 claims abstract description 17
- 235000011941 Tilia x europaea Nutrition 0.000 claims abstract description 17
- 239000004571 lime Substances 0.000 claims abstract description 17
- 239000004576 sand Substances 0.000 claims abstract description 17
- 230000003064 anti-oxidating effect Effects 0.000 claims abstract description 16
- FAIAAWCVCHQXDN-UHFFFAOYSA-N phosphorus trichloride Chemical compound ClP(Cl)Cl FAIAAWCVCHQXDN-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910052602 gypsum Inorganic materials 0.000 claims abstract description 14
- 239000010440 gypsum Substances 0.000 claims abstract description 14
- 238000003756 stirring Methods 0.000 claims description 177
- 238000010438 heat treatment Methods 0.000 claims description 51
- KKEYFWRCBNTPAC-UHFFFAOYSA-N Terephthalic acid Chemical compound OC(=O)C1=CC=C(C(O)=O)C=C1 KKEYFWRCBNTPAC-UHFFFAOYSA-N 0.000 claims description 48
- 238000001816 cooling Methods 0.000 claims description 34
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 27
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 26
- 239000000243 solution Substances 0.000 claims description 25
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 24
- 230000003647 oxidation Effects 0.000 claims description 19
- 238000007254 oxidation reaction Methods 0.000 claims description 19
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 18
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 18
- LPNYRYFBWFDTMA-UHFFFAOYSA-N potassium tert-butoxide Chemical compound [K+].CC(C)(C)[O-] LPNYRYFBWFDTMA-UHFFFAOYSA-N 0.000 claims description 18
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 17
- HEDRZPFGACZZDS-UHFFFAOYSA-N Chloroform Chemical compound ClC(Cl)Cl HEDRZPFGACZZDS-UHFFFAOYSA-N 0.000 claims description 16
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 16
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 16
- 229910052782 aluminium Inorganic materials 0.000 claims description 16
- JQWHASGSAFIOCM-UHFFFAOYSA-M sodium periodate Chemical compound [Na+].[O-]I(=O)(=O)=O JQWHASGSAFIOCM-UHFFFAOYSA-M 0.000 claims description 16
- 238000010025 steaming Methods 0.000 claims description 16
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 claims description 16
- FYSNRJHAOHDILO-UHFFFAOYSA-N thionyl chloride Chemical compound ClS(Cl)=O FYSNRJHAOHDILO-UHFFFAOYSA-N 0.000 claims description 13
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 10
- 239000001257 hydrogen Substances 0.000 claims description 10
- 229910052739 hydrogen Inorganic materials 0.000 claims description 10
- 229910052786 argon Inorganic materials 0.000 claims description 9
- ZVVXVFDNCIMZHX-UHFFFAOYSA-N iodo-methyl-triphenyl-$l^{5}-phosphane Chemical compound C=1C=CC=CC=1P(I)(C=1C=CC=CC=1)(C)C1=CC=CC=C1 ZVVXVFDNCIMZHX-UHFFFAOYSA-N 0.000 claims description 9
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 9
- 239000011780 sodium chloride Substances 0.000 claims description 9
- LIOBPVZSSVYQSS-UHFFFAOYSA-N 2-(3,4-diaminophenyl)acetic acid Chemical compound NC1=CC=C(CC(O)=O)C=C1N LIOBPVZSSVYQSS-UHFFFAOYSA-N 0.000 claims description 8
- MPAIWVOBMLSHQA-UHFFFAOYSA-N 3,6-dihydroxybenzene-1,2-dicarbonitrile Chemical compound OC1=CC=C(O)C(C#N)=C1C#N MPAIWVOBMLSHQA-UHFFFAOYSA-N 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 8
- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 claims description 8
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 claims description 8
- UKVIEHSSVKSQBA-UHFFFAOYSA-N methane;palladium Chemical compound C.[Pd] UKVIEHSSVKSQBA-UHFFFAOYSA-N 0.000 claims description 5
- 239000011398 Portland cement Substances 0.000 claims description 2
- 239000006004 Quartz sand Substances 0.000 claims description 2
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 229960002523 mercuric chloride Drugs 0.000 claims description 2
- LWJROJCJINYWOX-UHFFFAOYSA-L mercury dichloride Chemical compound Cl[Hg]Cl LWJROJCJINYWOX-UHFFFAOYSA-L 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 4
- 239000002982 water resistant material Substances 0.000 claims 1
- 239000004114 Ammonium polyphosphate Substances 0.000 abstract description 5
- 235000019826 ammonium polyphosphate Nutrition 0.000 abstract description 5
- 229920001276 ammonium polyphosphate Polymers 0.000 abstract description 5
- VMRIVYANZGSGRV-UHFFFAOYSA-N 4-phenyl-2h-triazin-5-one Chemical compound OC1=CN=NN=C1C1=CC=CC=C1 VMRIVYANZGSGRV-UHFFFAOYSA-N 0.000 abstract description 4
- 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 abstract description 2
- 239000003063 flame retardant Substances 0.000 abstract description 2
- 230000000052 comparative effect Effects 0.000 description 13
- RCTYPNKXASFOBE-UHFFFAOYSA-M chloromercury Chemical compound [Hg]Cl RCTYPNKXASFOBE-UHFFFAOYSA-M 0.000 description 6
- 239000012280 lithium aluminium hydride Substances 0.000 description 6
- 239000004952 Polyamide Substances 0.000 description 3
- 230000000694 effects Effects 0.000 description 3
- 229920002647 polyamide Polymers 0.000 description 3
- IOHPVZBSOKLVMN-UHFFFAOYSA-N 2-(2-phenylethyl)benzoic acid Chemical compound OC(=O)C1=CC=CC=C1CCC1=CC=CC=C1 IOHPVZBSOKLVMN-UHFFFAOYSA-N 0.000 description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 2
- KDLHZDBZIXYQEI-UHFFFAOYSA-N Palladium Chemical compound [Pd] KDLHZDBZIXYQEI-UHFFFAOYSA-N 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 235000011114 ammonium hydroxide Nutrition 0.000 description 2
- 239000011575 calcium Substances 0.000 description 2
- 229910052791 calcium Inorganic materials 0.000 description 2
- 239000000920 calcium hydroxide Substances 0.000 description 2
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 2
- OSGAYBCDTDRGGQ-UHFFFAOYSA-L calcium sulfate Chemical compound [Ca+2].[O-]S([O-])(=O)=O OSGAYBCDTDRGGQ-UHFFFAOYSA-L 0.000 description 2
- 239000004567 concrete Substances 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- HOOWDPSAHIOHCC-UHFFFAOYSA-N dialuminum tricalcium oxygen(2-) Chemical compound [O--].[O--].[O--].[O--].[O--].[O--].[Al+3].[Al+3].[Ca++].[Ca++].[Ca++] HOOWDPSAHIOHCC-UHFFFAOYSA-N 0.000 description 2
- MNUOZFHYBCRUOD-UHFFFAOYSA-N hydroxyphthalic acid Natural products OC(=O)C1=CC=CC(O)=C1C(O)=O MNUOZFHYBCRUOD-UHFFFAOYSA-N 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- WLJVXDMOQOGPHL-UHFFFAOYSA-N phenylacetic acid Chemical compound OC(=O)CC1=CC=CC=C1 WLJVXDMOQOGPHL-UHFFFAOYSA-N 0.000 description 2
- XNGIFLGASWRNHJ-UHFFFAOYSA-N phthalic acid Chemical compound OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 description 2
- 239000000654 additive Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
- 230000001070 adhesive effect Effects 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 150000001408 amides Chemical class 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 125000004093 cyano group Chemical group *C#N 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 229960003424 phenylacetic acid Drugs 0.000 description 1
- 239000003279 phenylacetic acid Substances 0.000 description 1
- 229920000412 polyarylene Polymers 0.000 description 1
- 230000001681 protective effect Effects 0.000 description 1
- 230000008707 rearrangement Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000007363 ring formation reaction Methods 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
Classifications
-
- 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
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/02—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing hydraulic cements other than calcium sulfates
- C04B28/04—Portland cements
-
- 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
-
- 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
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/20—Resistance against chemical, physical or biological attack
-
- 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
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/20—Resistance against chemical, physical or biological attack
- C04B2111/27—Water resistance, i.e. waterproof or water-repellent materials
-
- 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
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/20—Resistance against chemical, physical or biological attack
- C04B2111/28—Fire resistance, i.e. materials resistant to accidental fires or high temperatures
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/91—Use of waste materials as fillers for mortars or concrete
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
The invention discloses an antioxidant cement-based waterproof material and a preparation process thereof, and relates to the technical field of waterproof materials. The antioxidation cement-based waterproof material prepared by the invention comprises 30-50 parts of cement, 60-200 parts of siliceous fine sand, 20-42 parts of water, 15-34 parts of lime, 10-20 parts of o-phthalonitrile aluminate, 3-10 parts of phosphorus trichloride, 12-28 parts of polyarylamide and 24-60 parts of gypsum; firstly mixing phthalonitrile aluminate, lime and phosphorus trichloride in proportion to form antioxidative hydroxyphenyl triazine and flame-retardant ammonium polyphosphate, then adding cement base materials mixed by cement, siliceous fine sand and water, and adding polyarylamide to mix to prepare the antioxidative cement-based waterproof material; the antioxidation cement-based waterproof material prepared by the invention has strong antioxidation, flame retardance, thermal stability and waterproof property.
Description
Technical Field
The invention relates to the technical field of adhesives, in particular to an antioxidant cement-based waterproof material and a preparation process thereof.
Background
Along with the increasing of construction scale, the use of concrete is more and more extensive, but because the concrete wall body is easy to generate microcracks, the impermeability is poor, and the problems of basement seepage, bathroom seepage, wall seepage and the like are easy to occur in the house. Other waterproof materials with different action mechanisms basically face ageing problems, so that the waterproof effect can be exerted only in a short period of time, and leakage problems frequently occur at waterproof positions.
The cement-base waterproof material is prepared with cement, sand and stone as main material and through adding small amount of organic and inorganic additive to form one compact layer on the surface or inside of cement base material to prevent water from passing through. However, the cement-based waterproof material is a multiphase composite brittle material, so that cracks are easily generated in the cement-based material under the environment of high temperature difference, the waterproof performance is poor, and the service life of a building is seriously influenced. Therefore, the development of the antioxidation cement-based waterproof material with strong antioxidation, flame retardance, thermal stability and waterproofness has important social benefits.
Disclosure of Invention
The invention aims to provide an antioxidant cement-based waterproof material and a preparation process thereof, so as to solve the problems in the prior art.
In order to solve the technical problems, the invention provides the following technical scheme:
the antioxidation cement-based waterproof material comprises, by weight, 30-50 parts of cement, 60-200 parts of siliceous fine sand, 20-42 parts of water, 15-34 parts of lime, 10-20 parts of phthalonitrile aluminate, 3-10 parts of phosphorus trichloride, 12-28 parts of polyarylamide and 24-60 parts of gypsum.
Further, the cement is Portland cement.
Further, the siliceous fine sand is quartz sand of 70-140 meshes.
Further, a preparation process of the antioxidant cement-based waterproof material comprises the following steps: under the condition of 60-80 ℃ and argon protection, phthalonitrile aluminate, sodium periodate, tetrahydrofuran and water are mixed according to the mass ratio of 1:0.6:3:0.72 to 1:0.8:5.6:1.12 mixing, stirring for 110-130 min at 300-500 r/min, steaming for 1-3 h at 200-300 Pa and 100-102 ℃ at 1800-2000 r/min, adding methanol 3-5 times of phthalonitrile aluminate, continuously stirring for 30-50 min, cooling to 7-9 ℃, adding sulfoxide chloride 0.6-0.8 times of phthalonitrile aluminate, continuously stirring for 23-25 h, microwave treating for 40-60 min under 2400-2500 MHz and 700-900W microwave conditions, naturally cooling to room temperature, adding lime aqueous solution 1.5-1.7 times of phthalonitrile aluminate, heating to 60-80 ℃, continuously stirring for 2-4 h, increasing pressure to 1-3 MPa, adding phosphorus trichloride 0.3-0.5 times of phthalonitrile aluminate, continuously stirring for 30-50 min, heating to 280-300 ℃, continuously stirring for 1.5-2.5 h, then adding the mixture into a cement base material with 3-5 times of the mass of the phthalonitrile aluminate, stirring for 20-40 min at 100-200 r/min, adding the polyarylamide with 1.2-1.4 times of the mass of the phthalonitrile aluminate, heating to 140-160 ℃, continuously stirring for 11-13 h, cooling to 100-115 ℃, adding sodium chloride with 0.7-0.9 times of the mass of the phthalonitrile aluminate, continuously stirring for 5-7 h, adding palladium carbon with 0.09-0.11 times of the mass of the phthalonitrile aluminate, introducing hydrogen with 10-20 times of the mass of the phthalonitrile aluminate at 90-100 ℃ and 2-3 MPa, continuously stirring for 7-8 h, continuously stirring for 4-6 h after heating to 115-119 ℃, and then under the condition of 30-50 ℃ according to the mass ratio of 1:4: 9-1: 5:11 adding potassium tert-butoxide, methyl triphenyl phosphorus iodide and diethyl ether, wherein the mass of the potassium tert-butoxide is 0.4-0.6 times of that of the phthalonitrile aluminate, continuously stirring for 10-14 h, adding aluminum oxide with the mass of 1-3 times of that of the phthalonitrile aluminate, continuously stirring for 1-3 h, adding hydroxyl toluene sulfonyl iodobenzene with the mass of 0.8-1 times of that of the phthalonitrile aluminate, continuously stirring for 1-4 h at room temperature, continuously adding aluminum lithium hydride with the mass of 1-1.4 times of that of the phthalonitrile aluminate, continuously stirring for 0.8-1.2 h, and naturally cooling to room temperature to prepare the antioxidant cement-based waterproof material.
Further, the preparation method of the phthalonitrile aluminate comprises the following steps: aluminum, 3, 6-dihydroxyphthalonitrile and carbon tetrachloride are mixed according to the mass ratio of 1:18: 20-1: 19:22, stirring for 20-40 min at 100-200 r/min, then adding mercuric chloride with the mass of 0.019-0.021 times of that of aluminum, heating to 130-140 ℃, continuously stirring for 6-12 h, and performing rotary steaming for 3-5 h at 1800-2200 r/min at 10-20 Pa and 130-140 ℃ to prepare the o-phthalonitrile aluminate.
Further, the preparation method of the polyarylamide comprises the following steps: terephthalic acid and chloroform are mixed according to the mass ratio of 1: 6-1: 8, mixing, stirring for 20-30 min at 400-600 r/min, then adding nano titanium dioxide with the mass of 0.06-0.08 times of terephthalic acid, heating to 80-100 ℃ at 9-10 ℃/min, adding 3, 4-diaminophenylacetic acid with the mass of 1.2-2.4 times of terephthalic acid, and continuously stirring for 2-4 h to prepare the polyarylamide.
Further, the mass ratio of lime to water in the lime water solution is 1:0.31 to 1:0.33.
further, the preparation method of the cement base material comprises the following steps: cement, water, siliceous fine sand and gypsum are mixed according to the mass ratio of 1:0.6:2:0.8 to 1:0.8:4:1.2, mixing, stirring for 10-30 min at 80-100 r/min to obtain the cement base material.
Compared with the prior art, the invention has the following beneficial effects:
the antioxidation cement-based waterproof material prepared by the invention comprises cement, siliceous fine sand, water, lime, phthalonitrile aluminate, phosphorus trichloride, polyarylamide and gypsum.
Firstly, cyano groups in part of phthalonitrile aluminate are polymerized to form triazinyl aluminate, lime is hydrolyzed to form calcium hydroxide, the calcium hydroxide reacts with the phthalonitrile aluminate and the triazinyl aluminate to form tricalcium aluminate, hydroxyphthalic acid, ammonia water and hydroxyphenyltriazine, so that the oxidation resistance of the antioxidation cement-based waterproof material is enhanced; the ammonia water and the phosphorus trichloride react and polymerize to form ammonium polyphosphate, so that the flame retardant property of the antioxidation cement-based waterproof material is enhanced.
Secondly, the phenylacetic acid in the phthalic acid and the polyamide reacts and then is hydrolyzed and reduced to form 2- (2-phenethyl) benzoic acid, ammonium polyphosphate promotes dehydration cyclization, rearrangement and reduction of the 2- (2-phenethyl) benzoic acid to form a dibenzo-octamembered ring structure, when the temperature is increased, the polyamide containing the dibenzo-octamembered ring structure is heated and contracted when the cement base material is heated and expanded, and when the temperature is reduced, the cement base material is contracted, the polyamide containing the dibenzo-octamembered ring structure is expanded, so that the heat stability of the antioxidation cement-based waterproof material is enhanced; the tricalcium aluminate and calcium sulfate in the gypsum are mutually combined under the action of water to form hydrated calcium sulfoaluminate needle-shaped crystals on the surfaces of the cement particles to form a protective film, so that the moisture is prevented from entering the inside of the cement particles, and the waterproof effect is further achieved.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
In order to more clearly illustrate the method provided by the invention, the following examples are used for describing the detailed description, and the test methods of each index of the antioxidant cement-based waterproof material prepared in the following examples are as follows:
oxidation resistance: the same mass of the antioxidation cement-based waterproof materials prepared in the examples and the comparative examples were put into an environment with humidity of 80% and temperature of 40 ℃ for oxidation for 28 days, and the compressive strength before and after oxidation was measured according to GB 1845, and the rate of change of compressive strength before and after oxidation= (compressive strength before oxidation-compressive strength after oxidation)/(compressive strength before and after oxidation) was 100%/compressive strength before and after oxidation.
Flame retardancy: the oxidation-resistant cement-based waterproof materials prepared in the same quality examples and comparative examples were tested for oxygen index according to GB/T8624.
Thermal stability: taking the antioxidant cement-based waterproof materials prepared in the same quality examples and comparative examples, preserving heat at 180 ℃ for 4 hours, reducing the temperature to-55 ℃ at 5-6 ℃ and preserving heat for 4 hours continuously, and observing whether cracks appear in the antioxidant cement-based waterproof materials after the steps are circulated for 20 times.
Waterproof property: the same mass of the antioxidant cement-based waterproof materials prepared in examples and comparative examples were taken, and the 28d permeation resistance pressure, the second permeation resistance pressure (56 d), and the permeation pressure ratio (28 d) were measured according to GB 1845.
Example 1
(1) Aluminum, 3, 6-dihydroxyphthalonitrile and carbon tetrachloride are mixed according to the mass ratio of 1:18:20, mixing, stirring for 20min at 100r/min, then adding mercury chloride with the mass of 0.019 times of that of aluminum, heating to 130 ℃, continuously stirring for 6h, and performing rotary steaming at 1800r/min for 3h at 10Pa and 130 ℃ to prepare the o-phthalonitrile aluminate;
(2) Terephthalic acid and chloroform are mixed according to the mass ratio of 1:6, mixing, stirring for 20min at 400r/min, then adding nano titanium dioxide with the mass of 0.06 times of terephthalic acid, heating to 80 ℃ at 9 ℃/min, adding 3, 4-diaminophenylacetic acid with the mass of 1.2 times of terephthalic acid, and continuously stirring for 2h to obtain the polyarylamide;
(3) Cement, water, siliceous fine sand and gypsum are mixed according to the mass ratio of 1:0.6:2: mixing 0.8, and stirring for 10min at 80r/min to obtain cement base material;
(4) Under the condition of 60 ℃ and argon protection, phthalonitrile aluminate, sodium periodate, tetrahydrofuran and water are mixed according to the mass ratio of 1:0.6:3:0.72, mixing, stirring for 110min at 300r/min, steaming for 1h at 1800r/min under 200Pa and 100 ℃, adding methanol with 3 times of the mass of the phthalonitrile aluminate, continuously stirring for 30min, cooling to 7 ℃, adding thionyl chloride with 0.6 times of the mass of the phthalonitrile aluminate, continuously stirring for 23h, carrying out microwave treatment under 2400MHz and 700W microwave conditions for 40min, naturally cooling to room temperature, and adding lime water solution with 1.5 times of the mass of the phthalonitrile aluminate, wherein the mass ratio of lime to water in the lime water solution is 1:0.31, heating to 60 ℃, continuously stirring for 2 hours, increasing the pressure to 1MPa, adding phosphorus trichloride with the mass of 0.3 times of that of the phthalonitrile aluminate, continuously stirring for 30 minutes, heating to 280 ℃, continuously stirring for 1.5 hours, then adding the mixture into a cement base material with the mass of 3 times of that of the phthalonitrile aluminate, stirring for 20 minutes at 100r/min, adding the polyarylamide with the mass of 1.2 times of that of the phthalonitrile aluminate, continuously stirring for 11 hours after heating to 140 ℃, cooling to 100 ℃, adding sodium chloride with the mass of 0.7 times of that of the phthalonitrile aluminate, continuously stirring for 5 hours, adding hydrogen with the mass of 0.09 times of that of the phthalonitrile aluminate at 90 ℃, continuously stirring for 7 hours under 2MPa, continuously stirring for 4 hours after heating to 115 ℃, and then under the condition of 30 ℃, according to the mass ratio of 1:4:9 adding potassium tert-butoxide, methyl triphenyl phosphorus iodide and diethyl ether, wherein the mass of the potassium tert-butoxide is 0.4 times of that of the phthalonitrile aluminate, continuing stirring for 10 hours, adding aluminum oxide with the mass of 1 time of that of the phthalonitrile aluminate, continuing stirring for 1 hour, adding hydroxyl toluene sulfonyl iodobenzene with the mass of 0.8 time of that of the phthalonitrile aluminate, continuing stirring for 1 hour at room temperature, continuing adding aluminum lithium hydride with the mass of the phthalonitrile aluminate, continuing stirring for 0.8 hour, and naturally cooling to room temperature to prepare the antioxidant cement-based waterproof material.
Example 2
(1) Aluminum, 3, 6-dihydroxyphthalonitrile and carbon tetrachloride are mixed according to the mass ratio of 1:18.5:21, stirring for 30min at 150r/min, then adding mercury chloride with the mass of 0.02 times of that of aluminum, heating to 135 ℃, continuously stirring for 9h, and performing rotary steaming at 2000r/min for 4h at 15Pa and 135 ℃ to prepare o-phthalonitrile aluminate;
(2) Terephthalic acid and chloroform are mixed according to the mass ratio of 1:7, mixing, stirring for 25min at 500r/min, then adding nano titanium dioxide with the mass of 0.07 times of terephthalic acid, adding 3, 4-diaminophenylacetic acid with the mass of 1.8 times of terephthalic acid, heating to 90 ℃ at 9.5 ℃/min, and continuously stirring for 3h to obtain the polyarylamide;
(3) Cement, water, siliceous fine sand and gypsum are mixed according to the mass ratio of 1:0.7:3:1, mixing, and stirring for 20min at 90r/min to prepare a cement base material;
(4) Under the condition of 70 ℃ and argon protection, phthalonitrile aluminate, sodium periodate, tetrahydrofuran and water are mixed according to the mass ratio of 1:0.7:4.3:0.92, stirring for 120min at 400r/min, steaming for 2h at 1900r/min at 250Pa and 101 ℃, adding methanol with the mass of 4 times of the phthalonitrile aluminate, continuously stirring for 40min, cooling to 8 ℃, adding thionyl chloride with the mass of 0.7 times of the phthalonitrile aluminate, continuously stirring for 24h, carrying out microwave treatment for 50min under the microwave condition of 2450MHz and 800W, naturally cooling to room temperature, and adding lime water solution with the mass of 1.6 times of the phthalonitrile aluminate, wherein the mass ratio of lime to water in the lime water solution is 1:0.32, heating to 70 ℃, continuously stirring for 3 hours, increasing the pressure to 2MPa, adding phosphorus trichloride with the mass of 0.4 times of that of the phthalonitrile aluminate, continuously stirring for 40 minutes, heating to 290 ℃, continuously stirring for 2 hours, then adding the mixture into a cement base material with the mass of 4 times of that of the phthalonitrile aluminate, stirring for 30 minutes at 150r/min, adding the polyarylamide with the mass of 1.3 times of that of the phthalonitrile aluminate, continuously stirring for 12 hours after heating to 150 ℃, cooling to 107.5 ℃, adding sodium chloride with the mass of 0.8 times of that of the phthalonitrile aluminate, continuously stirring for 6 hours, adding hydrogen with the mass of 0.1 times of that of the phthalonitrile aluminate, continuously stirring for 7.5 hours at 95 ℃ and 2.5MPa, continuously stirring for 5 hours after heating to 117 ℃, and then under the condition of 40 ℃, according to the mass ratio of 1:4.5:10 adding potassium tert-butoxide, methyl triphenyl phosphorus iodide and diethyl ether, wherein the mass of the potassium tert-butoxide is 0.5 times of that of the phthalonitrile aluminate, continuing stirring for 12 hours, adding aluminum oxide which is 2 times of that of the phthalonitrile aluminate, continuing stirring for 2 hours, adding hydroxyl toluene sulfonyl iodobenzene which is 0.9 times of that of the phthalonitrile aluminate, continuing stirring for 2.5 hours at room temperature, continuing adding lithium aluminum hydride which is 1.2 times of that of the phthalonitrile aluminate, continuing stirring for 1 hour, and naturally cooling to room temperature to obtain the antioxidant cement-based waterproof material.
Example 3
(1) Aluminum, 3, 6-dihydroxyphthalonitrile and carbon tetrachloride are mixed according to the mass ratio of 1:19:22, mixing, stirring for 40min at 200r/min, then adding mercury chloride with the mass of 0.021 times of that of aluminum, heating to 140 ℃, continuously stirring for 12h, and performing rotary steaming at 2200r/min for 5h at 20Pa and 140 ℃ to prepare o-phthalonitrile aluminate;
(2) Terephthalic acid and chloroform are mixed according to the mass ratio of 1:8, mixing, stirring for 30min at 600r/min, then adding nano titanium dioxide with the mass of 0.08 times of terephthalic acid, heating to 100 ℃ at 10 ℃/min, adding 3, 4-diaminophenylacetic acid with the mass of 2.4 times of terephthalic acid, and continuously stirring for 4h to obtain the polyarylamide;
(3) Cement, water, siliceous fine sand and gypsum are mixed according to the mass ratio of 1:0.8:4:1.2, mixing, and stirring for 30min at 100r/min to prepare a cement base material;
(4) Under the condition of 80 ℃ and argon protection, phthalonitrile aluminate, sodium periodate, tetrahydrofuran and water are mixed according to the mass ratio of 1:0.8:5.6:1.12, mixing, stirring for 130min at 500r/min, steaming for 3h at 2000r/min at 300Pa and 102 ℃, adding methanol with the mass of 5 times of the phthalonitrile aluminate, continuously stirring for 50min, cooling to 9 ℃, adding thionyl chloride with the mass of 0.8 times of the phthalonitrile aluminate, continuously stirring for 25h, carrying out microwave treatment under the microwave condition of 2500MHz and 900W for 60min, naturally cooling to room temperature, and adding lime water solution with the mass of 1.7 times of the phthalonitrile aluminate, wherein the mass ratio of lime to water in the lime water solution is 1:0.33, heating to 80 ℃, continuously stirring for 4 hours, increasing the pressure to 3MPa, adding phosphorus trichloride with the mass of 0.5 times of that of the phthalonitrile aluminate, continuously stirring for 50 minutes, heating to 300 ℃, continuously stirring for 2.5 hours, then adding the mixture into a cement base material with the mass of 5 times of that of the phthalonitrile aluminate, stirring for 40 minutes at 200r/min, adding the polyarylamide with the mass of 1.4 times of that of the phthalonitrile aluminate, continuously stirring for 13 hours after heating to 160 ℃, cooling to 115 ℃, adding sodium chloride with the mass of 0.9 times of that of the phthalonitrile aluminate, continuously stirring for 7 hours, adding hydrogen with the mass of 0.11 times of that of the phthalonitrile aluminate at 100 ℃, introducing hydrogen with the mass of 20 times of that of the phthalonitrile aluminate at 3MPa, continuously stirring for 8 hours, continuously stirring for 6 hours after heating to 119 ℃, and then under the condition of 50 ℃, according to the mass ratio of 1:5:11 adding potassium tert-butoxide, methyl triphenyl phosphorus iodide and diethyl ether, wherein the mass of the potassium tert-butoxide is 0.6 times of that of the phthalonitrile aluminate, continuing stirring for 14h, adding aluminum oxide 3 times of that of the phthalonitrile aluminate, continuing stirring for 3h, adding hydroxyl toluene sulfonyl iodobenzene 1 time of that of the phthalonitrile aluminate, continuing stirring for 4h at room temperature, continuing adding lithium aluminum hydride 1.4 times of that of the phthalonitrile aluminate, continuing stirring for 1.2h, and naturally cooling to room temperature to obtain the antioxidant cement-based waterproof material.
Comparative example 1
(1) Aluminum, 3, 6-dihydroxyphthalonitrile and carbon tetrachloride are mixed according to the mass ratio of 1:18.5:21, stirring for 30min at 150r/min, then adding mercury chloride with the mass of 0.02 times of that of aluminum, heating to 135 ℃, continuously stirring for 9h, and performing rotary steaming at 2000r/min for 4h at 15Pa and 135 ℃ to prepare o-phthalonitrile aluminate;
(2) Cement, water, siliceous fine sand and gypsum are mixed according to the mass ratio of 1:0.7:3:1, mixing, and stirring for 20min at 90r/min to prepare a cement base material;
(3) Under the condition of 70 ℃ and argon protection, phthalonitrile aluminate, sodium periodate, tetrahydrofuran and water are mixed according to the mass ratio of 1:0.7:4.3:0.92, stirring for 120min at 400r/min, steaming for 2h at 1900r/min at 250Pa and 101 ℃, adding methanol with the mass of 4 times of the phthalonitrile aluminate, continuously stirring for 40min, cooling to 8 ℃, adding thionyl chloride with the mass of 0.7 times of the phthalonitrile aluminate, continuously stirring for 24h, carrying out microwave treatment for 50min under the microwave condition of 2450MHz and 800W, naturally cooling to room temperature, and adding lime water solution with the mass of 1.6 times of the phthalonitrile aluminate, wherein the mass ratio of lime to water in the lime water solution is 1:0.32, heating to 70 ℃, continuously stirring for 3 hours, increasing the pressure to 2MPa, adding phosphorus trichloride with the mass of 0.4 times of that of the phthalonitrile aluminate, continuously stirring for 40 minutes, heating to 290 ℃, continuously stirring for 2 hours, then adding the mixture into a cement base material with the mass of 4 times of that of the phthalonitrile aluminate, stirring for 30 minutes at 150r/min, continuously stirring for 12 hours after heating to 150 ℃, cooling to 107.5 ℃, adding sodium chloride with the mass of 0.8 times of that of the phthalonitrile aluminate, continuously stirring for 6 hours, adding palladium carbon with the mass of 0.1 time of that of the phthalonitrile aluminate, introducing hydrogen with the mass of 15 times of that of the phthalonitrile aluminate at 95 ℃, continuously stirring for 7.5 hours at 2.5MPa, continuously stirring for 5 hours after heating to 117 ℃, and then stirring for 1 according to the mass ratio of 1:4.5:10 adding potassium tert-butoxide, methyl triphenyl phosphorus iodide and diethyl ether, wherein the mass of the potassium tert-butoxide is 0.5 times of that of the phthalonitrile aluminate, continuing stirring for 12 hours, adding aluminum oxide which is 2 times of that of the phthalonitrile aluminate, continuing stirring for 2 hours, adding hydroxyl toluene sulfonyl iodobenzene which is 0.9 times of that of the phthalonitrile aluminate, continuing stirring for 2.5 hours at room temperature, continuing adding lithium aluminum hydride which is 1.2 times of that of the phthalonitrile aluminate, continuing stirring for 1 hour, and naturally cooling to room temperature to obtain the antioxidant cement-based waterproof material.
Comparative example 2
(1) Terephthalic acid and chloroform are mixed according to the mass ratio of 1:7, mixing, stirring for 25min at 500r/min, then adding nano titanium dioxide with the mass of 0.07 times of terephthalic acid, adding 3, 4-diaminophenylacetic acid with the mass of 1.8 times of terephthalic acid, heating to 90 ℃ at 9.5 ℃/min, and continuously stirring for 3h to obtain the polyarylamide;
(2) Cement, water, siliceous fine sand and gypsum are mixed according to the mass ratio of 1:0.7:3:1, mixing, and stirring for 20min at 90r/min to prepare a cement base material;
(3) Under the condition of 70 ℃ and argon protection, lime water solution and phosphorus trichloride are mixed according to the mass ratio of 1:5, mixing, and stirring for 30min at 150r/min, wherein the mass ratio of lime to water in the lime water solution is 1:0.32, boosting to 2MPa, adding phosphorus trichloride which is 0.4 times of the mass of the lime water solution, continuously stirring for 40min, heating to 290 ℃, continuously stirring for 2h, then adding the mixture into cement base materials which is 4 times of the mass of the lime water solution, stirring for 30min at 150r/min, adding the polyarylamide which is 1.3 times of the mass of the lime water solution, continuously stirring for 12h after heating to 150 ℃, cooling to 107.5 ℃, adding sodium chloride which is 0.8 times of the mass of the lime water solution, continuously stirring for 6h, adding palladium carbon which is 0.1 time of the mass of the lime water solution, introducing hydrogen which is 15 times of the mass of the lime water solution at 95 ℃ and 2.5MPa, continuously stirring for 7.5h, continuously stirring for 5h after heating to 117 ℃, and then under the condition of 40 ℃, stirring according to the mass ratio of 1:4.5:10 adding potassium tert-butoxide, methyl triphenyl phosphorus iodide and diethyl ether, wherein the mass of the potassium tert-butoxide is 0.5 times of the mass of the lime water solution, continuing stirring for 12h, adding aluminum oxide with the mass of 2 times of the lime water solution, continuing stirring for 2h, adding hydroxyl toluene sulfonyl iodobenzene with the mass of 0.9 times of the lime water solution, continuing stirring for 2.5h at room temperature, continuing adding lithium aluminum hydride with the mass of 1.2 times of the lime water solution, continuing stirring for 1h, and naturally cooling to room temperature to prepare the antioxidant cement-based waterproof material.
Comparative example 3
(1) Aluminum, 3, 6-dihydroxyphthalonitrile and carbon tetrachloride are mixed according to the mass ratio of 1:18.5:21, stirring for 30min at 150r/min, then adding mercury chloride with the mass of 0.02 times of that of aluminum, heating to 135 ℃, continuously stirring for 9h, and performing rotary steaming at 2000r/min for 4h at 15Pa and 135 ℃ to prepare o-phthalonitrile aluminate;
(2) Terephthalic acid and chloroform are mixed according to the mass ratio of 1:7, mixing, stirring for 25min at 500r/min, then adding nano titanium dioxide with the mass of 0.07 times of terephthalic acid, adding 3, 4-diaminophenylacetic acid with the mass of 1.8 times of terephthalic acid, heating to 90 ℃ at 9.5 ℃/min, and continuously stirring for 3h to obtain the polyarylamide;
(3) Cement, water, siliceous fine sand and gypsum are mixed according to the mass ratio of 1:0.7:3:1, mixing, and stirring for 20min at 90r/min to prepare a cement base material;
(4) Under the condition of 70 ℃ and argon protection, phthalonitrile aluminate, sodium periodate, tetrahydrofuran and water are mixed according to the mass ratio of 1:0.7:4.3:0.92, stirring for 120min at 400r/min, steaming for 2h at 1900r/min at 250Pa and 101 ℃, adding methanol with the mass of 4 times of the phthalonitrile aluminate, continuously stirring for 40min, cooling to 8 ℃, adding thionyl chloride with the mass of 0.7 times of the phthalonitrile aluminate, continuously stirring for 24h, carrying out microwave treatment for 50min under the microwave condition of 2450MHz and 800W, naturally cooling to room temperature, and adding lime water solution with the mass of 1.6 times of the phthalonitrile aluminate, wherein the mass ratio of lime to water in the lime water solution is 1:0.32, heating to 70 ℃, continuously stirring for 3 hours, increasing the pressure to 2MPa, continuously stirring for 40 minutes, heating to 290 ℃, continuously stirring for 2 hours, then adding the mixture into cement base material with the mass of 4 times of phthalonitrile aluminate, stirring for 30 minutes at 150r/min, adding the poly (aryl amide) with the mass of 1.3 times of phthalonitrile aluminate, continuously stirring for 12 hours after heating to 150 ℃, cooling to 107.5 ℃, adding sodium chloride with the mass of 0.8 times of phthalonitrile aluminate, continuously stirring for 6 hours, adding palladium carbon with the mass of 0.1 time of phthalonitrile aluminate, introducing hydrogen with the mass of 15 times of phthalonitrile aluminate at 95 ℃ and 2.5MPa, continuously stirring for 7.5 hours, continuously stirring for 5 hours after heating to 117 ℃, and then stirring for 1 according to the mass ratio of 1:4.5:10 adding potassium tert-butoxide, methyl triphenyl phosphorus iodide and diethyl ether, wherein the mass of the potassium tert-butoxide is 0.5 times of that of the phthalonitrile aluminate, continuing stirring for 12 hours, adding aluminum oxide which is 2 times of that of the phthalonitrile aluminate, continuing stirring for 2 hours, adding hydroxyl toluene sulfonyl iodobenzene which is 0.9 times of that of the phthalonitrile aluminate, continuing stirring for 2.5 hours at room temperature, continuing adding lithium aluminum hydride which is 1.2 times of that of the phthalonitrile aluminate, continuing stirring for 1 hour, and naturally cooling to room temperature to obtain the antioxidant cement-based waterproof material.
Comparative example 4
(1) Aluminum, 3, 6-dihydroxyphthalonitrile and carbon tetrachloride are mixed according to the mass ratio of 1:18.5:21, stirring for 30min at 150r/min, then adding mercury chloride with the mass of 0.02 times of that of aluminum, heating to 135 ℃, continuously stirring for 9h, and performing rotary steaming at 2000r/min for 4h at 15Pa and 135 ℃ to prepare o-phthalonitrile aluminate;
(2) Terephthalic acid and chloroform are mixed according to the mass ratio of 1:7, mixing, stirring for 25min at 500r/min, then adding nano titanium dioxide with the mass of 0.07 times of terephthalic acid, adding 3, 4-diaminophenylacetic acid with the mass of 1.8 times of terephthalic acid, heating to 90 ℃ at 9.5 ℃/min, and continuously stirring for 3h to obtain the polyarylamide;
(3) Cement, water, siliceous fine sand and gypsum are mixed according to the mass ratio of 1:0.7:3:1, mixing, and stirring for 20min at 90r/min to prepare a cement base material;
(4) Under the condition of 70 ℃ and argon protection, phthalonitrile aluminate, sodium periodate, tetrahydrofuran and water are mixed according to the mass ratio of 1:0.7:4.3:0.92 mixing, stirring at 400r/min for 120min, steaming at 1900r/min for 2h at 250Pa and 101 ℃, adding methanol which is 4 times of the mass of phthalonitrile aluminate, continuously stirring for 40min, cooling to 8 ℃, adding sulfoxide chloride which is 0.7 times of the mass of phthalonitrile aluminate, continuously stirring for 24h, microwave treating for 50min under 2450MHz and 800W microwave condition, naturally cooling to room temperature, heating to 70 ℃, continuously stirring for 3h, increasing the pressure to 2MPa, adding phosphorus trichloride which is 0.4 times of the mass of phthalonitrile aluminate, continuously stirring for 40min, heating to 290 ℃, continuously stirring for 2h, then adding into cement base material which is 4 times of the mass of phthalonitrile aluminate, stirring for 30min at 150r/min, adding polyarylene amide which is 1.3 times of the mass of phthalonitrile aluminate, continuously stirring for 12h after heating to 150 ℃, cooling to 107.5 ℃, adding sodium chloride which is 0.8 times of the mass of phthalonitrile aluminate, continuously stirring for 6h, adding palladium which is 0.1 time of the mass of phthalonitrile aluminate, introducing hydrogen which is 2.95 MPa at 2.5h, continuously stirring for 15 h after heating to 15 h, continuously stirring for 15 h, and continuously stirring for 15 h at the temperature which is equal to 5 h: 4.5:10 adding potassium tert-butoxide, methyl triphenyl phosphorus iodide and diethyl ether, wherein the mass of the potassium tert-butoxide is 0.5 times of that of the phthalonitrile aluminate, continuing stirring for 12 hours, adding aluminum oxide which is 2 times of that of the phthalonitrile aluminate, continuing stirring for 2 hours, adding hydroxyl toluene sulfonyl iodobenzene which is 0.9 times of that of the phthalonitrile aluminate, continuing stirring for 2.5 hours at room temperature, continuing adding lithium aluminum hydride which is 1.2 times of that of the phthalonitrile aluminate, continuing stirring for 1 hour, and naturally cooling to room temperature to obtain the antioxidant cement-based waterproof material.
Effect example
The following table 1 shows the results of analysis of oxidation resistance, flame retardancy, thermal stability, and water resistance of the oxidation-resistant cement-based waterproof materials prepared by using examples 1 to 3 of the present invention and comparative examples 1 to 4.
TABLE 1
From table 1, it can be found that the antioxidation cement-based waterproof materials prepared in examples 1, 2 and 3 are strong in antioxidation, flame retardance, thermal stability and waterproof property; from comparison of experimental data of examples 1, 2 and 3 and comparative example 1, it was found that an antioxidative cement-based waterproof material prepared using a polyarylamide can form a polyarylamide having a dibenzo-octamembered ring structure, and the prepared antioxidative cement-based waterproof material has a high thermal stability; from the experimental data of examples 1, 2, 3 and comparative example 2, it can be found that the oxidation-resistant cement-based waterproof material prepared by using phthalonitrile aluminate can form hydroxyphenyl triazine, ammonium polyphosphate and polyarylamide containing dibenzo-octamembered ring structure, and the oxidation resistance, flame retardance, thermal stability and water resistance of the prepared oxidation-resistant cement-based waterproof material are stronger; from the experimental data of examples 1, 2 and 3 and comparative example 3, it can be found that the phosphorus trichloride is used for preparing the antioxidation cement-based waterproof material, so that ammonium polyphosphate and the polyarylamide containing dibenzo-octamembered ring structure can be formed, and the prepared antioxidation cement-based waterproof material has stronger flame retardance and thermal stability; from the experimental data of examples 1, 2, 3 and comparative example 4, it can be found that the oxidation-resistant cement-based waterproof material prepared by using lime can be made of hydroxyphenyl triazine, poly (aryl amide) containing dibenzo-octa-ring structure, hydrated calcium sulfoaluminate needle crystal, and the oxidation-resistant cement-based waterproof material prepared by the method has strong oxidation resistance, thermal stability and waterproof property.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential characteristics thereof. The present embodiments are, therefore, to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein. Any reference sign in a claim should not be construed as limiting the claim concerned.
Claims (8)
1. The antioxidation cement-based waterproof material is characterized by comprising, by weight, 30-50 parts of cement, 60-200 parts of siliceous fine sand, 20-42 parts of water, 15-34 parts of lime, 10-20 parts of phthalonitrile aluminate, 3-10 parts of phosphorus trichloride, 12-28 parts of polyarylamide and 24-60 parts of gypsum.
2. An oxidation resistant cement-based water resistant material according to claim 1, wherein said cement is portland cement.
3. An oxidation-resistant cement-based waterproof material according to claim 2, wherein the siliceous fine sand is 70 to 140 mesh quartz sand.
4. The preparation process of the antioxidant cement-based waterproof material is characterized by comprising the following steps of: under the condition of 60-80 ℃ and argon protection, phthalonitrile aluminate, sodium periodate, tetrahydrofuran and water are mixed according to the mass ratio of 1:0.6:3:0.72 to 1:0.8:5.6:1.12 mixing, stirring for 110-130 min at 300-500 r/min, steaming for 1-3 h at 200-300 Pa and 100-102 ℃ at 1800-2000 r/min, adding methanol 3-5 times of phthalonitrile aluminate, continuously stirring for 30-50 min, cooling to 7-9 ℃, adding sulfoxide chloride 0.6-0.8 times of phthalonitrile aluminate, continuously stirring for 23-25 h, microwave treating for 40-60 min under 2400-2500 MHz and 700-900W microwave conditions, naturally cooling to room temperature, adding lime aqueous solution 1.5-1.7 times of phthalonitrile aluminate, heating to 60-80 ℃, continuously stirring for 2-4 h, increasing pressure to 1-3 MPa, adding phosphorus trichloride 0.3-0.5 times of phthalonitrile aluminate, continuously stirring for 30-50 min, heating to 280-300 ℃, continuously stirring for 1.5-2.5 h, then adding the mixture into a cement base material with 3-5 times of the mass of the phthalonitrile aluminate, stirring for 20-40 min at 100-200 r/min, adding the polyarylamide with 1.2-1.4 times of the mass of the phthalonitrile aluminate, heating to 140-160 ℃, continuously stirring for 11-13 h, cooling to 100-115 ℃, adding sodium chloride with 0.7-0.9 times of the mass of the phthalonitrile aluminate, continuously stirring for 5-7 h, adding palladium carbon with 0.09-0.11 times of the mass of the phthalonitrile aluminate, introducing hydrogen with 10-20 times of the mass of the phthalonitrile aluminate at 90-100 ℃ and 2-3 MPa, continuously stirring for 7-8 h, continuously stirring for 4-6 h after heating to 115-119 ℃, and then under the condition of 30-50 ℃ according to the mass ratio of 1:4: 9-1: 5:11 adding potassium tert-butoxide, methyl triphenyl phosphorus iodide and diethyl ether, wherein the mass of the potassium tert-butoxide is 0.4-0.6 times of that of the phthalonitrile aluminate, continuously stirring for 10-14 h, adding aluminum oxide with the mass of 1-3 times of that of the phthalonitrile aluminate, continuously stirring for 1-3 h, adding hydroxyl toluene sulfonyl iodobenzene with the mass of 0.8-1 times of that of the phthalonitrile aluminate, continuously stirring for 1-4 h at room temperature, continuously adding aluminum lithium hydride with the mass of 1-1.4 times of that of the phthalonitrile aluminate, continuously stirring for 0.8-1.2 h, and naturally cooling to room temperature to prepare the antioxidant cement-based waterproof material.
5. The process for preparing an antioxidative cement-based waterproof material according to claim 4, wherein the preparation method of the o-phthalonitrile aluminate is as follows: aluminum, 3, 6-dihydroxyphthalonitrile and carbon tetrachloride are mixed according to the mass ratio of 1:18: 20-1: 19:22, stirring for 20-40 min at 100-200 r/min, then adding mercuric chloride with the mass of 0.019-0.021 times of that of aluminum, heating to 130-140 ℃, continuously stirring for 6-12 h, and performing rotary steaming for 3-5 h at 1800-2200 r/min at 10-20 Pa and 130-140 ℃ to prepare the o-phthalonitrile aluminate.
6. The process for preparing an antioxidative cement-based waterproof material according to claim 4, wherein the preparation method of the polyarylamide is as follows: terephthalic acid and chloroform are mixed according to the mass ratio of 1: 6-1: 8, mixing, stirring for 20-30 min at 400-600 r/min, then adding nano titanium dioxide with the mass of 0.06-0.08 times of terephthalic acid, heating to 80-100 ℃ at 9-10 ℃/min, adding 3, 4-diaminophenylacetic acid with the mass of 1.2-2.4 times of terephthalic acid, and continuously stirring for 2-4 h to prepare the polyarylamide.
7. The process for preparing an antioxidative cement-based waterproof material according to claim 4, wherein the mass ratio of lime to water in the lime water solution is 1:0.31 to 1:0.33.
8. the process for preparing an antioxidant cement-based waterproof material according to claim 4, wherein the preparation method of the cement base material is as follows: cement, water, siliceous fine sand and gypsum are mixed according to the mass ratio of 1:0.6:2:0.8 to 1:0.8:4:1.2, mixing, stirring for 10-30 min at 80-100 r/min to obtain the cement base material.
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| CN114835446A (en) * | 2022-06-01 | 2022-08-02 | 张皓 | Heat-insulation ceramsite concrete material and preparation method thereof |
| CN114956672A (en) * | 2022-06-16 | 2022-08-30 | 王志方 | Semi-flexible asphalt and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114835446A (en) * | 2022-06-01 | 2022-08-02 | 张皓 | Heat-insulation ceramsite concrete material and preparation method thereof |
| CN114956672A (en) * | 2022-06-16 | 2022-08-30 | 王志方 | Semi-flexible asphalt and preparation method thereof |
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