CN113149704A - Preparation method of autoclaved eggshell sand - Google Patents
Preparation method of autoclaved eggshell sand Download PDFInfo
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- CN113149704A CN113149704A CN202110630696.6A CN202110630696A CN113149704A CN 113149704 A CN113149704 A CN 113149704A CN 202110630696 A CN202110630696 A CN 202110630696A CN 113149704 A CN113149704 A CN 113149704A
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- sand
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- 210000003278 egg shell Anatomy 0.000 title claims abstract description 35
- 102000002322 Egg Proteins Human genes 0.000 title claims abstract description 34
- 108010000912 Egg Proteins Proteins 0.000 title claims abstract description 34
- 239000004576 sand Substances 0.000 title claims abstract description 33
- 238000002360 preparation method Methods 0.000 title claims abstract description 7
- 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 9
- 238000006243 chemical reaction Methods 0.000 claims abstract description 8
- 239000010881 fly ash Substances 0.000 claims abstract description 6
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 43
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 18
- 239000000843 powder Substances 0.000 claims description 17
- 239000000463 material Substances 0.000 claims description 13
- 229910002027 silica gel Inorganic materials 0.000 claims description 12
- 239000000741 silica gel Substances 0.000 claims description 12
- 238000003756 stirring Methods 0.000 claims description 11
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical compound [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 claims description 10
- 239000003638 chemical reducing agent Substances 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 9
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 5
- 229910000019 calcium carbonate Inorganic materials 0.000 claims description 5
- 238000005498 polishing Methods 0.000 claims description 5
- OSMSIOKMMFKNIL-UHFFFAOYSA-N calcium;silicon Chemical compound [Ca]=[Si] OSMSIOKMMFKNIL-UHFFFAOYSA-N 0.000 claims description 4
- 229910052602 gypsum Inorganic materials 0.000 claims description 4
- 239000010440 gypsum Substances 0.000 claims description 4
- 239000011398 Portland cement Substances 0.000 claims description 3
- 238000010438 heat treatment Methods 0.000 claims description 3
- 229910052791 calcium Inorganic materials 0.000 claims description 2
- 239000011575 calcium Substances 0.000 claims description 2
- 238000000227 grinding Methods 0.000 claims description 2
- 238000007873 sieving Methods 0.000 claims description 2
- 238000005406 washing Methods 0.000 claims description 2
- 239000002994 raw material Substances 0.000 abstract description 12
- 239000004566 building material Substances 0.000 abstract description 5
- 239000002910 solid waste Substances 0.000 abstract description 5
- 239000000047 product Substances 0.000 description 6
- 239000000378 calcium silicate Substances 0.000 description 5
- 229910052918 calcium silicate Inorganic materials 0.000 description 5
- OYACROKNLOSFPA-UHFFFAOYSA-N calcium;dioxido(oxo)silane Chemical compound [Ca+2].[O-][Si]([O-])=O OYACROKNLOSFPA-UHFFFAOYSA-N 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 239000008187 granular material Substances 0.000 description 4
- 239000002245 particle Substances 0.000 description 4
- 239000004568 cement Substances 0.000 description 3
- 229910052573 porcelain Inorganic materials 0.000 description 3
- 239000000919 ceramic Substances 0.000 description 2
- 230000006837 decompression Effects 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
- 238000000034 method Methods 0.000 description 2
- 229910052863 mullite Inorganic materials 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 230000003068 static effect Effects 0.000 description 2
- 239000004575 stone Substances 0.000 description 2
- 238000001291 vacuum drying Methods 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- 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
- 239000002969 artificial stone Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 239000004567 concrete Substances 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 230000008030 elimination Effects 0.000 description 1
- 238000003379 elimination reaction Methods 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
- 238000007689 inspection 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
- 229920005646 polycarboxylate Polymers 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
- 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
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
- 239000008030 superplasticizer 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
Abstract
The invention discloses a preparation method of autoclaved eggshell sand, which is prepared by taking bulk industrial solid waste fly ash, furnace slag and carbide slag as raw materials and performing blank making, autoclaved reaction, shaping and drying. The eggshell sand has hard shell, good sphericity, controllable grain diameter and controllable shell thickness, and can meet the requirements of raw materials for future precision, light weight and high-strength building materials.
Description
Technical Field
The invention discloses a preparation method of autoclaved eggshell sand, which is prepared by taking fly ash, furnace slag and carbide slag as raw materials and performing blank making, autoclaved reaction, shaping and drying. Belongs to silicate, autoclaved lightweight building materials, artificial hollow stone and artificial hollow sand, and belongs to the comprehensive utilization of bulk industrial solid wastes.
Background
The application of the aerated concrete derived from the artificial mullite technology, in particular to the aerated block, is extremely common. The building material can meet the building market demand and digest a large amount of industrial solid wastes, thereby being a building material project with two birds with one stone. However, along with the popularization of new technologies such as building energy conservation, assembly type buildings, heat preservation and the same service life of buildings, the air-adding block cannot meet the technical indexes of self-heat-preservation building blocks in severe cold regions, and falls into the situation of forced upgrading or forced elimination. The eggshell structure with the hollow core and the compact shell has good structural strength, and the aerated block similar to the piled eggshells can be manufactured by one hole, one shell and one shell. If the eggshell sand with a hollow structure similar to an eggshell can be prepared, the problems are solved, and the eggshell sand becomes an excellent building material with fine, light and high strength in the future.
The porcelain granules have certain similarities of eggshell sand, but limited mass is wasted in the internal structure of the porcelain granules, the specific surface area of the porcelain granules is large, and the structure is loose. All the mass of the eggshell sand is concentrated on the shell which is dense and hard, the inside of the eggshell sand is clean and falls off, and the shell compactness is high. As for the products with the volume weight less than 350 kg and the strength more than or equal to 5MPa required by the current market, the ceramsite can not be basically produced, because the compressive strength of 5MPa can not be easily realized by the ceramsite with the volume weight. The eggshell sand has proper particle size, reasonable grading and proper shell thickness to achieve the aim.
Disclosure of Invention
The artificial stone technology which takes a large amount of industrial solid wastes as raw materials and forms a mullite phase through an autoclave reaction is mature. The problem to be solved is to prepare the eggshell sand with a thin and compact shell, high strength and large volume and a hollow interior by using the mature material technology, but the eggshell sand has no similar technology, especially has controllable particle size and controllable shell thickness.
The industrialization of the silica gel hollow sphere provides possibility for preparing the eggshell sand by using the silicon-calcium material. The silica gel hollow sphere is formed by taking inorganic silica gel as a raw material, extruding and granulating and then foaming at high temperature. The product has the characteristics of good sphericity and good particle diameter consistency. Particularly, the main component of the product is high-activity silicon oxide which can be slowly dissolved in a high-alkali environment, and silicic acid formed after dissolution can quickly react with a calcareous raw material to form calcium silicate so as to form early strength.
The experiment is carried out in a drum mixer, firstly, the silica gel hollow sphere is put into the drum mixer, then, deionized water mixed with a water reducing agent is added, the ground calcium silicate powder which is sieved by a 100-mesh sieve 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 certain strength. It seems to be all right well. However, the prepared eggshell sand is put into a mould box, is sent into a reaction kettle to be pressurized by steam, and is taken out after the steam curing is finished, so that the result is not satisfactory, and the eggshell sand is completely stuck together and cannot be completely separated. Various isolation methods are tried, and finally calcium carbonate is selected as an isolating agent to obtain the eggshell sand which can be simply dispersed.
On the basis, various water reducing agents are researched, a polycarboxylic acid water reducing agent is selected as the preferable water reducing agent, and the proportioning relation of deionized water and the polycarboxylic acid water reducing agent is determined. Further optimizing the relationship among the thickness, the grain diameter and the number of grains of the shell, water, the water reducing agent and the silicon-calcium powder material, and obtaining the shell with high compactness. To obtain: adding 0.15 nr of silica gel hollow spheres with the radius r and the number of n of the particle diameters2～0.25 nr2The mixed liquid of deionized water and polycarboxylic acid water reducing agent is stirred and slowly added with 0.4 nr2～0.8nr2Continuously stirring the ground calcium silicate powder for more than 3min to wrap the calcium silicate powder into spherical shells, and slowly adding 0.003 nr of calcium silicate powder while stirring2～0.006 nr2The preparation method comprises the following steps of preparing a mixed liquid by mass of calcium carbonate, wherein the mixed liquid is a mixed liquid of 5 parts by mass of deionized water and 0.1-0.65 part by mass of a polycarboxylic acid water reducing agent, researching the time for dissolving and reacting a silica gel hollow sphere with a calcium raw material in the mixed material and the time for forming the shell strength, dissolving and reacting the silica gel hollow sphere in the mixed liquid after adding a powder material, wherein the reaction rate is higher than the dissolving rate, the silica gel hollow sphere can collapse when slurry is very thin or stirrer materials are too much, the powder material feeding time is less than or equal to 6 min and cannot be added at one time, and the time from powder feeding to blank forming is controlled to be 9-12 min, so that a complete blank forming process is formed.
The raw material formula is further optimized, a large amount of industrial solid waste is used, the fly ash, the furnace slag, the carbide slag, the desulfurized gypsum and the cement are used as raw materials, the raw materials are ground and then are sieved by a 100-mesh sieve, and a powder material is formed, wherein 80-120 parts by mass of the fly ash, 5-25 parts by mass of the furnace slag, 30-60 parts by mass of the carbide slag, 0.5-1.5 parts by mass of the desulfurized gypsum and 15-30 parts by mass of the portland cement are used.
The eggshell sand blank has limited strength, and the blank is broken or deformed when falling from a high place or the mould box is too deep, so the eggshell sand blank is lightly taken and placed when being put into a mould, and the height of the mould box is less than or equal to 60 cm.
The relationship between the pressurization maintenance time, the heating rate, the decompression rate and the product quality is researched, wherein the pressurization and the decompression are carried out at the speed of less than or equal to 5 ℃/min. And the steam curing process parameter that the temperature is controlled at 160-190 ℃ in the pressure maintaining period, the pressure is 1-1.2 MPa, and the pressure maintaining time is more than or equal to 30 min.
A vibration polishing machine with stirring is selected as a shaping device, 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 shaped wet eggshell sand at the temperature below 100 ℃, or naturally airing until the free water is less than or equal to 3 percent to obtain the finished eggshell sand product.
Detailed description of the preferred embodiment 1
Now, the preparation method of the autoclaved eggshell sand is elaborated in detail by taking laboratory samples as examples
Experimental equipment: a 100-mesh standard sieve; the rotating speed of the 5L roller stirrer is 80 r/min; 2L ceramic ball mill; a 90L static autoclave; 2L oscillating polisher and vacuum drying oven
Preparing raw materials: the silica gel hollow spheres are 2L (16000) with the diameter of 5 mm; liquid material, deionized water 200mL + polycarboxylate superplasticizer 13 g; the material of the powder comprises 400g of fly ash, 40g of slag, 110g of carbide slag, 20g of desulfurized gypsum and 90g of portland cement; grinding all powder materials in a ceramic ball mill for 20min, and sieving with a 100-mesh standard sieve with the sieve allowance omitted; 1000 mesh light calcium carbonate 5g
Firstly, blank making: adding all the silica gel hollow spheres into a roller stirrer, stirring, adding 198g of liquid, slowly adding all the powder material within 3min, continuously stirring for more than 3min to wrap the powder material into balls, slowly adding 5g of calcium carbonate while stirring to form blanks, taking out the blanks, pouring the blanks into a stainless steel die box of 20cm x 10cm
② steam pressure reaction: putting the stainless steel mold box and the prepared blank into a static autoclave, heating to 186 ℃ at the speed of 2 ℃/min, maintaining the pressure for more than or equal to 30min, naturally cooling, opening the autoclave, taking out the mold box
Thirdly, shaping and polishing: pouring the eggshell sand in the mold box into a vibration polishing machine, polishing for 5min, and washing to obtain wet eggshell sand
And fourthly, drying: and (3) putting the wet eggshell sand into a vacuum drying oven, and drying at 90 ℃ for 120min to obtain an eggshell sand finished product.
And (4) detecting the compressive strength, performing spot inspection on 10 granules, and obtaining the average compressive strength of 139N and the minimum compressive strength of 136N.
Claims (1)
1. The preparation method of the autoclaved eggshell sand is characterized by comprising the following steps: adding silica gel hollow spheres with the radius r of n into a roller stirrer, and simultaneously adding 0.15 nr2～0.25 nr2Adding 0.4 nr of liquid of certain mass while stirring slowly in 3min2～0.8nr2Continuously stirring the silicon calcium powder with good quality for more than 1-3 min to wrap the silicon calcium powder into balls, and then stirring and simultaneously adding 0.003 nr2～0.006 nr2Forming a blank by mass of calcium carbonate, namely performing steam pressure reaction: putting the prepared blank into a mold box with the height of less than or equal to 60cm, putting the mold box and the blank into an autoclave reactor together, introducing steam into the autoclave reactor, heating to 160-190 ℃ at the speed of less than or equal to 5 ℃/min, maintaining the pressure for more than or equal to 30min, releasing the pressure, taking out of a mold, and shaping and polishing: putting the blank subjected to the autoclaved reaction into a shaping stirrer, shaping and washing to obtain wet eggshell sand, and drying: drying or naturally drying the wet eggshell sand to obtain an eggshell sand finished product; the mass of the 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 a polycarboxylic acid water reducing agent, and the ground silico-calcium powder is prepared by grinding 80-120 parts by mass of fly ash, 5-25 parts by mass of furnace 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 by a ball mill and sieving the ground materials with a 100-mesh sieve; the rotating speed of the roller stirrer is 40-200 revolutions per minute; the shaping stirrer is a vibration polisher for stirring; 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.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202110630696.6A CN113149704B (en) | 2021-06-07 | 2021-06-07 | Preparation method of autoclaved eggshell sand |
Applications Claiming Priority (1)
| 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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| Publication Number | Publication Date |
|---|---|
| CN113149704A true CN113149704A (en) | 2021-07-23 |
| CN113149704B CN113149704B (en) | 2023-08-01 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202110630696.6A Active CN113149704B (en) | 2021-06-07 | 2021-06-07 | Preparation method of autoclaved eggshell sand |
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| Country | Link |
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| CN (1) | CN113149704B (en) |
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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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2021
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| 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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| JP2002037645A (en) * | 2000-05-19 | 2002-02-06 | Asahi Glass Co Ltd | Fine hollow aluminosilicate glass ball and its manufacturing method |
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| Publication number | Publication date |
|---|---|
| CN113149704B (en) | 2023-08-01 |
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