CN115259760A - Preparation method of sulfate-erosion-resistant high-durability concrete - Google Patents
Preparation method of sulfate-erosion-resistant high-durability concrete Download PDFInfo
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- CN115259760A CN115259760A CN202210952480.6A CN202210952480A CN115259760A CN 115259760 A CN115259760 A CN 115259760A CN 202210952480 A CN202210952480 A CN 202210952480A CN 115259760 A CN115259760 A CN 115259760A
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- 239000004567 concrete Substances 0.000 title claims abstract description 60
- 238000002360 preparation method Methods 0.000 title claims abstract description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 53
- 238000002156 mixing Methods 0.000 claims abstract description 40
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims abstract description 36
- 239000003638 chemical reducing agent Substances 0.000 claims abstract description 29
- 239000004568 cement Substances 0.000 claims abstract description 24
- 230000003628 erosive effect Effects 0.000 claims abstract description 20
- 235000014676 Phragmites communis Nutrition 0.000 claims abstract description 19
- 229920002678 cellulose Polymers 0.000 claims abstract description 17
- 239000001913 cellulose Substances 0.000 claims abstract description 17
- 239000002131 composite material Substances 0.000 claims abstract description 16
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 11
- 238000006266 etherification reaction Methods 0.000 claims abstract description 7
- KCXFHTAICRTXLI-UHFFFAOYSA-N propane-1-sulfonic acid Chemical group CCCS(O)(=O)=O KCXFHTAICRTXLI-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims description 39
- 239000000047 product Substances 0.000 claims description 23
- 229920000168 Microcrystalline cellulose Polymers 0.000 claims description 20
- 238000000034 method Methods 0.000 claims description 20
- 235000019813 microcrystalline cellulose Nutrition 0.000 claims description 20
- 239000008108 microcrystalline cellulose Substances 0.000 claims description 20
- 229940016286 microcrystalline cellulose Drugs 0.000 claims description 20
- 229910052500 inorganic mineral Inorganic materials 0.000 claims description 17
- 239000011707 mineral Substances 0.000 claims description 17
- 239000000203 mixture Substances 0.000 claims description 16
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 15
- 235000010980 cellulose Nutrition 0.000 claims description 14
- 238000006243 chemical reaction Methods 0.000 claims description 14
- 239000002245 particle Substances 0.000 claims description 13
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims description 12
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 12
- 239000002270 dispersing agent Substances 0.000 claims description 12
- 239000001509 sodium citrate Substances 0.000 claims description 12
- NLJMYIDDQXHKNR-UHFFFAOYSA-K sodium citrate Chemical compound O.O.[Na+].[Na+].[Na+].[O-]C(=O)CC(O)(CC([O-])=O)C([O-])=O NLJMYIDDQXHKNR-UHFFFAOYSA-K 0.000 claims description 12
- 239000004575 stone Substances 0.000 claims description 12
- 239000002253 acid Substances 0.000 claims description 11
- 239000004576 sand Substances 0.000 claims description 11
- 230000003113 alkalizing effect Effects 0.000 claims description 10
- -1 3-propyl Chemical group 0.000 claims description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 9
- FSSPGSAQUIYDCN-UHFFFAOYSA-N 1,3-Propane sultone Chemical compound O=S1(=O)CCCO1 FSSPGSAQUIYDCN-UHFFFAOYSA-N 0.000 claims description 8
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- 238000000227 grinding Methods 0.000 claims description 8
- 239000012535 impurity Substances 0.000 claims description 8
- 239000000843 powder Substances 0.000 claims description 8
- 238000007873 sieving Methods 0.000 claims description 8
- 238000000967 suction filtration Methods 0.000 claims description 8
- 239000000725 suspension Substances 0.000 claims description 8
- VDZOOKBUILJEDG-UHFFFAOYSA-M tetrabutylammonium hydroxide Chemical compound [OH-].CCCC[N+](CCCC)(CCCC)CCCC VDZOOKBUILJEDG-UHFFFAOYSA-M 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- 238000005303 weighing Methods 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 239000004744 fabric Substances 0.000 claims description 6
- 239000002002 slurry Substances 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 239000012065 filter cake Substances 0.000 claims description 5
- 239000010881 fly ash Substances 0.000 claims description 5
- 239000002893 slag Substances 0.000 claims description 5
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 4
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 4
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 4
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 4
- 239000005642 Oleic acid Substances 0.000 claims description 4
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 4
- 150000002148 esters Chemical class 0.000 claims description 4
- 150000002191 fatty alcohols Chemical class 0.000 claims description 4
- 238000001914 filtration Methods 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 4
- UIUXUFNYAYAMOE-UHFFFAOYSA-N methylsilane Chemical compound [SiH3]C UIUXUFNYAYAMOE-UHFFFAOYSA-N 0.000 claims description 4
- 230000007935 neutral effect Effects 0.000 claims description 4
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 4
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 4
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims 2
- 238000012216 screening Methods 0.000 claims 1
- 229910021487 silica fume Inorganic materials 0.000 claims 1
- 239000002994 raw material Substances 0.000 abstract description 7
- 230000001603 reducing effect Effects 0.000 abstract description 7
- 238000002425 crystallisation Methods 0.000 abstract description 3
- 230000008025 crystallization Effects 0.000 abstract description 3
- 238000003912 environmental pollution Methods 0.000 abstract description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 abstract description 3
- 239000013078 crystal Substances 0.000 description 10
- 230000007797 corrosion Effects 0.000 description 8
- 238000005260 corrosion Methods 0.000 description 8
- 230000000694 effects Effects 0.000 description 8
- 238000005452 bending Methods 0.000 description 5
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 4
- 239000011863 silicon-based powder Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 3
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 3
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 2
- 239000000920 calcium hydroxide Substances 0.000 description 2
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 2
- 230000003111 delayed effect Effects 0.000 description 2
- 201000010099 disease Diseases 0.000 description 2
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 2
- 229910001653 ettringite Inorganic materials 0.000 description 2
- 229910052602 gypsum Inorganic materials 0.000 description 2
- 239000010440 gypsum Substances 0.000 description 2
- 239000003607 modifier Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229920005646 polycarboxylate Polymers 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 239000008030 superplasticizer Substances 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
-
- 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
- C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
- C04B24/04—Carboxylic acids; Salts, anhydrides or esters thereof
- C04B24/06—Carboxylic acids; Salts, anhydrides or esters thereof containing hydroxy groups
-
- 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
- C04B24/00—Use of organic materials as active ingredients for mortars, concrete or artificial stone, e.g. plasticisers
- C04B24/16—Sulfur-containing compounds
- C04B24/161—Macromolecular compounds comprising sulfonate or sulfate groups
- C04B24/168—Polysaccharide derivatives, e.g. starch sulfate
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2103/00—Function or property of ingredients for mortars, concrete or artificial stone
- C04B2103/30—Water reducers, plasticisers, air-entrainers, flow improvers
- C04B2103/302—Water reducers
-
- 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
- C04B2111/2015—Sulfate resistance
-
- 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
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/50—Mortars, concrete or artificial stone characterised by specific physical values for the mechanical strength
-
- 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 a preparation method of sulfate erosion resistant high-durability concrete, and particularly relates to the technical field of concrete preparation. The sulfate erosion resistant high-durability concrete prepared by the raw material formula can greatly improve the fluidity and slump of the concrete, simultaneously can effectively reduce the water consumption for mixing, obviously improves the working performance of the concrete, can more fully and effectively utilize the existing cellulose resources by chemically modifying the reed pulp, and can also reduce the environmental pollution caused by improper treatment; more importantly, the prepared composite water reducing agent is subjected to etherification reaction with hydroxyl on a cellulose molecular chain through an etherifying agent, propyl sulfonic acid groups are introduced, and a crystallization area of cellulose is damaged, so that the water solubility of a product is improved, a good water reducing effect is shown on cement paste, and the aims of reducing cost and optimizing performance are fulfilled.
Description
Technical Field
The invention relates to the technical field of concrete preparation, in particular to a preparation method of sulfate erosion resistant high-durability concrete.
Background
Concrete is one of the most widely used and most used building materials in the world today, plays a role and a function which cannot be replaced by other materials, and the research on the durability of the concrete is generally concerned by people. Wherein the attack damage caused by sulfate is one of the important influencing factors of the concrete durability. In recent years, sulfate corrosion diseases of concrete tend to be frequent and increasingly serious in various places, the functionality and safety of concrete members are reduced due to sulfate corrosion of the concrete, serious loss is brought to national economy, old materials of old methods for treating the sulfate corrosion diseases of the concrete, which are used along for many years, cannot completely meet the current requirement on corrosion protection, and the improvement of the durability of the concrete by using an additional modifier becomes a hotspot of research of people.
However, the method for improving the durability of concrete by using an additional modifier in the prior art has the disadvantages of complex process and high production cost, and the modified durability has poor effect and needs to be improved.
Disclosure of Invention
In view of the above problems in the prior art, the present invention is to provide a method for preparing a highly durable concrete resistant to sulfate attack, and the problems to be solved by the present invention are: how to reduce the cost of preparing a high-durability concrete resistant to sulfate attack and improve the durability of the concrete.
In order to solve the problems, the technical scheme adopted by the invention is as follows:
a preparation method of sulfate erosion resistant high-durability concrete comprises the following specific preparation steps:
the method comprises the following steps: weighing dry reed pulp, adding the reed pulp into a reaction container, adding a dilute hydrochloric acid solution, mixing and stirring the reed pulp in a water bath heating state at 55-65 ℃, filtering impurities and pulp residues with larger particles in a product by a filter screen after fully mixing, washing the product to be neutral, drying the product obtained by suction filtration at 80-95 ℃ to constant weight, grinding and sieving to obtain white or near-white powder which is microcrystalline cellulose for later use;
step two: weighing the microcrystalline cellulose obtained in the step one, adding the microcrystalline cellulose into a reaction container, adding a dispersing agent to prepare a suspension, dropwise adding an alkalizing agent to alkalize the microcrystalline cellulose at the alkalizing temperature of 10-20 ℃, then slowly dropwise adding 1, 3-propyl sultone into the alkalized suspension, carrying out etherification reaction at the temperature of 85-95 ℃, after the reaction is finished, washing the product for several times by sequentially using isopropanol, absolute ethyl alcohol and methanol, carrying out suction filtration to obtain a filter cake, drying at the temperature of 60-70 ℃ for 12-15 h, grinding and sieving to obtain white or light yellow powder, namely propyl sultone, and mixing the propyl sultone and a polycarboxylic acid water reducer together to obtain a composite water reducer for later use;
step three: adding cement, mineral admixture and the composite water reducing agent obtained in the second step into a stirrer for mixing, then adding sodium citrate for stirring and mixing, then adding broken stone and sand for stirring and mixing, finally adding deionized water for stirring uniformly, and obtaining a sample A for later use;
step four: pouring the sample A obtained in the third step into a test mold, removing bubbles in the slurry by vibration, covering wet cloth on the surface, placing the sample for 24 to 48 hours in an environment with the temperature of 25 to 35 ℃ and the humidity of minus 65 plus or minus 5 percent, removing the sample from the test mold, and curing the sample for 14 to 16 days in an environment with the temperature of 20 to 35 ℃ and the humidity of 90 plus or minus 5 percent to obtain the sulfate erosion resistant high-durability concrete.
Further, the mass fraction ratio of the reed pulp to the dilute hydrochloric acid solution in the step one is 6: (7 to 11).
Furthermore, the filter screen in the first step can screen 120 meshes of impurities and above and pulp residues with larger particles.
Furthermore, the mass fraction ratio of the microcrystalline cellulose to the dispersing agent in the second step is 1 (10-15).
Further, the dispersant in the second step is one or a mixture of two or more of fatty alcohol polyoxyethylene ether methylsilane and oleic acid polyoxyethylene ester.
Further, the alkalizing agent in the second step is one or a mixture of two or more of potassium hydroxide, sodium hydroxide and tetrabutylammonium hydroxide.
Further, the mass fraction ratio of the propyl cellulose sulfonate to the polycarboxylic acid water reducing agent in the second step is 3: (20 to 35).
Further, the mass fraction ratio of the cement, the mineral admixture, the composite water reducing agent, the sodium citrate, the broken stone and the sand in the third step is (1-3): 2:0.5:0.1:7:4.
further, the mineral admixture is one or a mixture of two or more of fly ash, ground slag and silicon powder.
Further, in the first step, the mixing and stirring speed is 350-450 r/min, the stirring time is 20-35 min, and in the third step, the mixing and stirring speed is 350-450 r/min, and the stirring time is 35-55 min.
Compared with the prior art, the invention has the beneficial effects that:
(1) The sulfate erosion resistant high-durability concrete prepared by adopting the raw material formula can greatly improve the fluidity and slump of the concrete, simultaneously can effectively reduce the water consumption for mixing, has a dispersing effect on cement particles, improves the fluidity of concrete mixtures, and obviously improves the working performance of the concrete, and the modified cellulose water reducing agent prepared by taking natural cellulose as a raw material through chemically modifying reed pulp can more fully and effectively utilize the existing cellulose resources and can also reduce the environmental pollution caused by improper treatment; more importantly, the prepared composite water reducing agent is subjected to etherification reaction with hydroxyl on a cellulose molecular chain through an etherifying agent, propyl sulfonic acid groups are introduced, and a crystallization area of cellulose is damaged, so that the water solubility of a product is improved, a good water reducing effect is shown on cement paste, and the aims of reducing cost and optimizing performance are fulfilled.
(2) The sulfate erosion resistant high-durability concrete prepared by the raw material formula can improve the sulfate erosion resistance of the concrete, and the added sodium citrate can reduce the speed of calcium hydroxide separating out from the set cement, so that the generation of gypsum and ettringite crystals can be delayed and the generated crystals are coarse, under the condition of a certain total crystal generation amount, the larger the crystal particles are, the smaller the total volume of the crystals is, the smaller the damage caused by the expansion effect of the concrete is, and the effect of reducing the expansion damage of the concrete can be further achieved, so that the sulfate erosion resistance of the concrete can be improved, and meanwhile, the added mineral admixture can fill the defects and pores in the concrete, so that the mixture can be fully wrapped on the surface of the cement particles, and can be more easily connected into a network to inhibit the formation and expansion of cracks, improve the breaking strength of the material and improve the durability of the concrete.
Detailed Description
The invention is further described with reference to specific examples.
Example 1
A preparation method of sulfate erosion resistant high-durability concrete comprises the following specific preparation steps:
the method comprises the following steps: weighing dry reed pulp, adding the reed pulp into a reaction container, adding dilute hydrochloric acid solution into the reaction container, mixing and stirring the reed pulp in a water bath heating state at 55 ℃, filtering out impurities and pulp residues with larger particles in a product after fully mixing, washing the product to be neutral by water, drying the product obtained by suction filtration at 80 ℃ to constant weight, grinding and sieving the product to obtain white or near-white powder which is microcrystalline cellulose for later use;
step two: weighing the microcrystalline cellulose obtained in the first step, adding the microcrystalline cellulose into a reaction container, adding a dispersing agent to prepare a suspension, dropwise adding an alkalizing agent to alkalize the microcrystalline cellulose at 10 ℃, slowly dropwise adding 1, 3-propyl sultone into the alkalized suspension, performing etherification reaction at 95 ℃, washing the product for several times by sequentially using isopropanol, absolute ethyl alcohol and methanol after the reaction is finished, performing suction filtration to obtain a filter cake, drying the filter cake at 60 ℃ for 12 hours, grinding and sieving to obtain white or light yellow powder, namely propyl sul-fonate, and mixing the propyl sul-fonate with a polycarboxylic acid water reducer to obtain a composite water reducer for later use;
step three: adding cement, mineral admixture and the composite water reducing agent obtained in the second step into a stirrer for mixing, then adding sodium citrate, stirring and mixing, then adding crushed stone and sand, stirring and mixing, finally adding deionized water, and stirring uniformly to obtain a sample A for later use;
step four: pouring the sample A obtained in the third step into a test mold, vibrating to remove air bubbles in the slurry, covering wet cloth on the surface, placing for 24 hours in an environment with the temperature of 25 ℃ and the humidity of-65 +/-5%, removing the sample from the test mold, and curing for 14 days in an environment with the temperature of 20 ℃ and the humidity of 90 +/-5% to obtain the high-durability concrete resistant to sulfate corrosion.
The mass fraction ratio of the reed pulp to the dilute hydrochloric acid solution in the first step is 6:11.
the filter screen in the step one can screen 120 meshes and above of impurities and pulp residues with larger particles.
And the mass fraction ratio of the microcrystalline cellulose to the dispersing agent in the second step is 1.
The dispersant in the second step is one or a mixture of two or more of fatty alcohol polyoxyethylene ether methyl silane and oleic acid polyoxyethylene ester.
The alkalizing agent in the second step is one or a mixture of two or more of potassium hydroxide, sodium hydroxide and tetrabutyl ammonium hydroxide.
The mass fraction ratio of the propyl cellulose sulfonate to the polycarboxylic acid water reducing agent in the second step is 3:22.
in the third step, the mass fraction ratio of the cement, the mineral admixture, the composite water reducing agent, the sodium citrate, the broken stone and the sand is 1:2:0.5:0.1:7:4.
the mineral admixture is one or a mixture of two or more of fly ash, ground slag and silicon powder.
In the first step, the mixing and stirring speed is 350r/min, the stirring time is 20min, and in the third step, the mixing and stirring speed is 350r/min, and the stirring time is 55min.
Example 2
A preparation method of sulfate erosion resistant high-durability concrete comprises the following specific preparation steps:
the method comprises the following steps: weighing dry reed pulp, adding the reed pulp into a reaction container, adding dilute hydrochloric acid solution into the reaction container, mixing and stirring the reed pulp in a water bath heating state at 55 ℃, filtering out impurities and pulp residues with larger particles in a product after fully mixing, washing the product to be neutral by water, drying the product obtained by suction filtration at 80 ℃ to constant weight, grinding and sieving the product to obtain white or near-white powder which is microcrystalline cellulose for later use;
step two: weighing the microcrystalline cellulose obtained in the step one, adding the microcrystalline cellulose into a reaction container, adding a dispersing agent to prepare a suspension, dropwise adding an alkalizing agent to alkalize the microcrystalline cellulose at the alkalizing temperature of 10 ℃, then slowly dropwise adding 1,3 propyl sultone into the alkalized suspension, carrying out etherification reaction at the temperature of 95 ℃, after the reaction is finished, sequentially washing the product with isopropanol, absolute ethyl alcohol and methanol for several times, carrying out suction filtration to obtain a filter cake, drying at the temperature of 60 ℃ for 12 hours, grinding and sieving to obtain white or light yellow powder, namely propyl sultone, and mixing the propyl sultone and a polycarboxylic acid water reducer together to obtain a composite water reducer for later use;
step three: adding cement, mineral admixture and the composite water reducing agent obtained in the second step into a stirrer for mixing, adding broken stone and sand for stirring and mixing, finally adding deionized water, and stirring uniformly to obtain a sample A for later use;
step four: pouring the sample A obtained in the third step into a test mold, vibrating to remove air bubbles in the slurry, covering wet cloth on the surface, placing for 24 hours in an environment with the temperature of 25 ℃ and the humidity of-65 +/-5%, removing the sample from the test mold, and curing for 14 days in an environment with the temperature of 20 ℃ and the humidity of 90 +/-5% to obtain the high-durability concrete resistant to sulfate corrosion.
The mass fraction ratio of the reed pulp to the dilute hydrochloric acid solution in the first step is 6:11.
the filter screen in the step one can screen 120 meshes of impurities and more than 120 meshes of pulp residues with larger particles.
And the mass fraction ratio of the microcrystalline cellulose to the dispersing agent in the second step is 1.
And the dispersant in the second step is one or a mixture of two or more of fatty alcohol polyoxyethylene ether methylsilane and oleic acid polyoxyethylene ester.
The alkalizing agent in the second step is one or a mixture of two or more of potassium hydroxide, sodium hydroxide and tetrabutyl ammonium hydroxide.
The mass fraction ratio of the propyl cellulose sulfonate to the polycarboxylic acid water reducing agent in the second step is 3:22.
in the third step, the mass fraction ratio of the cement, the mineral admixture, the composite water reducing agent, the broken stone and the sand is 1:2:0.5:7:4.
the mineral admixture is one or a mixture of two or more of fly ash, ground slag and silicon powder.
In the first step, the mixing and stirring speed is 350r/min, the stirring time is 20min, and in the third step, the mixing and stirring speed is 350r/min, and the stirring time is 55min.
Example 3
A preparation method of sulfate erosion resistant high-durability concrete comprises the following specific preparation steps:
the method comprises the following steps: adding cement, mineral admixture and polycarboxylic acid water reducing agent into a stirrer for mixing, then adding sodium citrate, stirring and mixing, then adding broken stone and sand, stirring and mixing, finally adding deionized water, and stirring uniformly to obtain a sample A for later use;
step two: pouring the sample A obtained in the third step into a test mold, vibrating to remove air bubbles in the slurry, covering wet cloth on the surface, placing for 24 hours in an environment with the temperature of 25 ℃ and the humidity of-65 +/-5%, removing the sample from the test mold, and curing for 14 days in an environment with the temperature of 20 ℃ and the humidity of 90 +/-5% to obtain the high-durability concrete resistant to sulfate corrosion.
In the third step, the mass fraction ratio of the cement, the mineral admixture, the polycarboxylic acid water reducing agent, the sodium citrate, the broken stone and the sand is 1:2:0.5:0.1:7:4.
the mineral admixture is one or a mixture of two or more of fly ash, ground slag and silicon powder.
In the second step, the mixing and stirring speed is 350r/min, and the stirring time is 55min.
Comparative example
A preparation method of sulfate erosion resistant high-durability concrete comprises the following specific preparation steps:
the method comprises the following steps: adding cement, mineral admixture and polycarboxylate superplasticizer into a stirrer, stirring and mixing, adding broken stone and sand, stirring and mixing, finally adding deionized water, and stirring uniformly to obtain a sample A for later use;
step two: pouring the sample A obtained in the third step into a test mold, vibrating to remove air bubbles in the slurry, covering wet cloth on the surface, placing for 24 hours in an environment with the temperature of 25 ℃ and the humidity of-65 +/-5%, removing the sample from the test mold, and curing for 14 days in an environment with the temperature of 20 ℃ and the humidity of 90 +/-5% to obtain the high-durability concrete resistant to sulfate corrosion.
The sources of the raw materials in the above examples and comparative examples are: the diluted hydrochloric acid is produced by Wuhanjing Brilliant biological science and technology limited company, the 1,3 propyl sultone is produced by Hubei Jiang Tuitahua chemical industry limited company, the product number of absolute ethyl alcohol is R8382-1GA, the product number of methanol is PHR1372-3X1.5ML, the polycarboxylic acid water reducing agent is produced by Hubei Chengfeng chemical industry limited company, and the product number of sodium citrate is V900443-100G.
The high-durability concrete resistant to sulfate erosion prepared in the above examples 1 to 3 was taken as an experimental group 1, an experimental group 2 and an experimental group 3, the high-durability concrete resistant to sulfate erosion produced in the comparative example was taken as a control group, and the compressive strength, the bending strength, the cement paste fluidity and the water reduction rate of the selected high-durability concrete resistant to sulfate erosion were tested (the compressive strength and the bending strength were both tested and recorded according to the national standard GB/T50107-2010, the cement paste fluidity was tested and recorded according to the national standard GB8077-2000, and the water reduction rate was tested and recorded according to the national standard GB 8077-2012), and the test results are shown in table 1.
TABLE 1 test results
| Compressive strength/MPa | Bending strength/MPa | Fluidity/mm of cement paste | Water reduction rate/%) | |
| Experimental group 1 | 55.9 | 8.2 | 221 | 30.5 |
| Experimental group 2 | 57.2 | 8.9 | 237 | 31.6 |
| Experimental group 3 | 56.5 | 8.5 | 245 | 32.4 |
| Control group | 53 | 7.3 | 210 | 29.2 |
As can be seen from table 1, the sulfate erosion resistant high-durability concrete produced by the method has better compressive strength, bending strength and cement paste fluidity effects, compared with example 3, compared with example 1, the cement paste fluidity effect is reduced without adding a composite water reducing agent, compared with example 2, compared with example 1, sodium citrate is not added, the compressive strength and bending strength effects are reduced, the sulfate erosion resistant high-durability concrete prepared by the raw material formula of the invention can greatly improve the fluidity and slump of the concrete, simultaneously can effectively reduce the mixing water consumption, has a dispersing effect on cement particles, improves the fluidity of concrete mixtures, and obviously improves the working performance of the concrete, and the reed pulp is chemically modified, and the modified cellulose water reducing agent prepared by taking natural cellulose as a raw material can more fully and effectively utilize the existing cellulose resources and reduce the environmental pollution caused by improper treatment; more importantly, the prepared composite water reducing agent is subjected to etherification reaction with hydroxyl on a cellulose molecular chain through an etherifying agent, propyl sulfonic acid groups are introduced, and a crystallization area of cellulose is destroyed, so that the improvement of the water solubility of a product is facilitated, a good water reducing effect is shown on cement paste, and the purposes of reducing cost and optimizing performance can be achieved; the added sodium citrate can reduce the speed of calcium hydroxide separating out from the cement stone, so that the generation of gypsum and ettringite crystals can be delayed, the generated crystals are coarse, under the condition of a certain total crystal generation amount, the larger the crystal particles are, the smaller the total volume of the crystals is, the smaller the damage to the expansion action of the concrete is, and the expansion damage of the concrete can be reduced.
Claims (10)
1. The preparation method of the sulfate erosion resistant high-durability concrete is characterized by comprising the following specific preparation steps of:
the method comprises the following steps: weighing dry reed pulp, adding the reed pulp into a reaction container, adding a dilute hydrochloric acid solution, mixing and stirring the reed pulp in a water bath heating state at 55-65 ℃, filtering impurities and pulp residues with larger particles in a product by a filter screen after fully mixing, washing the product to be neutral, drying the product obtained by suction filtration at 80-95 ℃ to constant weight, grinding and sieving to obtain white or near-white powder which is microcrystalline cellulose for later use;
step two: weighing the microcrystalline cellulose obtained in the step one, adding the microcrystalline cellulose into a reaction container, adding a dispersing agent to prepare a suspension, dropwise adding an alkalizing agent to alkalize the microcrystalline cellulose at the temperature of 10-20 ℃, then slowly dropwise adding 1, 3-propyl sultone into the alkalized suspension, carrying out etherification reaction at the temperature of 85-95 ℃, after the reaction is finished, washing the product with isopropanol, absolute ethyl alcohol and methanol for several times, carrying out suction filtration to obtain a filter cake, drying at the temperature of 60-70 ℃ for 12-15 h, grinding and sieving to obtain white or light yellow powder, namely propyl sultone, and mixing the propyl sultone and a polycarboxylic acid water reducer together to obtain a composite water reducer for later use;
step three: adding cement, mineral admixture and the composite water reducing agent obtained in the second step into a stirrer for mixing, then adding sodium citrate for stirring and mixing, then adding broken stone and sand for stirring and mixing, finally adding deionized water for stirring uniformly, and obtaining a sample A for later use;
step four: pouring the sample A obtained in the third step into a test mold, removing bubbles in the slurry by vibration, covering wet cloth on the surface, placing the sample for 24 to 48 hours in an environment with the temperature of 25 to 35 ℃ and the humidity of minus 65 plus or minus 5 percent, removing the sample from the test mold, and curing the sample for 14 to 16 days in an environment with the temperature of 20 to 35 ℃ and the humidity of 90 plus or minus 5 percent to obtain the sulfate erosion resistant high-durability concrete.
2. The method for preparing the sulfate attack resistant high-durability concrete as claimed in claim 1, wherein the mass fraction ratio of the reed pulp to the dilute hydrochloric acid solution in the first step is 6: (7 to 11).
3. The method as claimed in claim 1, wherein the screen of the first step is capable of screening 120 mesh or more impurities and pulp residue with larger particles.
4. The method for preparing the concrete with high durability and sulfate attack resistance as claimed in claim 1, wherein the mass fraction ratio of the microcrystalline cellulose to the dispersant in the second step is 1 (10-15).
5. The method for preparing the sulfate attack resistant high-durability concrete according to claim 1, wherein the dispersant in the second step is one or a mixture of two or more of fatty alcohol polyoxyethylene ether methylsilane and oleic acid polyoxyethylene ester.
6. The method as claimed in claim 1, wherein the alkalizing agent in the second step is one or a mixture of two or more of potassium hydroxide, sodium hydroxide and tetrabutylammonium hydroxide.
7. The method for preparing the sulfate attack resistant high-durability concrete according to claim 1, wherein the mass fraction ratio of the cellulose propyl sulfonate to the polycarboxylic acid water reducing agent in the second step is 3: (20 to 35).
8. The method for preparing the sulfate attack resistant high-durability concrete according to claim 1, wherein the mass fraction ratio of the cement, the mineral admixture, the composite water reducing agent, the sodium citrate, the broken stone and the sand in the third step is (1-3): 2:0.5:0.1:7:4.
9. the method of claim 1, wherein the mineral admixture is one or a mixture of two or more of fly ash, ground slag and silica fume.
10. The method for preparing the sulfate attack resistant highly durable concrete according to claim 1, wherein in the first step, the mixing and stirring speed is 350 to 450r/min and the stirring time is 20 to 35min, and in the third step, the mixing and stirring speed is 350 to 450r/min and the stirring time is 35 to 55min.
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