CN113912418B - High-strength porous shale brick sintered by modified straw and preparation method thereof - Google Patents
High-strength porous shale brick sintered by modified straw and preparation method thereof Download PDFInfo
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- CN113912418B CN113912418B CN202111462582.1A CN202111462582A CN113912418B CN 113912418 B CN113912418 B CN 113912418B CN 202111462582 A CN202111462582 A CN 202111462582A CN 113912418 B CN113912418 B CN 113912418B
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- 239000010902 straw Substances 0.000 title claims abstract description 139
- 239000011449 brick Substances 0.000 title claims abstract description 94
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 239000007788 liquid Substances 0.000 claims abstract description 50
- 150000007524 organic acids Chemical class 0.000 claims abstract description 38
- 229920002678 cellulose Polymers 0.000 claims abstract description 37
- 239000001913 cellulose Substances 0.000 claims abstract description 37
- 238000005245 sintering Methods 0.000 claims abstract description 28
- 239000002440 industrial waste Substances 0.000 claims abstract description 23
- 238000001035 drying Methods 0.000 claims abstract description 16
- 238000002156 mixing Methods 0.000 claims abstract description 13
- 238000002791 soaking Methods 0.000 claims abstract description 13
- 239000002994 raw material Substances 0.000 claims abstract description 10
- 238000000034 method Methods 0.000 claims description 17
- AEMOLEFTQBMNLQ-DTEWXJGMSA-N D-Galacturonic acid Natural products O[C@@H]1O[C@H](C(O)=O)[C@H](O)[C@H](O)[C@H]1O AEMOLEFTQBMNLQ-DTEWXJGMSA-N 0.000 claims description 13
- IAJILQKETJEXLJ-UHFFFAOYSA-N Galacturonsaeure Natural products O=CC(O)C(O)C(O)C(O)C(O)=O IAJILQKETJEXLJ-UHFFFAOYSA-N 0.000 claims description 13
- IAJILQKETJEXLJ-RSJOWCBRSA-N aldehydo-D-galacturonic acid Chemical compound O=C[C@H](O)[C@@H](O)[C@@H](O)[C@H](O)C(O)=O IAJILQKETJEXLJ-RSJOWCBRSA-N 0.000 claims description 13
- AEMOLEFTQBMNLQ-UHFFFAOYSA-N beta-D-galactopyranuronic acid Natural products OC1OC(C(O)=O)C(O)C(O)C1O AEMOLEFTQBMNLQ-UHFFFAOYSA-N 0.000 claims description 13
- 239000000203 mixture Substances 0.000 claims description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 12
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims description 10
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 8
- 125000002924 primary amino group Chemical group [H]N([H])* 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- DPDPQQHHTHKSRN-UHFFFAOYSA-N 4-aminooxane-4-carboxylic acid Chemical compound OC(=O)C1(N)CCOCC1 DPDPQQHHTHKSRN-UHFFFAOYSA-N 0.000 claims description 5
- 238000005520 cutting process Methods 0.000 claims description 5
- 238000000227 grinding Methods 0.000 claims description 5
- 238000010438 heat treatment Methods 0.000 claims description 5
- 239000000843 powder Substances 0.000 claims description 5
- 238000003756 stirring Methods 0.000 claims description 5
- -1 3-aminotetralin-2H-pyran-3-carboxylic acid Chemical compound 0.000 claims description 4
- 125000003545 alkoxy group Chemical group 0.000 claims description 4
- 229910052736 halogen Inorganic materials 0.000 claims description 4
- 150000002367 halogens Chemical class 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- 229940126062 Compound A Drugs 0.000 claims description 3
- NLDMNSXOCDLTTB-UHFFFAOYSA-N Heterophylliin A Natural products O1C2COC(=O)C3=CC(O)=C(O)C(O)=C3C3=C(O)C(O)=C(O)C=C3C(=O)OC2C(OC(=O)C=2C=C(O)C(O)=C(O)C=2)C(O)C1OC(=O)C1=CC(O)=C(O)C(O)=C1 NLDMNSXOCDLTTB-UHFFFAOYSA-N 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 3
- 150000001875 compounds Chemical class 0.000 claims description 3
- 125000006273 (C1-C3) alkyl group Chemical group 0.000 claims 2
- 239000012535 impurity Substances 0.000 abstract description 10
- 239000004566 building material Substances 0.000 abstract description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 15
- 230000000052 comparative effect Effects 0.000 description 14
- 238000011056 performance test Methods 0.000 description 12
- AEMRFAOFKBGASW-UHFFFAOYSA-N Glycolic acid Chemical compound OCC(O)=O AEMRFAOFKBGASW-UHFFFAOYSA-N 0.000 description 8
- 239000007864 aqueous solution Substances 0.000 description 7
- 239000011148 porous material Substances 0.000 description 7
- 238000010304 firing Methods 0.000 description 5
- 238000012986 modification Methods 0.000 description 5
- 230000004048 modification Effects 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 4
- 239000003245 coal Substances 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- 229910052739 hydrogen Inorganic materials 0.000 description 4
- 238000005406 washing Methods 0.000 description 4
- 230000015556 catabolic process Effects 0.000 description 3
- 239000003818 cinder Substances 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- QWPPOHNGKGFGJK-UHFFFAOYSA-N hypochlorous acid Chemical compound ClO QWPPOHNGKGFGJK-UHFFFAOYSA-N 0.000 description 3
- 150000007522 mineralic acids Chemical class 0.000 description 3
- 239000002893 slag Substances 0.000 description 3
- 239000000243 solution Substances 0.000 description 3
- RBDJRWBQJANLBU-UHFFFAOYSA-N 3-aminooxane-3-carboxylic acid Chemical compound OC(=O)C1(N)CCCOC1 RBDJRWBQJANLBU-UHFFFAOYSA-N 0.000 description 2
- 229920000742 Cotton Polymers 0.000 description 2
- 241000209140 Triticum Species 0.000 description 2
- 235000021307 Triticum Nutrition 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 125000000217 alkyl group Chemical group 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000006835 compression Effects 0.000 description 2
- 238000007906 compression Methods 0.000 description 2
- 230000001419 dependent effect Effects 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000004134 energy conservation Methods 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- 239000012466 permeate Substances 0.000 description 2
- 239000010802 sludge Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 241000196324 Embryophyta Species 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- 229920002488 Hemicellulose Polymers 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 239000011469 building brick Substances 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 238000002485 combustion reaction Methods 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000001599 direct drying Methods 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000009830 intercalation Methods 0.000 description 1
- 230000002687 intercalation Effects 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229920005610 lignin Polymers 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000002715 modification method Methods 0.000 description 1
- 235000005985 organic acids Nutrition 0.000 description 1
- 230000035515 penetration Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
- C04B38/06—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof by burning-out added substances by burning natural expanding materials or by sublimating or melting out added substances
- C04B38/063—Preparing or treating the raw materials individually or as batches
- C04B38/0635—Compounding ingredients
- C04B38/0645—Burnable, meltable, sublimable materials
- C04B38/0675—Vegetable refuse; Cellulosic materials, e.g. wood chips, cork, peat, paper
-
- 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
- C04B33/00—Clay-wares
- C04B33/02—Preparing or treating the raw materials individually or as batches
- C04B33/04—Clay; Kaolin
-
- 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
- C04B33/00—Clay-wares
- C04B33/02—Preparing or treating the raw materials individually or as batches
- C04B33/13—Compounding ingredients
- C04B33/132—Waste materials; Refuse; Residues
-
- 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
- C04B33/00—Clay-wares
- C04B33/02—Preparing or treating the raw materials individually or as batches
- C04B33/13—Compounding ingredients
- C04B33/132—Waste materials; Refuse; Residues
- C04B33/1321—Waste slurries, e.g. harbour sludge, industrial muds
-
- 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
- C04B33/00—Clay-wares
- C04B33/02—Preparing or treating the raw materials individually or as batches
- C04B33/13—Compounding ingredients
- C04B33/132—Waste materials; Refuse; Residues
- C04B33/135—Combustion residues, e.g. fly ash, incineration waste
-
- 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
- C04B2235/00—Aspects relating to ceramic starting mixtures or sintered ceramic products
- C04B2235/70—Aspects relating to sintered or melt-casted ceramic products
- C04B2235/96—Properties of ceramic products, e.g. mechanical properties such as strength, toughness, wear resistance
-
- 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
- Y02P40/60—Production of ceramic materials or ceramic elements, e.g. substitution of clay or shale by alternative raw materials, e.g. ashes
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Materials Engineering (AREA)
- Dispersion Chemistry (AREA)
- Environmental & Geological Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Combustion & Propulsion (AREA)
- Compositions Of Oxide Ceramics (AREA)
- Porous Artificial Stone Or Porous Ceramic Products (AREA)
Abstract
The invention discloses a high-strength porous shale brick sintered by using modified straw and a preparation method thereof, belonging to the technical field of building materials. Specifically, firstly, soaking straw which at least comprises 23.5 weight percent of cellulose in a modifying liquid for more than 50 minutes, drying to obtain modified straw, and then mixing and sintering the raw materials to prepare a sintered brick; the modifying liquid comprises 0.05-10 mol/L of polar organic acid with molecular weight less than or equal to 220, and the pH value of the modifying liquid is 3.5-6.5; the raw materials comprise 40-100 parts of shale, 20-60 parts of modified straw and 10-50 parts of industrial waste residue in a mass ratio. According to the invention, part of organic impurities and inorganic matters in the straw can be removed, and the porosity of the straw is improved on the premise of ensuring the structural strength and toughness of the straw, so that other sintering components are easier to infiltrate into the straw, and the mechanical strength and the porosity of the sintered brick are improved.
Description
Technical Field
The invention belongs to the technical field of building materials, and particularly relates to a high-strength porous shale brick sintered by using modified straws and a preparation method thereof.
Background
Along with the continuous improvement of the requirements of energy conservation, environmental protection and environmental protection, the requirements of various countries in the world on the energy conservation technology of buildings are also higher. The conventional brick material is complex in preparation process and easy to pollute the environment, especially the firing of red bricks is easy to destroy cultivated land and consume coal in a large amount, and the periphery of a brick factory is seriously polluted, so that plants and crops are difficult to survive. The straw is a green and environment-friendly renewable resource, but a large amount of straw is still used as an incineration raw material or directly used as waste for combustion in real life, which causes the atmospheric pollution, damages the ecological environment and wastes valuable renewable resources. Therefore, the building brick made of the straw not only can effectively utilize the precious renewable resources, but also avoids pollution caused by firing the traditional brick, and a plurality of related researches are reported at present.
Through retrieval, chinese patent No. 102126869A discloses a shale straw sintered heat-insulating light brick which is prepared from 40-70 parts of shale, 18-30 parts of crop straw and 20-40 parts of industrial waste residues by mass, and a sintering preparation method thereof. According to the patent, the straw, the shale and the industrial waste residues are added for mixed sintering, so that not only is the use of materials forbidden by China such as clay and the like for making bricks avoided, but also the sintered bricks with small density and high strength can be obtained after sintering. However, the method for directly mixing and sintering the straws can lead the pore structure of the sintered brick to be mainly dependent on the macroscopic size of the straws, because the straws contain a great amount of cellulose and also contain hemicellulose, lignin, other inorganic matters and other impurities, the mechanical strength of the straws is mainly dependent on a network structure formed by long-chain cellulose and the lap joint of the long-chain cellulose, but the existence of the impurities can prevent the penetration of other components, so that the pores formed by final sintering are too large and uneven, and the mechanical property and the porosity of the sintered brick are further reduced, so if the impurities can be removed, the straws can be effectively loosened, the porosity of the straws is increased, and the porosity and the strength of the sintered brick can be increased by mixing the straws with other components to prepare the sintered brick.
Therefore, it is needed to design a method for effectively removing impurities in the straw and loosening the straw, so that the porous straw and other sintering components are mixed and sintered, and the mechanical property and the porosity of the sintered brick are improved.
Disclosure of Invention
1. Problems to be solved
Aiming at the problems of lower porosity, non-uniformity and insufficient mechanical property of a sintered brick formed by mixing and sintering the straw with a sintering component due to the fact that the straw is compact in the prior art, the invention provides the high-strength porous shale brick sintered by using the modified straw and the preparation method thereof; by modifying the straw, the straw becomes loose and porous, thereby effectively solving the problems of lower porosity and insufficient mechanical property of the sintered brick formed by sintering the straw with compacter straw.
2. Technical proposal
In order to solve the problems, the technical scheme adopted by the invention is as follows:
the invention relates to a preparation method for sintering a high-strength porous shale brick by using modified straw, which comprises the steps of firstly soaking straw which at least comprises 23.5wt% of cellulose in a modified liquid for more than 50min, drying to obtain the modified straw, and then mixing and sintering raw materials to prepare the sintered brick; the modifying liquid comprises 0.05-10 mol/L of polar organic acid with molecular weight less than or equal to 220, and the pH value of the modifying liquid is 3.5-6.5; the raw materials comprise 40-100 parts of shale, 20-60 parts of modified straw and 10-50 parts of industrial waste residue in a mass ratio.
The preparation method of the invention has the following action principle: because organic matters such as cellulose and the like in the straw and other sintering components such as shale, industrial waste residues and the like are generally firmly combined, and are difficult to permeate into the straw, the pores in the sintered brick obtained by sintering the mixed straw mainly depend on the macroscopic size of the straw, and the obtained pores are not uniform and large, so that the method is not beneficial to manufacturing of the high-strength and high-porosity sintered porous brick. According to the invention, the straw is modified by soaking the straw in the modifying liquid, the polar organic acid in the modifying liquid can corrode inorganic matters and degrade other organic impurities to generate certain pores, and on the other hand, the action principle of D-galacturonic acid and cellulose in fig. 1 can be referred, when the straw contacts cellulose, the straw can permeate between closely-combined cellulose chains to prop the cellulose chains, so that a skeleton network formed by overlapping the cellulose becomes more porous, and certain pores are further generated, thereby ensuring the mechanical strength of the straw, and the straw becomes porous.
Although the acid solution has certain degradation capability on cellulose, the degradation of cellulose can be avoided as much as possible by controlling the components, concentration, pH and temperature of the modifying solution. On the basis, the degradation of cellulose can be further prevented by optimizing the structure of the polar organic acid, so that the modified straw still contains a large amount of cellulose networks, and the mechanical strength and toughness of the straw are further ensured.
Preferably, the modifying liquid also comprises inorganic acid, and the inorganic acid comprises HCl, HBr, H 2 SO 4 、H 2 SO 3 、HNO 3 、HClO 4 One or more of (a)The inorganic acid is used for adjusting the pH value of the modified liquid, and can continuously transfer hydrogen ions to the polar organic acid to promote the polar organic acid to continuously consume other surrounding organic impurities and inorganic matters in the process of embedding the polar organic acid into the middle of cellulose, so that the straw becomes more porous.
Preferably, the polar organic acid comprises acetic acid or glycolic acid or compound a; the chemical formula of the compound A is as follows:
in the above chemical formula, the R 1 Is- (CH) 2 ) n COOH, said R 2 ～R 10 At least one of them being hydroxy or amino or carboxyl, the others being identical or different and each independently being-H or C 1～3 Alkyl or alkoxy or carboxyl or amino or hydroxyl or halogen, wherein n=0 to 2;
or said R 1 Is- (CH) optionally substituted by hydroxy or amino or carboxy 2 ) n COOH, said R 2 ～R 10 Identical or different and are each independently-H or C 1～3 Alkyl or alkoxy or carboxyl or amino or hydroxyl or halogen, where n=1 or 2.
Preferably, the compound a comprises 4-aminotetrahydropyran-4-carboxylic acid or 3-aminotetrahydro-2H-pyran-3-carboxylic acid or 1-amino- (tetrahydropyran-3-yl) acetic acid or D-galacturonic acid.
Wherein the structural formula of the 4-aminotetrahydropyran-4-carboxylic acid isThe structural formula of the 3-aminotetrahydro-2H-pyran-3-carboxylic acid is +.>1-amino- (tetrahydropyran-3-yl) acetic acid has the structural formulaD-galactoseUronic acid with the formula->
Preferably, the specific operation steps are:
(1) Cutting and cleaning the straws;
(2) Heating the modified liquid to 30-60 ℃, immersing the cleaned straw in the modified liquid, uniformly stirring and soaking for 1-5 h;
(3) Filtering the soaked straw and drying to obtain modified straw;
(4) And (3) grinding shale and industrial waste residues, putting the ground shale and the modified straw into a mixer, uniformly mixing, and then extruding, forming and sintering to obtain the sintered brick.
Preferably, in the step (1), the straw is cut to 0.2 cm-5 cm and washed 3-5 times with clean water.
Preferably, the straw comprises 35-65wt% of cellulose; in the step (2), the modifying liquid comprises 0.5mol/L to 4mol/L of polar organic acid, and the pH value of the modifying liquid is=4 to 5.
Preferably, in the step (3), the soaked straw is filtered and then dried, and then the straw is transferred into deionized water to be soaked for 2-10 min, and the straw is taken out and dried to obtain the modified straw. The method is characterized in that the embedded small molecular polar organic acid still has certain water solubility, the direct cleaning has the risk of falling off, the direct drying can lead the polar organic acid to be tightly combined with cellulose, and then the deionized water soaking is carried out for a short time, so that the impurities in the reaction product can be effectively removed.
Preferably, in the step (4), shale and industrial waste residue are firstly ground into powder of 0.3-3 mm, then 50-80 parts of shale, 25-40 parts of modified straw and 15-25 parts of industrial waste residue are put into a mixer according to the mass ratio to be uniformly mixed, the mixture is extruded and molded by a vacuum extruder of 2-5 MPa, and finally the mixture is dried and then is placed into a sintering furnace of 850-1200 ℃ to be sintered, so that the sintered brick is obtained.
Preferably, the straw includes rice straw, cotton straw, wheat straw, and the like.
Preferably, the shale comprises a ferrous shale or a siliceous shale, and the industrial waste residue comprises one or a mixture of a plurality of slag, coal cinder or industrial sludge.
Preferably, the cellulose content in the straw is X wt%, the concentration of the polar organic acid in the modified liquid is Y mol/L, Y/x=0.01-0.12, and under the condition that the proportion, the cellulose content and the content of the polar organic acid can be better matched, and on the premise that the straw becomes loose and porous, excessive organic impurities can not be doped.
The invention also provides a sintered brick, which is prepared by the preparation method for sintering the high-strength porous shale brick by using the modified straw.
3. Advantageous effects
Compared with the prior art, the invention has the beneficial effects that:
(1) The invention relates to a preparation method for sintering a high-strength porous shale brick by using modified straw, which comprises the steps of firstly soaking straw which at least comprises 23.5wt% of cellulose in a modified liquid for more than 50min, drying to obtain the modified straw, and then mixing and sintering raw materials to prepare the sintered brick; the modifying liquid comprises 0.05-10 mol/L of polar organic acid with molecular weight less than or equal to 220, and the pH value of the modifying liquid is 3.5-6.5; the raw materials comprise 40-100 parts of shale, 20-60 parts of modified straw and 10-50 parts of industrial waste residue in a mass ratio; by the method, part of organic impurities and inorganic matters in the straw can be removed, the porosity of the straw is improved on the premise of ensuring the structural strength and toughness of the straw, so that other sintering components are easier to infiltrate into the straw, and the mechanical strength and the porosity of the sintered brick are improved.
(2) The sintered brick is prepared by the preparation method for sintering the high-strength porous shale brick by using the modified straw, the average compressive strength of the sintered brick is 17.0-19.1 MPa, the porosity is kept above 35%, and the highest porosity can reach 38.7%, so that the sintered brick has excellent mechanical property and porosity.
Drawings
Fig. 1 is a schematic diagram of the principle of straw soaking modification of the present invention.
Detailed Description
The following detailed description of exemplary embodiments of the invention refers to the accompanying drawings, which form a part hereof, and in which are shown by way of illustration exemplary embodiments in which features of the invention are identified by reference numerals. The following more detailed description of the embodiments of the invention is not intended to limit the scope of the invention, as claimed, but is merely illustrative and not limiting of the invention's features and characteristics in order to set forth the best mode of carrying out the invention and to sufficiently enable those skilled in the art to practice the invention. It will be understood that various modifications and changes may be made without departing from the scope of the invention as defined by the appended claims. The detailed description and drawings are to be regarded in an illustrative rather than a restrictive sense, and if any such modifications and variations are desired to be included within the scope of the invention described herein. Furthermore, the background art is intended to illustrate the status and meaning of the development of the technology and is not intended to limit the invention or the application and field of application of the invention.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs; the terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
Several preferred polar organic acids in the present invention include acetic acid, glycolic acid, 4-aminotetrahydropyran-4-carboxylic acid, 3-aminotetralin-2H-pyran-3-carboxylic acid, 1-amino- (tetrahydropyran-3-yl) acetic acid and D-galacturonic acid, all of which are commercially available.
The method for detecting the performance of the baked brick comprises the following steps:
the sintered rectangular hexahedron with nominal dimensions of 240mm long, 115mm wide and 53mm high was subjected to compression resistance test and porosity test, both of which were tested with reference to the standard of GB13544-2000 "sintered porous brick", the compression resistance test of the present invention was based on 10.0MPa or more, the porosity test was based on 25% or more, and the above test results were recorded in Table 1.
The invention is further described below in connection with specific embodiments.
Example 1
The embodiment provides a high-strength porous shale brick sintered by modified straw, which adopts wheat straw with cellulose content of 50wt%, adopts siliceous shale as shale, adopts coal cinder as industrial waste residue, and prepares modified liquid before preparing the sintered brick:
the modified liquid in this example was a mixed aqueous solution of 4mol/L D-galacturonic acid and HCl, and the pH of the modified liquid was adjusted to 4.8 with HCl; the ratio of the concentration Y of the polar organic acid to the cellulose content X in this example was 0.08.
The preparation method comprises the following steps:
(1) Cutting the straw into 0.5cm, and washing with clear water for 3 times;
(2) Heating the modifying liquid to 35 ℃, immersing the cleaned straw in the modifying liquid, uniformly stirring and immersing for 1.5h;
(3) Filtering soaked straws, drying at 60 ℃, transferring the straws into deionized water, soaking for 3min, taking out and drying to obtain modified straws;
(4) Firstly, grinding shale and industrial waste residues into powder of 0.3mm, then, putting 60 parts of shale, 37 parts of modified straw and 15 parts of industrial waste residues together according to the mass ratio into a mixer for uniform mixing, then, extruding and forming the mixture by using a vacuum extruder of 3MPa, and finally, drying and then, placing the mixture in a sintering furnace at 1100 ℃ for firing to obtain the sintered brick, wherein the performance detection result is shown in Table 1.
Table 1, sintered brick performance data obtained for each example and comparative example
| Description of the embodiments | Average compressive strength | Porosity of the porous material |
| Example 1 | 18.9MPa | 38.5％ |
| Example 2 | 19.1MPa | 38.0％ |
| Example 3 | 18.3MPa | 38.7％ |
| Example 4 | 19.0MPa | 37.2％ |
| Example 5 | 18.1MPa | 38.4％ |
| Example 6 | 18.0MPa | 38.4％ |
| Example 7 | 18.2MPa | 36.6％ |
| Example 8 | 17.8MPa | 38.2％ |
| Example 9 | 17.9MPa | 37.8％ |
| Example 10 | 17.0MPa | 37.3％ |
| Example 11 | 17.5MPa | 35.1％ |
| Example 12 | 17.4MPa | 36.0％ |
| Comparative example 1 | 14.6MPa | 31.6％ |
| Comparative example 2 | 14.2MPa | 33.4％ |
| Comparative example 3 | 17.5MPa | 34.1％ |
Example 2
The embodiment provides a high-strength porous shale brick sintered by modified straw, which adopts straw with 45wt% cellulose content, shale adopts siliceous shale, industrial waste residue adopts a mixture of coal cinder and slag, and modified liquid is prepared before the sintered brick is prepared:
the modified liquid in this example was 1.8mol/L of D-galacturonic acid and HClO 4 Mixing the aqueous solutions with HClO 4 Adjusting the pH of the modified liquid to 5.5; the ratio of the concentration Y of the polar organic acid to the cellulose content X in this example was 0.04.
The preparation method comprises the following steps:
(1) Cutting the straw into 1cm, and washing with clear water for 3 times;
(2) Heating the modified liquid to 35 ℃, immersing the cleaned straw in the modified liquid, uniformly stirring and immersing for 3 hours;
(3) Filtering soaked straws, drying at 60 ℃, transferring the straws into deionized water, soaking for 2min, taking out and drying to obtain modified straws;
(4) Firstly, grinding shale and industrial waste residues into powder of 0.5mm, then, putting 55 parts of shale, 40 parts of modified straw and 20 parts of industrial waste residues together according to the mass ratio into a mixer, uniformly mixing, extruding and forming the mixture by using a vacuum extruder of 3MPa, and finally, drying and then, placing the mixture in a sintering furnace at 950 ℃ for firing to obtain the sintered brick, wherein the performance detection result is shown in Table 1.
Example 3
The embodiment provides a high-strength porous shale brick sintered by using modified straw, cotton straw with cellulose content of 35wt%, shale which is iron shale, industrial waste residue which is a mixture of slag and industrial sludge is adopted, and a modified liquid is prepared before the sintered brick is prepared:
the modified liquid in this example was prepared from 0.35mol/L of D-galacturonic acid and H 2 SO 3 Mixing the aqueous solutions with H 2 SO 3 Adjusting the pH of the modified liquid to 6.2; the ratio of the concentration Y of the polar organic acid to the cellulose content X in this example was 0.01.
The preparation method comprises the following steps:
(1) Cutting the straw into 1.5cm, and washing with clear water for 3 times;
(2) Heating the modifying liquid to 30 ℃, immersing the cleaned straw in the modifying liquid, uniformly stirring and immersing for 5 hours;
(3) Filtering soaked straws, drying at 60 ℃, transferring the straws into deionized water, soaking for 2min, taking out and drying to obtain modified straws;
(4) Firstly, grinding shale and industrial waste residues into powder of 0.6mm, then, putting 60 parts of shale, 35 parts of modified straw and 15 parts of industrial waste residues together according to the mass ratio into a mixer for uniform mixing, then, extruding and forming the mixture by using a vacuum extruder of 3MPa, and finally, drying and then, placing the mixture in a sintering furnace at 1150 ℃ for firing to obtain the sintered brick, wherein the performance detection result is shown in Table 1.
Example 4
The embodiment provides a high-strength porous shale brick sintered by modified straw, the preparation method is basically the same as that of embodiment 1, and the main difference between the two is that:
1) The modified liquid in this example was a mixed aqueous solution of 0.2mol/L D-galacturonic acid and HCl, and the pH of the modified liquid was adjusted to 6.5 with HCl; the ratio of the concentration Y of the polar organic acid to the content X of the cellulose in this example was 0.004.
The final sintered brick performance test results are shown in Table 1.
Example 5
The embodiment provides a high-strength porous shale brick sintered by modified straw, the preparation method is basically the same as that of embodiment 1, and the main difference between the two is that:
1) The modified liquid in this example was a mixed aqueous solution of 1mol/L D-galacturonic acid and HCl, and the pH of the modified liquid was adjusted to 5.6 with HCl; the ratio of the concentration Y of the polar organic acid to the cellulose content X in this example was 0.02.
The final sintered brick performance test results are shown in Table 1.
Example 6
The embodiment provides a high-strength porous shale brick sintered by modified straw, the preparation method is basically the same as that of embodiment 1, and the main difference between the two is that:
1) The modified liquid in this example was a mixed aqueous solution of 5.5mol/L D-galacturonic acid and HCl, and the pH of the modified liquid was adjusted to 4.6 with HCl; the ratio of the concentration Y of the polar organic acid to the cellulose content X in this example was 0.11.
The final sintered brick performance test results are shown in Table 1.
Example 7
The embodiment provides a high-strength porous shale brick sintered by modified straw, the preparation method is basically the same as that of embodiment 1, and the main difference between the two is that:
1) The modified liquid in this example was a mixed aqueous solution of 10mol/L D-galacturonic acid and HCl, and the pH of the modified liquid was adjusted to 4.5 with HCl; the ratio of the concentration Y of the polar organic acid to the cellulose content X in this example was 0.2.
The final sintered brick performance test results are shown in Table 1.
Example 8
The embodiment provides a high-strength porous shale brick sintered by modified straw, the preparation method is basically the same as that of embodiment 1, and the main difference between the two is that:
1) The polar organic acid in this example was 4-aminotetrahydropyran-4-carboxylic acid.
The final sintered brick performance test results are shown in Table 1.
Example 9
The embodiment provides a high-strength porous shale brick sintered by modified straw, the preparation method is basically the same as that of embodiment 1, and the main difference between the two is that:
1) The polar organic acid in this example was 3-aminotetralin-2H-pyran-3-carboxylic acid.
The final sintered brick performance test results are shown in Table 1.
Example 10
The embodiment provides a high-strength porous shale brick sintered by modified straw, the preparation method is basically the same as that of embodiment 1, and the main difference between the two is that:
1) The polar organic acid in this example was 1-amino- (tetrahydropyran-3-yl) acetic acid.
The final sintered brick performance test results are shown in Table 1.
Example 11
The embodiment provides a high-strength porous shale brick sintered by modified straw, the preparation method is basically the same as that of embodiment 1, and the main difference between the two is that:
1) The polar organic acid in this example was acetic acid.
The final sintered brick performance test results are shown in Table 1.
Example 12
The embodiment provides a high-strength porous shale brick sintered by modified straw, the preparation method is basically the same as that of embodiment 1, and the main difference between the two is that:
1) The polar organic acid in this example is glycolic acid.
The final sintered brick performance test results are shown in Table 1.
Comparative example 1
This comparative example provides a conventional sintered brick prepared in substantially the same manner as in example 1, with the main difference that:
1) The modified liquid contains no polar organic acid, and is only an aqueous HCl solution with ph=4.8.
The final sintered brick performance test results are shown in Table 1.
Comparative example 2
This comparative example provides a conventional sintered brick prepared in substantially the same manner as in example 1, with the main difference that:
1) The straw was directly washed without drying treatment after filtration in step (3) of example 1.
The final sintered brick performance test results are shown in Table 1.
Comparative example 3
This comparative example provides a conventional sintered brick prepared in substantially the same manner as in example 1, with the main difference that:
1) The soaking time in step (3) of example 1 was 60min.
The final sintered brick performance test results are shown in Table 1.
As can be seen by comparing the performance data of examples 1-12, the compressive strength of the sintered brick prepared by the straw modification method is not lower than 17.0MPa, and particularly the porosity is 35.1% -38.7%, compared with the traditional technology, the porosity of the sintered brick is effectively increased. It was also found that the presence of the polar organic acid plays a critical role in improving the performance of the sintered brick in comparison with comparative example 1.
In addition, from the comparison of the performance data of examples 1 to 10 and examples 11 to 12, the compressive strength and porosity of the sintered bricks obtained in examples 1 to 10 are higher, presumably because the polar organic acid molecules have similar structures to those of the cellulose monomers, resulting from intercalation between cellulose chains by hydrogen bonding, and especially, the compressive strength of the sintered bricks can reach 19.1MPa by using D-galacturonic acid in examples 1 to 3, which has a great correlation with the structure of the polar organic acid. Even so, the use of acetic acid or glycolic acid, a conventional drug, can also result in higher compressive strength and porosity of the baked brick, so the applicant suggests that for applications where the performance or accuracy requirements of the baked brick are not high, the use of acetic acid is sufficient, neither too toxic nor the raw materials are readily available, whereas if the requirements are high, small molecular organic acid monomers similar to those of D-galacturonic acid and the like can be used as much as possible.
In addition, the cases of comparative example 2 and comparative example 3 are similar, mainly because the polar organic acid partially embedded in the cellulose is removed, and the operation means of direct washing after soaking in comparative example 2 has a greater influence on the removal of the polar organic acid, and thus the compressive strength and porosity of the baked brick are not too high.
The invention has been described in detail hereinabove with reference to specific exemplary embodiments thereof. It will be understood that various modifications and changes may be made without departing from the scope of the invention as defined by the appended claims. The detailed description and drawings are to be regarded in an illustrative rather than a restrictive sense, and if any such modifications and variations are desired to be included within the scope of the invention described herein. Furthermore, the background art is intended to illustrate the status and meaning of the development of the technology and is not intended to limit the invention or the application and field of application of the invention.
More specifically, although exemplary embodiments of the present invention have been described herein, the present invention is not limited to these embodiments, but includes any and all embodiments that have been modified, omitted, e.g., combined, adapted, and/or substituted between the various embodiments, as would be recognized by those skilled in the art in light of the foregoing detailed description. The limitations in the claims are to be interpreted broadly based on the language employed in the claims and not limited to examples described in the foregoing detailed description or during the prosecution of the application, which examples are to be construed as non-exclusive. Any steps recited in any method or process claims may be executed in any order and are not limited to the order presented in the claims. The scope of the invention should, therefore, be determined only by the appended claims and their legal equivalents, rather than by the descriptions and examples given above.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. In case of conflict, the present specification, definitions, will control. Where a pressure, concentration, temperature, time, or other value or parameter is expressed as a range, preferred range, or as a range bounded by a list of upper preferable values and lower preferable values, this is to be understood as specifically disclosing all ranges formed from any pair of any upper range limit or preferred value and any lower range limit or preferred value, regardless of whether ranges are separately disclosed. For example, a range of 1-50 should be understood to include any number, combination of numbers, or subranges of numbers selected from 1, 2, 3, 4, 5, 6, 7, 8, 9, 10, 11, 12, 13, 14, 15, 16, 17, 18, 19, 20, 21, 22, 23, 24, 25, 26, 27, 28, 29, 30, 31, 32, 33, 34, 35, 36, 37, 38, 39, 40, 41, 42, 43, 44, 45, 46, 47, 48, 49, or 50, as well as all fractional values between the integers described above, such as 1.1, 1.2, 1.3, 1.4, 1.5, 1.6, 1.7, 1.8, and 1.9. Regarding sub-ranges, specifically considered are "nested sub-ranges" that extend from any end point within the range. For example, the nested subranges of exemplary ranges 1-50 can include 1-10, 1-20, 1-30, and 1-40 in one direction, or 50-40, 50-30, 50-20, and 50-10 in another direction.
Claims (9)
1. A method for preparing a high-strength porous shale brick by utilizing modified straw is characterized in that straw which at least comprises 23.5wt% of cellulose is soaked in a modifying liquid for more than 50min, the modified straw is obtained by drying, and then raw materials are mixed and sintered to prepare the sintered brick; the modifying liquid comprises 0.05-10 mol/L of polar organic acid with molecular weight less than or equal to 220, and the pH value of the modifying liquid is 3.5-6.5; the raw materials comprise 40-100 parts of shale, 20-60 parts of modified straw and 10-50 parts of industrial waste residue in a mass ratio;
the polar organic acid includes compound a; the chemical formula of the compound A is as follows:
in the above chemical formula, R1 is- (CH 2) nCOOH, at least one of R2 to R10 is hydroxyl or amino or carboxyl, and the others are the same or different and are each independently-H or C1-3 alkyl or alkoxy or carboxyl or amino or hydroxyl or halogen, wherein n=0 to 2; or said R1 is- (CH 2) nCOOH optionally substituted with hydroxy or amino or carboxy, said R2 to R10 are the same or different and are each independently-H or C1-3 alkyl or alkoxy or carboxy or amino or hydroxy or halogen, wherein n=1 or 2.
2. The method for preparing the high-strength porous shale brick sintered by using modified straws according to claim 1, wherein the compound A comprises 4-aminotetrahydropyran-4-carboxylic acid or 3-aminotetralin-2H-pyran-3-carboxylic acid or 1-amino- (tetrahydropyran-3-yl) acetic acid or D-galacturonic acid.
3. The method for preparing the high-strength porous shale brick sintered by using the modified straw according to claim 1, which is characterized by comprising the following specific operation steps:
(1) Cutting and cleaning the straws;
(2) Heating the modified liquid to 30-60 ℃, immersing the cleaned straw in the modified liquid, uniformly stirring and soaking for 1-5 h;
(3) Filtering the soaked straw and drying to obtain modified straw;
(4) And (3) grinding shale and industrial waste residues, putting the ground shale and the modified straw into a mixer, uniformly mixing, and then extruding, forming and sintering to obtain the sintered brick.
4. The method for preparing a porous shale brick sintered with modified straw according to claim 3, wherein in the step (1), the straw is cut to 0.2 cm-5 cm and washed 3-5 times with clean water.
5. The method for preparing the high-strength porous shale brick sintered by using the modified straw according to claim 3, wherein the straw comprises 35-65wt% of cellulose; in the step (2), the modifying liquid comprises 0.5mol/L to 4mol/L of polar organic acid, and the pH value of the modifying liquid is=4 to 5.
6. The method for preparing the high-strength porous shale brick by using the modified straw as claimed in claim 3, wherein in the step (3), the soaked straw is filtered and then dried, the straw is transferred into deionized water and soaked for 2-10 min, and the modified straw is obtained after being taken out and dried.
7. The method for preparing the high-strength porous shale brick by using the modified straw as claimed in claim 3, wherein in the step (4), shale and industrial waste residues are firstly ground into powder of 0.3-3 mm, 50-80 parts of shale, 25-40 parts of modified straw and 15-25 parts of industrial waste residues are then put into a mixer according to the mass ratio to be uniformly mixed, the mixture is extruded and molded by a vacuum extruder of 2-5 MPa, and finally the mixture is dried and then is put into a sintering furnace of 850-1200 ℃ to be sintered, so that the sintered brick is obtained.
8. The method for preparing the high-strength porous shale brick sintered by using modified straws according to claim 1, wherein the cellulose content in the straws is X wt%, and the concentration of the polar organic acid in the modified liquid is Y mol/L, and Y/x=0.01-0.12.
9. A baked brick characterized in that the baked brick is prepared by a preparation method for sintering high-strength porous shale bricks by using modified straws according to any one of claims 1-8.
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