CN118791323B - Synergist for solid waste-based cementing material and preparation method thereof - Google Patents
Synergist for solid waste-based cementing material and preparation method thereof Download PDFInfo
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- 239000000463 material Substances 0.000 title claims abstract description 92
- 239000002910 solid waste Substances 0.000 title claims abstract description 51
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000007791 liquid phase Substances 0.000 claims abstract description 93
- SONHXMAHPHADTF-UHFFFAOYSA-M sodium;2-methylprop-2-enoate Chemical compound [Na+].CC(=C)C([O-])=O SONHXMAHPHADTF-UHFFFAOYSA-M 0.000 claims abstract description 36
- 238000002156 mixing Methods 0.000 claims abstract description 35
- 229910003480 inorganic solid Inorganic materials 0.000 claims abstract description 29
- 239000007790 solid phase Substances 0.000 claims abstract description 29
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000006243 chemical reaction Methods 0.000 claims abstract description 26
- 229940044631 ferric chloride hexahydrate Drugs 0.000 claims abstract description 23
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 claims abstract description 23
- 238000001914 filtration Methods 0.000 claims abstract description 19
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 19
- 238000010438 heat treatment Methods 0.000 claims abstract description 16
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims abstract description 15
- SLINHMUFWFWBMU-UHFFFAOYSA-N Triisopropanolamine Chemical compound CC(O)CN(CC(C)O)CC(C)O SLINHMUFWFWBMU-UHFFFAOYSA-N 0.000 claims abstract description 15
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000000227 grinding Methods 0.000 claims abstract description 12
- 239000003513 alkali Substances 0.000 claims abstract description 8
- 238000002844 melting Methods 0.000 claims abstract description 7
- 230000008018 melting Effects 0.000 claims abstract description 7
- 239000000843 powder Substances 0.000 claims abstract description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 39
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 38
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 38
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 37
- 239000008367 deionised water Substances 0.000 claims description 34
- 229910021641 deionized water Inorganic materials 0.000 claims description 34
- 239000007788 liquid Substances 0.000 claims description 32
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 19
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 19
- 239000011780 sodium chloride Substances 0.000 claims description 19
- 239000002245 particle Substances 0.000 claims description 18
- 238000000034 method Methods 0.000 claims description 17
- 239000002002 slurry Substances 0.000 claims description 15
- 239000001110 calcium chloride Substances 0.000 claims description 12
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 12
- 239000003245 coal Substances 0.000 claims description 11
- 239000000126 substance Substances 0.000 claims description 10
- 238000012360 testing method Methods 0.000 claims description 9
- 238000003756 stirring Methods 0.000 claims description 6
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 5
- 238000010992 reflux Methods 0.000 claims description 5
- 229910052573 porcelain Inorganic materials 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 3
- 238000004364 calculation method Methods 0.000 claims description 2
- 239000000706 filtrate Substances 0.000 claims description 2
- ANBBXQWFNXMHLD-UHFFFAOYSA-N aluminum;sodium;oxygen(2-) Chemical compound [O-2].[O-2].[Na+].[Al+3] ANBBXQWFNXMHLD-UHFFFAOYSA-N 0.000 claims 3
- 229910001388 sodium aluminate Inorganic materials 0.000 claims 3
- 238000001354 calcination Methods 0.000 claims 2
- 229910052938 sodium sulfate Inorganic materials 0.000 claims 2
- 235000011152 sodium sulphate Nutrition 0.000 claims 2
- 229910018072 Al 2 O 3 Inorganic materials 0.000 claims 1
- 238000005406 washing Methods 0.000 claims 1
- 238000004846 x-ray emission Methods 0.000 claims 1
- 239000002585 base Substances 0.000 abstract description 11
- 230000036571 hydration Effects 0.000 abstract description 6
- 238000006703 hydration reaction Methods 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 5
- 230000009286 beneficial effect Effects 0.000 abstract description 4
- 238000004064 recycling Methods 0.000 abstract description 2
- 230000002195 synergetic effect Effects 0.000 abstract description 2
- 239000011734 sodium Substances 0.000 description 11
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 9
- 239000002994 raw material Substances 0.000 description 9
- 229910052708 sodium Inorganic materials 0.000 description 9
- 239000012535 impurity Substances 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 4
- 239000003153 chemical reaction reagent Substances 0.000 description 4
- 239000012071 phase Substances 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- 238000001228 spectrum Methods 0.000 description 4
- 238000004876 x-ray fluorescence Methods 0.000 description 4
- 229910021536 Zeolite Inorganic materials 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 3
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000004576 sand Substances 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- 239000010457 zeolite Substances 0.000 description 3
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 description 2
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 2
- 208000006083 Hypokinesia Diseases 0.000 description 2
- 239000004568 cement Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 229910001653 ettringite Inorganic materials 0.000 description 2
- 239000003292 glue Substances 0.000 description 2
- 229920002521 macromolecule Polymers 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 230000001737 promoting effect Effects 0.000 description 2
- 239000012747 synergistic agent Substances 0.000 description 2
- 239000011398 Portland cement Substances 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 229910000019 calcium carbonate Inorganic materials 0.000 description 1
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 description 1
- 239000000920 calcium hydroxide Substances 0.000 description 1
- 229910001861 calcium hydroxide Inorganic materials 0.000 description 1
- 239000000378 calcium silicate Substances 0.000 description 1
- 229910052918 calcium silicate Inorganic materials 0.000 description 1
- OYACROKNLOSFPA-UHFFFAOYSA-N calcium;dioxido(oxo)silane Chemical compound [Ca+2].[O-][Si]([O-])=O OYACROKNLOSFPA-UHFFFAOYSA-N 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
- 229910002092 carbon dioxide Inorganic materials 0.000 description 1
- 150000007942 carboxylates Chemical group 0.000 description 1
- 239000011083 cement mortar Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 230000000052 comparative effect Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000013256 coordination polymer Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 230000001050 lubricating effect Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000004570 mortar (masonry) Substances 0.000 description 1
- 239000013558 reference substance Substances 0.000 description 1
- 238000013112 stability test Methods 0.000 description 1
- 239000013589 supplement Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F222/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a carboxyl radical and containing at least one other carboxyl radical in the molecule; Salts, anhydrides, esters, amides, imides, or nitriles thereof
- C08F222/10—Esters
- C08F222/12—Esters of phenols or saturated alcohols
- C08F222/22—Esters containing nitrogen
-
- 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
- C04B18/00—Use of agglomerated or waste materials or refuse as fillers for mortars, concrete or artificial stone; Treatment of agglomerated or waste materials or refuse, specially adapted to enhance their filling properties in mortars, concrete or artificial stone
- C04B18/04—Waste materials; Refuse
- C04B18/0409—Waste from the purification of bauxite, e.g. red mud
-
- 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
- C04B18/00—Use of agglomerated or waste materials or refuse as fillers for mortars, concrete or artificial stone; Treatment of agglomerated or waste materials or refuse, specially adapted to enhance their filling properties in mortars, concrete or artificial stone
- C04B18/04—Waste materials; Refuse
- C04B18/12—Waste materials; Refuse from quarries, mining or the like
-
- 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
- C04B24/24—Macromolecular compounds
- C04B24/26—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C04B24/2652—Nitrogen containing polymers, e.g. polyacrylamides, polyacrylonitriles
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B40/00—Processes, in general, for influencing or modifying the properties of mortars, concrete or artificial stone compositions, e.g. their setting or hardening ability
- C04B40/0028—Aspects relating to the mixing step of the mortar preparation
- C04B40/0039—Premixtures of ingredients
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/04—Acids; Metal salts or ammonium salts thereof
- C08F220/06—Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
-
- 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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P40/00—Technologies relating to the processing of minerals
- Y02P40/10—Production of cement, e.g. improving or optimising the production methods; Cement grinding
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Organic Chemistry (AREA)
- Structural Engineering (AREA)
- Materials Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Civil Engineering (AREA)
- Environmental & Geological Engineering (AREA)
- Health & Medical Sciences (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Mining & Mineral Resources (AREA)
- Treatment Of Sludge (AREA)
Abstract
The invention provides a synergist for a solid waste-based cementing material and a preparation method thereof, belonging to the technical field of solid waste recycling. The organic liquid phase component is obtained by mixing triethanolamine and triisopropanolamine with maleic anhydride and ferric chloride hexahydrate respectively, then heating and reacting, mixing the intermediate obtained by the reaction with sodium methacrylate and concentrated sulfuric acid respectively, then heating and reacting, finally mixing according to a certain proportion, the inorganic liquid phase component is obtained by filtering the red mud and gangue powder after alkali melting and hydrothermal reaction, and the inorganic solid phase component is obtained by grinding the filter residue obtained by filtering the red mud and gangue powder after alkali melting and hydrothermal reaction. The invention plays a synergistic effect through the three components, is beneficial to the generation of AFt and C-S-H, ensures that the strength is rapidly formed, ensures that the strength is continuously increased in the later stage of hydration, and realizes the effects of early strength and high strength of the solid waste base cementing material.
Description
Technical Field
The invention belongs to the technical field of solid waste recycling, and particularly relates to a synergist for a solid waste-based cementing material and a preparation method thereof.
Background
The solid waste-based cementing material is used as a cement substitute product, can effectively reduce the CO 2 emission in the building field while improving the utilization rate of solid waste resources, accords with the double-carbon policy, and has important practical significance for promoting sustainable green development.
At present, the solid waste-based cementing material has the common problems of long setting time, low early strength, increased later strength, hypodynamia, difficult construction and the like.
Disclosure of Invention
The embodiment of the invention provides a synergist for a solid waste-based cementing material and a preparation method thereof, which are prepared from red mud and coal gangue, and aim to solve the problems of low early strength and increased later strength and hypodynamia of the solid waste-based cementing material.
In order to achieve the above purpose, the invention adopts the technical scheme that the synergist for the solid waste-based cementing material is characterized by comprising, by mass, 10-25 parts of an organic liquid phase component, 15-25 parts of an inorganic liquid phase component and 50-70 parts of an inorganic solid phase component.
The invention provides a preparation method of a synergist for a solid waste based cementing material, which comprises the steps of preparing an organic liquid phase component, preparing an inorganic liquid phase component and preparing an inorganic solid phase component, wherein the organic liquid phase component is prepared by mixing triethanolamine, triisopropanolamine, maleic anhydride and ferric chloride hexahydrate respectively according to a certain proportion, heating for reaction, modifying by sodium methacrylate and finally mixing according to a certain proportion, the inorganic liquid phase component is a filtrate obtained by filtering red mud and coal gangue powder after alkali melting and hydrothermal reaction, and the inorganic solid phase component is obtained by grinding filter residues obtained by filtering after the red mud and the coal gangue powder are subjected to alkali melting and hydrothermal reaction.
With reference to the second aspect, in one possible manner, the organic liquid phase component is prepared according to the following method:
Step one, mixing maleic anhydride, triethanolamine and ferric chloride hexahydrate according to the mass ratio of 1:1.2-2.0:0.05-0.2, and reacting to obtain a liquid a;
Preparing three parts of deionized water, wherein the mass of each part of deionized water is 0.5-1.0 times of the consumption of maleic anhydride, adding sodium carbonate into one part of deionized water until the deionized water is excessive, adding sodium chloride into one part of deionized water until the deionized water is excessive, adding calcium chloride into one part of deionized water until the deionized water is excessive, and retaining excessive sodium carbonate, sodium chloride and calcium chloride to obtain a sodium carbonate solution, a sodium chloride solution and a calcium chloride solution;
Mixing the intermediate a with sodium methacrylate and concentrated sulfuric acid in a three-neck flask according to a mass ratio of 259:68-103:3-5, heating at 70-95 ℃ for reaction, slowly dropwise adding sodium methacrylate with an initial dosage of 1-3 times of the mass of the sodium methacrylate by using a separating funnel during the reaction, controlling the dropwise adding time to be 90-150 min, and continuously reacting at the temperature for 60-120 min after the dropwise adding is finished to obtain an organic liquid phase component a, wherein the molecular formula of the organic liquid phase component a is as follows:
Step four, mixing maleic anhydride, triisopropanolamine and ferric chloride hexahydrate according to the mass ratio of 1:1.5-2.5:0.05-0.2, and reacting to obtain a liquid b;
Step five, treating the liquid b reacted in the step four according to the step two to obtain an intermediate b;
Step six, mixing the intermediate b with sodium methacrylate and concentrated sulfuric acid in a three-neck flask according to a mass ratio 289:68-103:0.15-0.25, heating and reacting at 70-95 ℃, slowly dropwise adding sodium methacrylate with an initial dosage of 1-3 times of the mass of the sodium methacrylate by using a separating funnel, controlling the dropwise adding time to be 90-150 min, and continuously reacting at the temperature for 60-120 min after the dropwise adding is finished to obtain an organic liquid phase component b, wherein the molecular formula of the organic liquid phase component b is as follows:
And seventhly, mixing the organic liquid phase component a and the organic liquid phase component b according to the mass ratio of 1:0.25-1.75 to obtain the finished organic liquid phase component.
In combination with the second aspect, in one possible manner, in the first step, maleic anhydride, triethanolamine and ferric chloride hexahydrate are mixed according to a proportion and then reacted for 120-180 min at 70-80 ℃ to obtain the liquid a.
With reference to the second aspect, in one implementation manner, in the second step, the sodium carbonate, the sodium chloride and the calcium chloride are respectively in excess of 1-3 g in deionized water.
In combination with the second aspect, in one implementation manner, in the fourth step, maleic anhydride, triisopropanolamine and ferric chloride hexahydrate are mixed according to a mass ratio and then reacted for 120-180 min at 70-80 ℃.
With reference to the second aspect, in one possible implementation manner, the molecular weight of the organic liquid phase component a is 7000 to 8000, and the molecular weight of the organic liquid phase component b is 7500 to 9000.
With reference to the second aspect, in one possible manner, the inorganic liquid phase component and the inorganic solid phase component are prepared according to the following method:
Step one, testing the mass fractions of Al 2O3 in the gangue and the red mud by using an X-ray fluorescence spectrum, respectively marking the mass fractions as omega 1 and omega 2, crushing the gangue to be below 0.30 mm to obtain gangue particles, and then calculating the feeding mass m 1 of the gangue particles and the feeding mass m 2 of the red mud according to the following mode:
(1) When omega 1 and omega 2 are not less than 20%, the gangue particles and the red mud can be fed according to any mass ratio;
(2) When only one of omega 1 and omega 2 is not less than 20%, calculating the mass ratio range of the gangue particles to the red mud according to the proportion of (m 1ω1+m2ω2）/（m1+m2) not less than 20%;
(3) When omega 1 and omega 2 are less than 20%, adding sodium metaaluminate with the mass of m 3 except for gangue particles and red mud, and calculating the mass ratio range of the gangue particles, the red mud and the sodium metaaluminate according to (m 1ω1+m2ω2+m3）/（m1+m2+m3) to be more than or equal to 20%;
mixing materials according to the calculation result to obtain a mixed material a;
grinding the mixed material a to 400-600 m 2/kg, mixing the mixed material a and solid sodium hydroxide in a ceramic crucible according to the mass ratio of 51:8-32, uniformly stirring, transferring the mixed material a and the solid sodium hydroxide into a muffle furnace, roasting the mixed material a for 60-120 min at 550-750 ℃, taking out the mixed material b after roasting, and airing the mixed material b in a dryer to room temperature;
Adding deionized water into the roasted mixed material b to obtain slurry, wherein the adding amount is that the mass ratio of the deionized water to the roasted mixed material b is 1:6-10, transferring the slurry to a three-neck flask, and carrying out hydrothermal reaction for 90-150 min at 105-125 ℃ by using a chemical microwave reactor under the condition of heating reflux;
And fourthly, filtering the slurry after the hydrothermal reaction, obtaining liquid after filtering, namely the finished inorganic liquid phase component, and grinding filter residues again to 400-600 m 2/kg to obtain the finished inorganic solid phase component.
In combination with the second aspect, in one implementation manner, in the second step, the mixture is stirred uniformly and then transferred to a muffle furnace, and baked for 60-120 min at 550-750 ℃.
With reference to the second aspect, in one possible implementation manner, the triethanolamine, the triisopropanolamine, the maleic anhydride, the ferric chloride hexahydrate, and the sodium methacrylate are all industrial pure, and the sodium metaaluminate is analytically pure.
Compared with the prior art, the synergist for the solid waste-based cementing material and the preparation method thereof have the beneficial effects that:
(1) AFt (i.e. ettringite) is a main source of early strength of the solid waste-based cementing material, the formation of AFt cannot be separated from Al element, and a synergist is added into the solid waste-based cementing material, so that the hydration activity of the Al phase can be excited after the alkaline melting-hydrothermal reaction of red mud and coal gangue, the hydration activity is further improved under the action of an inorganic liquid phase, and meanwhile, a large amount of Al phase is contained in the inorganic liquid phase to be used as supplement, thereby promoting the formation of ettringite AFt in the early hydration stage of the solid waste-based cementing material.
(2) The alkali fusion-hydrothermal reaction process can generate a part of zeolite-like phases, and combines with Si phases in the inorganic liquid phase to facilitate the formation of hydrated calcium silicate gel (C-S-H), thereby ensuring the increase of the later strength.
(3) Because the fineness of the inorganic solid phase component and the solid waste base cementing material is finer, and the raw materials contain coal gangue, the combined system of the inorganic solid phase component and the solid waste base cementing material is easier to generate agglomeration phenomenon, and poor workability is caused. The polymer macromolecules of the organic liquid phase component can be adsorbed on the surfaces of inorganic solid phase components and solid waste base cementing materials to form an adsorption layer due to the fact that the polymer macromolecules contain negatively charged carboxylate groups, the adsorption layer can play a role in dispersing the inorganic solid phase components and the solid waste base cementing materials, the steric hindrance effect generated by long molecular chains of the organic liquid phase component a and the organic liquid phase component b can also prevent the inorganic solid phase components and the solid waste base cementing materials from agglomerating (the stretching directions of chain links of the organic liquid phase components a and b in the space are shown in fig. 2 and 3), meanwhile, the other ends of the organic liquid phase component a and the organic liquid phase component b are relatively strong in polarity due to the fact that the other ends of the organic liquid phase component a and the organic liquid phase component b contain N, and the adsorption layer has hydrophilicity, so that on one hand, a water film can play a lubricating role, meanwhile, the inorganic solid phase components and the solid waste base cementing materials can be hydrated better, and the early strength can be improved.
(4) Because the organic liquid phase component contains Na +, after carbon dioxide in the air reacts with calcium hydroxide generated by hydration of the solid waste base cementing material to generate calcium carbonate, OH - remained in the liquid phase can form NaOH with Na +, so that an alkaline environment is continuously provided for the synergist, and the continuous increase of the strength of the synergist is facilitated.
The preparation method provided by the invention can be used for preparing the early-strength and high-strength solid waste-based cementing material, wherein the organic liquid phase component mainly plays a role in dispersing the solid waste-based cementing material and the inorganic solid phase component, continuously provides an alkaline environment and provides power for later strength increase, the inorganic liquid phase component mainly plays a role in providing an alkaline environment and improving early strength, and the active components in the inorganic solid phase can react under the excitation of the inorganic liquid phase component to improve the early strength. The three components play a synergistic role, are favorable for generating AFt and C-S-H, enable the AFt and the C-S-H to form strength rapidly, enable the strength to be increased continuously in the later stage of hydration, and achieve the effect of early strength and high strength of the solid waste-based cementing material.
Drawings
FIG. 1 is a process flow diagram of a preparation method of a synergist for a solid waste-based cementing material provided by an embodiment of the invention;
FIG. 2 is a schematic view showing the extending direction of the organic liquid phase component a chain link in the space according to the embodiment of the present invention;
fig. 3 is a schematic view showing the extending direction of the organic liquid phase component b links in the space according to the embodiment of the present invention.
Detailed Description
In order to make the technical problems, technical schemes and beneficial effects to be solved more clear, the invention is further described in detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
As two typical bulk solid wastes, the red mud and the coal gangue are accumulated in a large quantity, so that not only is the land resource wasted, but also the ecological environment is threatened, the human health is endangered, and the sustainable development of related enterprises is restricted. And red mud and coal gangue are applied and synthesized to the synergist for the solid waste-based cementing material, so that the high-value harmless utilization of the cementing material can be realized. Is beneficial to reducing the damage of red mud and coal gangue to the environment and improving the early strength and the later-stage growth strength of the solid waste-based cementing material.
The preparation method of the synergist for the solid waste-based cementing material provided by the embodiment of the invention is understood by combining with fig. 1 as follows:
Embodiment one:
In the embodiment, the proportion of the synergist for the solid waste base cementing material is 20 parts by mass of an organic liquid phase component, 25 parts by mass of an inorganic liquid phase component and 55 parts by mass of an inorganic solid phase component.
1. The preparation process of the organic liquid phase component comprises the following steps:
Step one, mixing maleic anhydride, triethanolamine and ferric chloride hexahydrate according to the mass ratio of 1:1.4:0.06, and reacting 130 min at 70 ℃ to obtain liquid a.
Preparing three parts of deionized water, wherein the mass of each part of deionized water is 0.5 times of the using amount of maleic anhydride, adding sodium carbonate to the excessive amount of 1 g parts of deionized water, adding sodium chloride to the excessive amount of 1 g parts of deionized water, adding calcium chloride to the excessive amount of 1 g parts of deionized water, retaining excessive sodium carbonate, sodium chloride and calcium chloride, sequentially passing the liquid a after the reaction in the step one through the sodium carbonate, sodium chloride and calcium chloride solution, drying the liquid a by using anhydrous sodium sulfate, and filtering the liquid a to obtain an intermediate a.
Step three, mixing the intermediate a with sodium methacrylate and concentrated sulfuric acid in a three-neck flask according to a mass ratio of 259:70:3, heating at 75 ℃ for reaction, and slowly dropwise adding sodium methacrylate with an initial dosage of 1 time of the mass of the sodium methacrylate by using a separating funnel, wherein the dropwise adding time is controlled at 100 min. After the completion of the dropwise addition, the reaction was continued at this temperature for 70 min to obtain an organic liquid phase component a.
And step four, mixing maleic anhydride, triisopropanolamine and ferric chloride hexahydrate according to the mass ratio of 1:1.8:0.08, and adding the mixture into the reaction kettle to react 130 min at the temperature of 70 ℃ to obtain liquid b.
And fifthly, treating the liquid b reacted in the step four according to the step two to obtain an intermediate b.
Step six, mixing the intermediate b with sodium methacrylate and concentrated sulfuric acid according to a mass ratio 289:75:0.16 in a three-neck flask, heating at 75 ℃ for reaction, and slowly dropwise adding sodium methacrylate with an initial dosage of 1 time of mass of sodium methacrylate by using a separating funnel during the reaction, wherein the dropwise adding time is controlled at 110 min. After the completion of the dropwise addition, the reaction was continued at this temperature for 60 min to obtain an organic liquid phase component b.
And seventhly, mixing the organic liquid phase component a and the organic liquid phase component b according to the proportion of 1:0.5 to obtain a finished organic liquid phase component.
2. The preparation process of the inorganic liquid phase component and the inorganic solid phase component is as follows:
Step one, the mass fractions of Al 2O3 in the gangue and the red mud measured by using an X-ray fluorescence spectrum are omega 1 =23.7% and omega 2 =20.3% respectively, and are not less than 20%, so that the gangue particles and the red mud can be mixed according to any proportion, and in the embodiment, the gangue particles and the red mud are mixed according to the mass ratio of 1:3, so that a mixed material a is obtained.
Grinding the mixed material a to 430 m 2/kg by utilizing a vertical mill, mixing the mixed material a and sodium hydroxide in a porcelain crucible according to the mass ratio of the mixed material a to the sodium hydroxide of 51:12, uniformly stirring, transferring the mixed material a and the sodium hydroxide into a muffle furnace, roasting for 75 minutes at 600 ℃, taking out the mixed material b after roasting, and airing the mixed material b in a dryer to room temperature.
Adding deionized water into the roasted mixed material b to obtain slurry, wherein the adding amount is that the mass ratio of the roasted mixed material b to the deionized water is 1:7, transferring the slurry to a three-neck flask, adding a little zeolite, and carrying out hydrothermal reaction at 105 ℃ by using a chemical microwave reactor under the condition of heating reflux to 90 min.
And fourthly, filtering the slurry after the hydrothermal reaction, obtaining liquid after filtering, namely the finished inorganic liquid phase component, and grinding filter residues again to 450m 2/kg to obtain the finished inorganic solid phase component.
3. The triethanolamine, triisopropanolamine, maleic anhydride, ferric chloride hexahydrate, and sodium methacrylate used in this example were all industrially pure and the sodium metaaluminate was analytically pure.
Embodiment two:
In the embodiment, the synergist for the solid waste based cementing material comprises 22 parts by mass of organic liquid phase component, 16 parts by mass of inorganic liquid phase component and 62 parts by mass of inorganic solid phase component.
1. The preparation process of the organic liquid phase component comprises the following steps:
Step one, mixing maleic anhydride, triethanolamine and ferric chloride hexahydrate according to the mass ratio of 1:1.6:0.12, and reacting 150 min at 75 ℃ to obtain liquid a.
Preparing three parts of deionized water, wherein the mass of each part of deionized water is 0.7 times of that of maleic anhydride, adding sodium carbonate to an excessive amount of 2 g, adding sodium chloride to an excessive amount of 1 g, adding calcium chloride to an excessive amount of 3g, retaining excessive sodium carbonate, sodium chloride and calcium chloride, sequentially passing the liquid a after reaction in the step one through the sodium carbonate, sodium chloride and calcium chloride solution, drying by using anhydrous sodium sulfate, and filtering to obtain an intermediate a.
Step three, mixing the intermediate a with sodium methacrylate and concentrated sulfuric acid in a three-neck flask according to a mass ratio of 259:86:4, heating at 85 ℃ for reaction, and slowly dropwise adding sodium methacrylate with the initial dosage of 2 times of the mass of the sodium methacrylate by using a separating funnel during the reaction, wherein the dropwise adding time is controlled at 110 min. After the completion of the dropwise addition, the reaction was continued at this temperature for 100 min hours to obtain an organic liquid phase component a.
And step four, mixing maleic anhydride, triisopropanolamine and ferric chloride hexahydrate according to the mass ratio of 1:2.1:0.1, and reacting 140 min at 70 ℃ to obtain liquid b.
And fifthly, treating the liquid a reacted in the step four according to the step two to obtain an intermediate b.
Step six, mixing the intermediate b with sodium methacrylate and concentrated sulfuric acid according to a mass ratio 289:85:0.19 in a three-neck flask, heating at 85 ℃ for reaction, and slowly dropwise adding sodium methacrylate with an initial dosage of 2 times of mass by using a separating funnel during the reaction, wherein the dropwise adding time is controlled at 135 min. After the completion of the dropwise addition, the reaction was continued at this temperature of 90 min to obtain an organic liquid phase component b.
And seventhly, mixing the organic liquid phase component a and the organic liquid phase component b according to the proportion of 1:1.25 to obtain a finished organic liquid phase component.
2. The preparation process of the inorganic liquid phase component and the inorganic solid phase component is as follows:
The mass fraction of Al 2O3 in the gangue and the red mud measured by using an X-ray fluorescence spectrum is omega 1 =24.0% and omega 2 =18.2%, only one of the mass fractions is not less than 20%, and the mass ratio of the gangue particles to the red mud is calculated according to the proportion of (m 1ω1+m2ω2）/（m1+m2) not less than 20%, and the gangue particles and the red mud are mixed according to the mass ratio of 3:1 in the embodiment, so that a mixed material a is obtained.
Grinding the mixed material a to 500 m 2/kg by utilizing a vertical mill, mixing the mixed material a and sodium hydroxide in a porcelain crucible according to the mass ratio of the mixed material a to the sodium hydroxide of 51:20, uniformly stirring, transferring the mixed material a and the sodium hydroxide into a muffle furnace, roasting for 95min at 650 ℃, taking out the mixed material b after roasting, and airing the mixed material b in a dryer to room temperature.
Adding deionized water into the roasted mixed material b to obtain slurry, wherein the adding amount is that the mass ratio of the roasted mixed material b to the deionized water is 1:8, transferring the slurry to a three-neck flask, adding a little zeolite, and carrying out hydrothermal reaction at 115 ℃ by using a chemical microwave reactor under the condition of heating reflux to 120 min.
And fourthly, filtering the slurry after the hydrothermal reaction, obtaining liquid after filtering, namely the finished inorganic liquid phase component, and grinding filter residues again to 495 m 2/kg to obtain the finished inorganic solid phase component.
3. The triethanolamine, triisopropanolamine, maleic anhydride, ferric chloride hexahydrate, and sodium methacrylate used in this example were all industrially pure and the sodium metaaluminate was analytically pure.
Embodiment III:
In the embodiment, the proportion of the synergist for the solid waste base cementing material is 13 parts by mass of the organic liquid phase component, 20 parts by mass of the inorganic liquid phase component and 67 parts by mass of the inorganic solid phase component.
1. The preparation process of the organic liquid phase component comprises the following steps:
step one, mixing maleic anhydride, triethanolamine and ferric chloride hexahydrate according to the mass ratio of 1:2.0:0.16, and reacting 170 min at 80 ℃ to obtain liquid a.
Step two, three parts of deionized water are prepared, wherein the mass of each part of deionized water is 0.8 times of the using amount of maleic anhydride, sodium carbonate is added to 3g in excess, sodium chloride is added to 3g in excess, calcium chloride is added to 2 g in excess, and excessive sodium carbonate, sodium chloride and calcium chloride are reserved. And (3) sequentially passing the liquid a reacted in the step (I) through the sodium carbonate, sodium chloride and calcium chloride solution, then drying with anhydrous sodium sulfate, and filtering to obtain an intermediate a.
Step three, mixing the intermediate a with sodium methacrylate and concentrated sulfuric acid in a three-neck flask according to a mass ratio of 259:96:5, heating at 90 ℃ for reaction, slowly dropwise adding sodium methacrylate which is 3 times of the initial dosage of the sodium methacrylate by using a separating funnel during the reaction, controlling the dropwise adding time to be 135 min, and continuing to react at the temperature for 110 min after the dropwise adding is finished, so as to obtain the organic liquid phase component a.
Step four, mixing maleic anhydride, triisopropanolamine and ferric chloride hexahydrate according to the mass ratio of 1:2.4:0.15, and reacting 160 min at 75 ℃ to obtain liquid b.
And fifthly, treating the liquid b reacted in the step four according to the step two to obtain an intermediate b.
Step six, mixing the intermediate b with sodium methacrylate and concentrated sulfuric acid according to a mass ratio 289:96:0.23 in a three-neck flask, heating and reacting at 95 ℃, slowly dropwise adding sodium methacrylate with an initial dosage of 2 times of the mass of the sodium methacrylate by using a separating funnel, controlling the dropwise adding time to be 145 min, and continuously reacting at the temperature 105 min after the dropwise adding is finished to obtain the organic liquid phase component b.
And seventhly, mixing the organic liquid phase component a and the organic liquid phase component b according to the proportion of 1:1.55 to obtain a finished organic liquid phase component.
2. The preparation process of the inorganic liquid phase component and the inorganic solid phase component is as follows:
The mass fractions of Al 2O3 in the gangue and the red mud measured by using an X-ray fluorescence spectrum are omega 1 =17.7% and omega 2 =19.1%, which are respectively smaller than 20%, and a certain mass of sodium metaaluminate is needed to be added, and the mass ratio range of the gangue particles, the red mud and the sodium metaaluminate (m 3) is calculated according to (m 1ω1+m2ω2+m3）/（m1+m2+m3) not less than 20%. In the embodiment, coal gangue particles, red mud and sodium metaaluminate are mixed according to the mass ratio of 1:3:0.3, so as to obtain a mixed material a.
Grinding the mixed material a to 530 m 2/kg by using a vertical mill, mixing the mixed material a and sodium hydroxide in a porcelain crucible according to the mass ratio of the mixed material a to the sodium hydroxide of 51:28, uniformly stirring, transferring the mixed material a and the sodium hydroxide into a muffle furnace, roasting for 110min at 720 ℃, taking out the mixed material b after roasting, and airing the mixed material b in a dryer to room temperature.
Adding deionized water into the roasted mixed material b to obtain slurry, wherein the adding amount is that the mass ratio of the roasted mixed material b to the deionized water is 1:9, transferring the slurry to a three-neck flask, adding a little zeolite, and carrying out hydrothermal reaction 140 min at 120 ℃ by using a chemical microwave reactor under the condition of heating reflux.
And fourthly, filtering the slurry after the hydrothermal reaction, obtaining liquid after filtering, namely the finished inorganic liquid phase component, and grinding filter residues again to 550 m 2/kg to obtain the finished inorganic solid phase component.
3. The triethanolamine, triisopropanolamine, maleic anhydride, ferric chloride hexahydrate, and sodium methacrylate used in this example were all industrially pure and the sodium metaaluminate was analytically pure.
The synergists in the first, second and third examples were used to prepare test pieces of gum sand and compared with the blank and comparative groups. Before the preparation of the mortar test block, the organic liquid phase component, the inorganic liquid phase component and water are mixed, the inorganic solid phase component and the solid waste base cementing material are mixed, and then the strength and the setting time are tested according to the relevant regulations of the current national standard of cement mortar strength test method (IOS) method (GB/T17671), cement standard consistency water consumption, setting time and stability test method (GB/T1346). The proportion table and the test result of the glue sand test block are shown in table 1 and table 2.
Table 1 glue sand test block proportioning table
TABLE 2 test results of gel test block strength and set time
As shown in tables 1 and 2, compared with the solid waste-based cementing material without the synergistic agent, the strength of the solid waste-based cementing material 3d after the synergistic agent is added is improved by 26.7-33.5%, the strength of the solid waste-based cementing material 28d is improved by 11.4-16.4%, the initial/final setting time is obviously shortened, and compared with ordinary Portland cement, the strength and the initial/final setting time are basically the same, which shows that the performance of the solid waste-based cementing material is obviously improved.
By way of explanation, analytical purity (AR, red labeled secondary) is slightly less than the top grade purity and the impurity content is slightly greater than the top grade purity, and is suitable for use in important analytical and general research works, such as general laboratory, research institute, and the like where reagents are commonly used, often denoted AR.
Chemical product purity is the purity of the raw material and relatively refers to the impurity content of the raw material. Industrial purity is relatively low grade purity, is suitable for use in relaxed laboratory work such as rinsing, desolventizing or as a raw material in production, and is very low purity.
Chemical product purity is the purity of the raw material and relatively refers to the impurity content of the raw material. The higher the purity, the fewer the impurity species and amount contained in the feedstock. Chemical raw materials can be classified into two main categories of industrial purity and reagent purity according to purity. The raw materials of the reagent can be classified into four grades according to the purity.
The quality grade purity (GR, green label, first grade product) is high in main component content and purity, is suitable for accurate analysis and scientific research determination work, and can be used as a reference substance;
Analytical purity (AR, red label, secondary product) with high content of main component, high purity and low interference impurity, and is suitable for general analysis and scientific research;
Chemical purity (CP, blue label, three-level product) with high content of main component and high purity, and interference impurities, and is suitable for general analysis and synthesis preparation in industrial and teaching processes;
The experimental purity (LR, yellow or brown label) is high in main component content, poor in purity, and only suitable for general chemical experiments and synthetic preparation.
The industrial purity (t.p. reagent, TECHNICALGRADE) is lower than that of the fourth grade, and is suitable for use in relaxed laboratory work such as rinsing, desolventizing or as a raw material in production, with very low purity.
In the foregoing embodiments, the descriptions of the embodiments are emphasized, and in part, not described or illustrated in any particular embodiment, reference is made to the related descriptions of other embodiments.
The foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, and alternatives falling within the spirit and principles of the invention.
Claims (9)
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