CN113149704B - Preparation method of autoclaved eggshell sand - Google Patents
Preparation method of autoclaved eggshell sand Download PDFInfo
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- CN113149704B CN113149704B CN202110630696.6A CN202110630696A CN113149704B CN 113149704 B CN113149704 B CN 113149704B CN 202110630696 A CN202110630696 A CN 202110630696A CN 113149704 B CN113149704 B CN 113149704B
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- 210000003278 egg shell Anatomy 0.000 title claims abstract description 37
- 102000002322 Egg Proteins Human genes 0.000 title claims abstract description 36
- 108010000912 Egg Proteins Proteins 0.000 title claims abstract description 36
- 239000004576 sand Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- 238000006243 chemical reaction Methods 0.000 claims abstract description 12
- 239000002893 slag Substances 0.000 claims abstract description 12
- 238000001035 drying Methods 0.000 claims abstract description 10
- 238000007493 shaping process Methods 0.000 claims abstract description 10
- 239000010881 fly ash Substances 0.000 claims abstract description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 47
- 239000000843 powder Substances 0.000 claims description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 17
- 229910002027 silica gel Inorganic materials 0.000 claims description 14
- 239000000741 silica gel Substances 0.000 claims description 14
- 238000003756 stirring Methods 0.000 claims description 9
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 8
- 239000003638 chemical reducing agent Substances 0.000 claims description 8
- OSMSIOKMMFKNIL-UHFFFAOYSA-N calcium;silicon Chemical compound [Ca]=[Si] OSMSIOKMMFKNIL-UHFFFAOYSA-N 0.000 claims description 6
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 229920005646 polycarboxylate Polymers 0.000 claims description 6
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 4
- 229910052602 gypsum Inorganic materials 0.000 claims description 4
- 239000010440 gypsum Substances 0.000 claims description 4
- 238000005498 polishing Methods 0.000 claims description 4
- 238000000034 method Methods 0.000 claims description 3
- 238000007873 sieving Methods 0.000 claims description 3
- 238000011010 flushing procedure Methods 0.000 claims description 2
- 238000000227 grinding Methods 0.000 claims description 2
- 239000011398 Portland cement Substances 0.000 claims 1
- 239000002994 raw material Substances 0.000 abstract description 13
- 239000002910 solid waste Substances 0.000 abstract description 5
- 239000004566 building material Substances 0.000 abstract description 4
- 239000000463 material Substances 0.000 description 6
- 239000000047 product Substances 0.000 description 6
- 238000005516 engineering process Methods 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- 239000000378 calcium silicate Substances 0.000 description 3
- 229910052918 calcium silicate Inorganic materials 0.000 description 3
- OYACROKNLOSFPA-UHFFFAOYSA-N calcium;dioxido(oxo)silane Chemical compound [Ca+2].[O-][Si]([O-])=O OYACROKNLOSFPA-UHFFFAOYSA-N 0.000 description 3
- 239000004568 cement Substances 0.000 description 3
- 229910001220 stainless steel Inorganic materials 0.000 description 3
- 239000010935 stainless steel Substances 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 2
- 238000010276 construction Methods 0.000 description 2
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 2
- 238000004090 dissolution Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 229910052863 mullite Inorganic materials 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 239000003469 silicate cement Substances 0.000 description 2
- 229910052814 silicon oxide Inorganic materials 0.000 description 2
- 230000003068 static effect Effects 0.000 description 2
- 238000001291 vacuum drying Methods 0.000 description 2
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000012141 concentrate Substances 0.000 description 1
- 230000009514 concussion Effects 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 238000005187 foaming Methods 0.000 description 1
- 238000002955 isolation Methods 0.000 description 1
- 239000006101 laboratory sample Substances 0.000 description 1
- 239000011344 liquid material Substances 0.000 description 1
- 238000012423 maintenance Methods 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 230000002787 reinforcement Effects 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 235000012239 silicon dioxide Nutrition 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 238000010025 steaming Methods 0.000 description 1
- 239000008030 superplasticizer Substances 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000002351 wastewater 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
- 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
- C04B40/02—Selection of the hardening environment
- C04B40/024—Steam hardening, e.g. in an autoclave
-
- 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
- C04B2111/40—Porous or lightweight 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
- 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)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The invention discloses a preparation method of autoclaved eggshell sand, which is prepared from bulk industrial solid waste fly ash, slag and carbide slag serving as raw materials through blank making, autoclaved reaction, shaping and drying. The eggshell sand shell is hard, good in sphericity, controllable in grain size and shell thickness, and can meet the raw material requirements of future refined, light and high-strength building materials.
Description
Technical Field
The invention discloses a preparation method of autoclaved eggshell sand, which takes fly ash, slag and carbide slag as raw materials and is obtained through blank making, autoclaved reaction, shaping and drying. Belongs to silicate, autoclaved maintenance light building materials, artificial hollow stones and artificial hollow sand, and belongs to comprehensive utilization of solid wastes in bulk industry.
Background
Aerated concrete derived from artificial mullite technology, particularly aerated concrete blocks, are extremely popular. The method meets the requirements of building markets, simultaneously digests a large amount of industrial solid wastes, and is a two-purpose building material project. However, with new technical popularization of energy conservation, assembly type construction, heat preservation, same service life of construction and the like of the building, the air adding block cannot meet the technical indexes of the self-heat-preservation building block in the severe cold region, and falls into a forced upgrading or forced obsolete place. The eggshell structure with the hollow shell and the compact shell has good structural strength, one hole, one shell and one shell, and the aerated block similar to eggshell stacking is manufactured, obviously, all indexes of the aerated block can reach the standard, but also obviously, no similar technology capable of realizing batch industrialized production exists. If eggshell sand having a hollow structure similar to eggshells can be prepared, not only the above problems are solved, but also the eggshell sand becomes an excellent building material raw material for future refinement, lightening and high reinforcement.
The ceramsite has some similarities of eggshell sand, but the internal structure wastes limited mass, the specific surface area of the ceramsite is large, and the structure is loose. The eggshell sand concentrates all the mass on the dense and hard shell, the inside of the eggshell sand is clean and free, and the compactness of the shell is high. For products with volume weight smaller than 350 kg and strength larger than or equal to 5MPa which are required in the market at present, the ceramsite is basically impossible, because the ceramsite with the volume weight is difficult to realize the compressive strength of 5 MPa. The eggshell sand is reasonably graded with proper grain size and proper shell thickness.
Disclosure of Invention
The technology of forming mullite phase by autoclaved reaction by taking bulk industrial solid wastes as raw materials is mature. The problem to be solved is to prepare the eggshell sand with thin and compact shell, high strength and large volume and hollow inside by using the mature material technology, but the similar technology, especially the high-strength eggshell sand with controllable particle size and controllable shell thickness, does not exist.
The industrialization of the silica gel hollow sphere provides possibility for preparing eggshell sand by using a silicon-calcium material. The silica gel hollow sphere is formed by taking inorganic silica gel as a raw material, extruding and granulating, and foaming at a high temperature. The product has the characteristics of good sphericity and good grain channel consistency. The main component of the product is high-activity silicon oxide, the high-activity silicon oxide can be slowly dissolved in a high-alkali environment, and silicic acid formed after dissolution can rapidly react with calcareous raw materials to generate calcium silicate so as to form early strength.
The experiment is carried out in a roller stirrer, firstly, the silica gel hollow sphere is put into the roller stirrer, then deionized water mixed with a water reducing agent is added, the ground and 100-mesh-sieve-sieved calcium silicate powder is slowly added, the powder begins to adhere to the silica gel hollow sphere to form a shell, the stirring is continued for a period of time, and the prefabricated eggshell sand blank has a certain strength. All appeared to be successful. However, the prepared eggshell sand is put into a mold box, the eggshell sand is sent into a reaction kettle to be pressurized by steam, the mold box is taken out after the steaming is finished, the result is unsatisfactory, the eggshell sand is all stuck together, and the eggshell sand cannot be completely separated. Various isolation methods are tried, and finally calcium carbonate is selected as an isolating agent, so that the eggshell sand which can be simply dispersed is obtained.
On the basis, various water reducers are studied, and the polycarboxylate water reducer is selected as a preferable one, so that deionized water and the polycarboxylate water reducer are clarifiedProportioning relation. The relation among the shell thickness, the particle size, the particle number, water, the water reducing agent and the calcium silicate powder is further optimized, and the shell with high compactness is obtained. The following steps are obtained: silica gel hollow sphere with radius r and number n of particle size, 0.15. 0.15 nr is added 2 ～0.25 nr 2 Mixing deionized water and polycarboxylate water reducer, stirring and slowly adding 0.4. 0.4 nr 2 ～0.8nr 2 Continuously stirring the ground silicon-calcium powder for more than 3min to wrap the powder into spherical shells, and slowly adding 0.003. 0.003 nr while stirring 2 ～0.006 nr 2 The mixed liquid is prepared from 5 parts by mass of deionized water and 0.1-0.65 part by mass of a polycarboxylate water reducer, the time for dissolving silica gel hollow spheres in the mixed material and reacting with calcareous raw materials in the material and the time for forming shell strength are researched, the silica gel hollow spheres are not dissolved in the mixed liquid, the silica gel hollow spheres begin to dissolve and react simultaneously after powder is added, the reaction rate is higher than the dissolution rate, the slurry is diluted or the stirrer is excessively used, the powder addition time is less than or equal to 6 minutes and can not be added at one time, the powder addition time is controlled to be 9-12 minutes from powder addition to blank forming, and a complete blank forming process is formed at the moment.
The raw material formula is further optimized, a large amount of industrial solid waste is used, fly ash, slag, carbide slag, desulfurized gypsum and cement are taken as raw materials, and the raw materials are ground and then pass through a 100-mesh sieve to form powder, wherein 80-120 parts by mass of fly ash, 5-25 parts by mass of slag, 30-60 parts by mass of carbide slag, 0.5-1.5 parts by mass of desulfurized gypsum and 15-30 parts by mass of silicate cement are adopted.
The eggshell sand blank has limited strength, and the blank is broken or deformed when the high place falls or the die box is too deep, so that the eggshell sand blank needs to be taken and put lightly when being put into the die, and the height of the die box is less than or equal to 60cm.
The relation between the pressure increasing and maintaining time, the temperature rising speed, the pressure reducing speed and the product quality is researched, wherein the pressure increasing and pressure releasing speed is less than or equal to 5 ℃/min. The temperature of the pressure maintaining period is controlled between 160 ℃ and 190 ℃, the pressure is between 1 and 1.2MPa, and the pressure maintaining time is more than or equal to 30 minutes.
The vibration polishing machine with stirring is selected as shaping equipment, shaping is realized by mutual friction of eggshell sand, the washed wastewater can be recycled through precipitation, and the precipitate is used as a cement raw material and is calcined into cement for recycling.
Drying the wet eggshell sand after shaping treatment at the temperature below 100 ℃ or naturally airing until the free water is less than or equal to 3%, thus obtaining the eggshell sand finished product.
Example 1
The preparation method of autoclaved eggshell sand is now described in detail by taking laboratory samples as examples
Experimental facilities: 100 target standard sieve; the rotating speed of the 5L roller stirrer is 80 revolutions per minute; 2L ceramic ball mill; 90L of static autoclaved reaction kettle; 2L concussion polisher and vacuum drying oven
Raw material preparation: silica gel hollow spheres, 2L of 5mm diameter silica gel hollow spheres, about 16000 grains; liquid material, 200mL of deionized water and 13g of polycarboxylate superplasticizer; 400g of powder, 40g of slag, 110g of carbide slag, 20g of desulfurized gypsum and 90g of silicate cement; grinding all powder materials in a ceramic ball mill for 20min, and sieving with a 100-target standard sieve, wherein the sieving remainder is ignored; 1000 mesh light calcium carbonate 5g
(1) Blank manufacturing: adding all silica gel hollow spheres into a roller stirrer, stirring, adding 198g of liquid, slowly adding all powder materials within 3min, continuously stirring for more than 3min, wrapping with spheres, stirring, slowly adding 5g of calcium carbonate while forming a blank, taking out the blank, and pouring into a stainless steel mould box with 20cm x 10cm
(2) Autoclaved reaction: the stainless steel mold box and the prepared blank are put into a static autoclaved reaction kettle, the temperature is raised to 186 ℃ at the speed of 2 ℃/min, the pressure is maintained for more than or equal to 30min, the stainless steel mold box is naturally cooled, and the reaction kettle is opened to take out the mold box
(3) Shaping and polishing: pouring the eggshell sand in the mould box into an oscillating polisher, polishing for 5min, and flushing to obtain wet eggshell sand
(4) And (3) drying: and (5) putting the wet eggshell sand into a vacuum drying oven, and drying at 90 ℃ for 120min to obtain an eggshell sand finished product.
The compressive strength was measured and 10 particles were spot inspected, with an average compressive strength of 139N and a minimum 136N.
Claims (1)
1. Preparation of autoclaved eggshell sandThe method is characterized in that (1) blank making: adding silica gel hollow spheres with radius r and number n into a roller stirrer, and simultaneously adding 0.15 to 0.15 nr 2 ～0.25 nr 2 Liquid of mass, stirred while slowly adding 0.4. 0.4 nr over 3min 2 ～0.8nr 2 The ground silicon-calcium powder begins to adhere to the silica gel hollow sphere to form a shell, the silicon-calcium powder is continuously stirred for more than 1 to 3 minutes and is wrapped on the sphere, and then the silicon-calcium powder is stirred and added with 0.003. 0.003 nr 2 ～0.006 nr 2 Forming a blank of the mass of calcium carbonate, (2) carrying out an autoclaved reaction: the prepared green body is put into a mould box with the height less than or equal to 60cm, the mould box and the green body are put into an autoclaved reaction kettle together, steam is introduced into the autoclaved reaction kettle, the temperature is raised to 160-190 ℃ at the speed less than or equal to 5 ℃/min, the pressure is maintained for more than or equal to 30min, the pressure is relieved, the green body is discharged from a mould, (3) shaping and polishing are carried out: putting the autoclaved blank into a shaping stirrer, shaping and flushing to obtain wet eggshell sand, (4) drying: drying or naturally drying the wet eggshell sand to obtain an eggshell sand finished product; the mass of r corresponding to cm is g; the liquid is a mixed liquid of 5 parts by mass of deionized water and 0.1-0.65 part by mass of polycarboxylate water reducer, the ground silicon-calcium powder is prepared by grinding 80-120 parts by mass of fly ash, 5-25 parts by mass of slag, 30-60 parts by mass of carbide slag, 0.5-1.5 parts by mass of desulfurized gypsum and 15-30 parts by mass of Portland cement through a ball mill and sieving with a 100-mesh sieve; the rotating speed of the roller stirrer is 40-200 revolutions per minute; the shaping stirrer is an oscillating polisher with stirring function; the drying is natural airing or drying at the temperature of less than or equal to 100 ℃ until the free water is less than or equal to 3 percent.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110630696.6A CN113149704B (en) | 2021-06-07 | 2021-06-07 | Preparation method of autoclaved eggshell sand |
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|---|---|---|---|
| CN202110630696.6A CN113149704B (en) | 2021-06-07 | 2021-06-07 | Preparation method of autoclaved eggshell sand |
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| CN113149704A CN113149704A (en) | 2021-07-23 |
| CN113149704B true CN113149704B (en) | 2023-08-01 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE4037576A1 (en) * | 1990-11-26 | 1993-07-01 | Weiss Anneliese | Hardenable mineral foam structure - made by reacting water-glass with oxide(s) from melting and sintering processes |
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| CN203022211U (en) * | 2013-01-28 | 2013-06-26 | 邓正凯 | Compound autoclaved aerated concrete self thermal insulation masonry block |
| CN106966687B (en) * | 2017-04-07 | 2020-07-24 | 俞家欢 | Fluidity-free rapid-setting strong-binding-force phosphate cement repairing material and preparation method thereof |
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| CN112794696B (en) * | 2021-01-14 | 2022-08-23 | 湖北工业大学 | Light sound-insulation calcium silicate board and preparation method thereof |
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| CN113149704A (en) | 2021-07-23 |
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