CN115959867A - Preparation method of modified oyster shell antibacterial calcium silicate board - Google Patents
Preparation method of modified oyster shell antibacterial calcium silicate board Download PDFInfo
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- CN115959867A CN115959867A CN202211498417.6A CN202211498417A CN115959867A CN 115959867 A CN115959867 A CN 115959867A CN 202211498417 A CN202211498417 A CN 202211498417A CN 115959867 A CN115959867 A CN 115959867A
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- OYACROKNLOSFPA-UHFFFAOYSA-N calcium;dioxido(oxo)silane Chemical compound [Ca+2].[O-][Si]([O-])=O OYACROKNLOSFPA-UHFFFAOYSA-N 0.000 title claims abstract description 58
- 239000000378 calcium silicate Substances 0.000 title claims abstract description 57
- 229910052918 calcium silicate Inorganic materials 0.000 title claims abstract description 57
- VTYYLEPIZMXCLO-UHFFFAOYSA-L Calcium carbonate Chemical class [Ca+2].[O-]C([O-])=O VTYYLEPIZMXCLO-UHFFFAOYSA-L 0.000 title claims abstract description 52
- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 43
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- 239000000843 powder Substances 0.000 claims abstract description 56
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 32
- 239000011575 calcium Substances 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 16
- 239000007787 solid Substances 0.000 claims abstract description 14
- 238000003756 stirring Methods 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000000835 fiber Substances 0.000 claims abstract description 11
- 238000000748 compression moulding Methods 0.000 claims abstract description 9
- 239000011812 mixed powder Substances 0.000 claims abstract description 9
- 239000011398 Portland cement Substances 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims abstract description 8
- 239000002002 slurry Substances 0.000 claims abstract description 7
- 238000002791 soaking Methods 0.000 claims abstract description 7
- 239000004568 cement Substances 0.000 claims description 18
- 238000001354 calcination Methods 0.000 claims description 12
- AXCZMVOFGPJBDE-UHFFFAOYSA-L calcium dihydroxide Chemical compound [OH-].[OH-].[Ca+2] AXCZMVOFGPJBDE-UHFFFAOYSA-L 0.000 claims description 9
- 239000000920 calcium hydroxide Substances 0.000 claims description 9
- 229910001861 calcium hydroxide Inorganic materials 0.000 claims description 9
- 238000001035 drying Methods 0.000 claims description 8
- 238000001914 filtration Methods 0.000 claims description 6
- 238000000643 oven drying Methods 0.000 claims description 6
- 229920002522 Wood fibre Polymers 0.000 claims description 5
- 230000036571 hydration Effects 0.000 claims description 5
- 238000006703 hydration reaction Methods 0.000 claims description 5
- 239000000377 silicon dioxide Substances 0.000 claims description 5
- 239000002025 wood fiber Substances 0.000 claims description 5
- 238000003825 pressing Methods 0.000 claims description 4
- 239000000126 substance Substances 0.000 claims description 4
- 238000001816 cooling Methods 0.000 claims description 3
- 238000000227 grinding Methods 0.000 claims description 3
- 235000012239 silicon dioxide Nutrition 0.000 claims description 3
- 229910001220 stainless steel Inorganic materials 0.000 claims description 3
- 239000010935 stainless steel Substances 0.000 claims description 3
- 238000004140 cleaning Methods 0.000 claims description 2
- 238000011068 loading method Methods 0.000 claims description 2
- 239000011268 mixed slurry Substances 0.000 claims description 2
- 238000010298 pulverizing process Methods 0.000 claims description 2
- 239000002994 raw material Substances 0.000 abstract description 10
- 239000002699 waste material Substances 0.000 abstract description 9
- 239000004566 building material Substances 0.000 abstract description 7
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 abstract description 3
- 229910052791 calcium Inorganic materials 0.000 abstract description 3
- 239000002028 Biomass Substances 0.000 abstract description 2
- 239000010796 biological waste Substances 0.000 abstract description 2
- 229910052500 inorganic mineral Inorganic materials 0.000 abstract description 2
- 239000011707 mineral Substances 0.000 abstract description 2
- 239000000203 mixture Substances 0.000 abstract description 2
- 239000000243 solution Substances 0.000 description 25
- 238000012360 testing method Methods 0.000 description 11
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 8
- 230000000052 comparative effect Effects 0.000 description 8
- 239000000463 material Substances 0.000 description 8
- 238000012986 modification Methods 0.000 description 6
- 230000004048 modification Effects 0.000 description 6
- 241000588724 Escherichia coli Species 0.000 description 5
- 241000191967 Staphylococcus aureus Species 0.000 description 5
- 241000237502 Ostreidae Species 0.000 description 4
- 235000020636 oyster Nutrition 0.000 description 4
- 238000004448 titration Methods 0.000 description 4
- 241000282414 Homo sapiens Species 0.000 description 3
- 229910004298 SiO 2 Inorganic materials 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 230000007423 decrease Effects 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- MKTRXTLKNXLULX-UHFFFAOYSA-P pentacalcium;dioxido(oxo)silane;hydron;tetrahydrate Chemical compound [H+].[H+].O.O.O.O.[Ca+2].[Ca+2].[Ca+2].[Ca+2].[Ca+2].[O-][Si]([O-])=O.[O-][Si]([O-])=O.[O-][Si]([O-])=O.[O-][Si]([O-])=O.[O-][Si]([O-])=O.[O-][Si]([O-])=O MKTRXTLKNXLULX-UHFFFAOYSA-P 0.000 description 3
- 239000012085 test solution Substances 0.000 description 3
- 238000005452 bending Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 238000004134 energy conservation Methods 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 230000036541 health Effects 0.000 description 2
- 238000007654 immersion Methods 0.000 description 2
- 244000005700 microbiome Species 0.000 description 2
- 238000005192 partition Methods 0.000 description 2
- KJFMBFZCATUALV-UHFFFAOYSA-N phenolphthalein Chemical compound C1=CC(O)=CC=C1C1(C=2C=CC(O)=CC=2)C2=CC=CC=C2C(=O)O1 KJFMBFZCATUALV-UHFFFAOYSA-N 0.000 description 2
- 238000005507 spraying Methods 0.000 description 2
- 241000894006 Bacteria Species 0.000 description 1
- 239000005909 Kieselgur Substances 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 description 1
- 229930006000 Sucrose Natural products 0.000 description 1
- 241000700605 Viruses Species 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 238000007605 air drying Methods 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 230000003385 bacteriostatic effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- OSMSIOKMMFKNIL-UHFFFAOYSA-N calcium;silicon Chemical compound [Ca]=[Si] OSMSIOKMMFKNIL-UHFFFAOYSA-N 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000005234 chemical deposition Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 239000004567 concrete Substances 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000008367 deionised water Substances 0.000 description 1
- 229910021641 deionized water Inorganic materials 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000000887 hydrating effect Effects 0.000 description 1
- BHEPBYXIRTUNPN-UHFFFAOYSA-N hydridophosphorus(.) (triplet) Chemical compound [PH] BHEPBYXIRTUNPN-UHFFFAOYSA-N 0.000 description 1
- 230000002401 inhibitory effect Effects 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 238000002715 modification method Methods 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000000630 rising effect Effects 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 239000002893 slag Substances 0.000 description 1
- 239000005720 sucrose Substances 0.000 description 1
- 230000008961 swelling Effects 0.000 description 1
- 238000009423 ventilation Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 230000004580 weight loss Effects 0.000 description 1
Classifications
-
- 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
- Curing Cements, Concrete, And Artificial Stone (AREA)
Abstract
The invention relates to a preparation method of a modified oyster shell antibacterial calcium silicate board. The method comprises soaking oyster shell (biomass waste) in Cu (NO) 3 ) 2 ·3H 2 In the O solution, the obtained solid is calcined after being filtered to obtain CuO/CaO powder; adding water to hydrate the mixture to obtain CuO/Ca (OH) 2 A powder; mixing the diatomite with the diatomite, adding fiber and ordinary portland cement to obtain mixed powder, adding water, and stirring to obtain a slurry; and carrying out compression molding and autoclaved curing to obtain the modified oyster shell antibacterial calcium silicate board. The invention relates to a method for preparing calcium silicate board by using modified biological waste oyster shell powder and diatomite rich in mineral resources as main raw materials, which realizes the preparation of calcium silicate boardThe calcium board has the whole body antibacterial effect, and solves the problems of serious pollution, resource shortage and the like of the traditional building materials.
Description
Technical Field
The invention belongs to the field of novel building materials, and particularly relates to a preparation method of a modified oyster shell antibacterial calcium silicate board.
Background
Calcium silicate boards are a new green and environment-friendly building material, and are popular among some consumers. The 'waste utilization' is widely developed in recent years, silica materials and calcium materials in wastes are reacted to generate tobermorite with good performance through treatment, energy conservation and environmental protection can be realized, cost is effectively reduced, and the method becomes a new trend of industrial development. At present, the scholars use the wastes such as phosphate tailings, phosphorous slag and the like to prepare a light calcium silicate board (CN 105130360B); the calcium silicate board has good breaking strength and good durability, and the basic performance requirements of the calcium silicate board can be met by combining ordinary portland cement with modified diatomite to prepare the calcium silicate board by a learner (CN 107602027A); in addition, researchers have proposed the preparation concept of the antibacterial calcium silicate board, and the antibacterial function of the calcium silicate board is realized by spraying an antibacterial material on the surface of the prepared calcium silicate board (CN 202280385).
In recent years, the widespread spread of global pandemics seriously threatens human health, work and life, and the combination of antibacterial performance with building materials is a new development trend. However, the existing mode of spraying the antibacterial material on the surface of the calcium silicate plate is easy to fall off to influence the antibacterial effect of the calcium silicate plate, and the antibacterial modification of the building raw material can ensure that the building material has continuous and stable antibacterial performance; meanwhile, the whole antibacterial activity of the building can effectively avoid the corrosion of microorganisms of the building, and the antibacterial agent has good market application prospect.
Disclosure of Invention
The invention aims to provide a preparation method of a modified oyster shell antibacterial calcium silicate board aiming at the defects in the prior art. The method comprises soaking oyster shell (biomass waste) in Cu (NO) 3 ) 2 ·3H 2 And in the O solution, filtering and calcining the obtained solid to enable main calcium raw materials of the calcium silicate board to obtain antibacterial modification, and finally realizing the whole body antibacterial effect of the calcium silicate board. The invention takes modified biological waste oyster shell powder and diatomite rich in mineral resources as main raw materialsThe preparation method of the calcium silicate board solves the problems of serious pollution, resource shortage and the like of the traditional building materials.
In order to achieve the purpose, the invention adopts the technical scheme that:
a preparation method of a modified oyster shell antibacterial calcium silicate board specifically comprises the steps of taking modified waste oyster shells, diatomite, wood fiber and cement as raw materials, and carrying out stirring, forming, pre-curing, autoclaved curing and other series of processes to obtain the modified oyster shell antibacterial calcium silicate board.
(1) Cleaning Concha Ostreae, oven drying, grinding into fine powder, soaking in Cu (NO) 3 ) 2 ·3H 2 Stirring in O solution for 2-12h, filtering, and oven drying to obtain Cu (NO) 3 ) 2 ·3H 2 O/CaCO 3 Powder;
wherein the pulverizing fineness of oyster shell powder is 100-3000 mesh, and each 800g oyster shell powder is soaked in 1-5LCu (NO) 3 ) 2 ·3H 2 In O solution; cu (NO) 3 ) 2 ·3H 2 O solution with concentration of 0.2-1 mol/L, oyster shell and Cu (NO) 3 ) 2 ·3H 2 O/CaCO 3 Drying the powder in a drying oven at 60-80 ℃ for 6-12h;
(2) Drying the solid, placing the dried solid in a muffle furnace for calcining for 5-10h at 800-950 ℃, repeatedly calcining for 1-3 times, and naturally cooling to room temperature to obtain CuO/CaO powder;
wherein, the volume of the muffle furnace can be used for calcining 1-3420g Cu (NO) per 27L 3 ) 2 ·3H 2 O/CaCO 3 A powder;
(3) Adding water into the solid to hydrate, filtering, and oven drying the obtained solid in a vacuum oven at 60-80 deg.C for 8-12h to obtain CuO/Ca (OH) 2 Powder;
wherein, the hydration procedure of CuO/CaO is as follows: adding 18g-100g of water into every 80g of calcined oyster shell powder and stirring for 2-5h;
(4) Mixing CuO/Ca (OH) 2 Mixing the powder with diatomite, adding fiber and ordinary portland cement to obtain mixed powder, adding water, and stirring to obtain slurry;
wherein the mass of the fiber is 0-5% of the mass of the mixed powder; the mass of the cement is 20-40% of the mass of the mixed powder; the mass of the water is 20-40% of the mass of the mixed powder; when the proportion of the substance is 0, the substance is not added, and the mixing and stirring of the slurry are carried out for 10-20min by adopting a pulverizer;
CuO/Ca(OH) 2 the mass ratio of the calcium hydroxide of the powder to the silicon dioxide in the diatomite is 0.83-1.2:1;
the fiber is wood fiber, and the cement is portland cement.
(5) Loading the mixed slurry into a stainless steel mold, performing compression molding in a press machine, and performing pre-curing at room temperature;
(6) Putting the pre-cured plate into a cement autoclave for autoclave curing;
(7) Drying the autoclaved plate at room temperature for 7-14 days to obtain the modified oyster shell antibacterial calcium silicate plate.
In the step (5), the mould pressing pressure of the press is 30-40MPa, the mould pressing time is 10-20min, and the pre-curing time is 8-12h.
In the step (6), the steam curing temperature is 160-200 ℃, the pressure is 0.5-1.9MPa, and the steam curing time is 8-12h.
The invention has the beneficial effects that:
the modified oyster shell antibacterial calcium silicate board prepared by the invention can be widely applied to suspended ceilings and partition walls of industrial and commercial engineering buildings, home decoration, liner plates of furniture, liner plates of billboards, shed plates of warehouses, network floors, wall plates of tunnels and other indoor engineering.
The modified oyster shell antibacterial calcium silicate board prepared by the technical scheme has the advantages that the modified waste oyster shells, diatomite, wood fibers and ordinary portland cement are used as main materials, the oyster shells can be recycled, and the problems of environmental pollution and resource shortage are relieved to a certain extent. Meanwhile, the raw material resources are rich, the price is low, and the prepared calcium silicate board has good performances of antibiosis, breaking strength and the like, and has good market application prospect.
The concrete expression is as follows:
(1) The invention is realized by a chemical deposition methodOyster shell is modified, and oyster shell powder subjected to antibacterial modification is used as a main raw material to prepare a calcium silicate board, so that the basic performance of the JC/T564.1-2018 fiber reinforced calcium silicate board is met, and the calcium silicate board has a good antibacterial effect. And the material modification method is simple and easy to implement, has stable properties and can be used for mass production. When 800g oyster shell powder is soaked in 1L Cu (NO) 3 ) 2 ·3H 2 The calcium silicate board prepared in the O (1 mol/L) modified solution shows good bacteriostatic effect on staphylococcus aureus and escherichia coli, and the antibacterial stability of the antibacterial modified calcium silicate board is further verified.
(2) The invention takes modified oyster shell and diatomite as main raw materials to prepare the calcium silicate board, tests on calcium-silicon ratio, forming pressure, curing temperature and curing time in the preparation process determine the preparation method of the calcium silicate board taking modified oyster shell and diatomite as main raw materials, and carries out range division on test conditions meeting the basic performance of JC/T564.1-2018 fiber reinforced calcium silicate board, when the calcium silicate board is prepared by the method in the embodiment 3, the flexural strength can reach 5.84MPa, and the conditions of fire resistance, wet rise rate and the like can also meet the national standard. In addition, the oyster shells which are wastes are accumulated for a long time, so that the living space of human beings is occupied, a large amount of bacteria and viruses are bred along with the increase of time, serious environmental pollution is caused, and serious harm is brought to the health of human bodies. By comprehensively utilizing the cement, the resource and environmental crisis caused by the large-scale use of the cement can be relieved, and the environmental problem caused by the accumulation of wastes can be relieved.
(3) The invention carries out antibacterial modification on the main raw materials for preparing the calcium silicate board, can effectively control the content of harmful microorganisms in buildings, and when the calcium silicate board is prepared by the method in the embodiment 3, 800g of oyster shell powder is soaked in 1L (1 mol/L) of Cu (NO) 3 ) 2 ·3H 2 After modification in O solution, the modification is prepared by using the O solution as a raw materialThe bacteriostasis rates of the sex oyster shell antibacterial calcium silicate board to escherichia coli and staphylococcus aureus can reach 93.14% and 100% respectively (the test results are shown in table 2). The antibacterial and anti-bending composite material has the advantages of bacteriostasis, good bending strength and the like, replaces the traditional building materials with high energy consumption, can be applied to building partitions, roof ceilings and the like, realizes indoor environment purification and building energy conservation, and has good market prospect.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The main component of the oyster shell powder in the invention is CaCO 3 80-95% by mass of oyster shell CaCO used in the following examples 3 The content was 91.82% (according to weight loss after calcination, according to CaCO 3 ＝CaO+CO 2 Calculated) is calculated), ca (OH) after hydrating it 2 The content is 85.46 percent of the total weight of the powder (obtained by testing by a method of 'GB T27815-2011 industrial milky calcium hydroxide', which is specifically shown in the specification);
CuO/Ca (OH) in the present invention 2 The mass ratio of the calcium hydroxide of the powder to the silicon dioxide in the diatomite is 0.83-1.2:1, ca (OH) in powder 2 The amount of the calcium hydroxide is calculated by the method of 'GB T27815-2011 industrial milky calcium hydroxide' on Ca (OH) in calcined hydrated oyster shell powder 2 And (5) testing the content. The specific method comprises the following steps:
about 1.5g of sample is quickly weighed in a weighing bottle to an accuracy of 0.0002g. The mixture was transferred to a 250mL Erlenmeyer flask with water, added to about 50mL and shaken to mix well. Adding 50mL of sucrose solution (30 g/L), stirring with a magnetic stirrer for 15min, adding 2-3 drops of phenolphthalein (10 g/L) indicator solution, mixing completely, and adding 4g/L of sodium hydroxide solution to obtain micropowder. Finally titrating to colorless by using a hydrochloric acid standard titration solution (0.5 mol/L) and keeping the color not to return for 30 s.
A blank test was also conducted, and the same operation as that for the measurement of the test solution and the same treatment as that for the sample were conducted except that no sample was added.
The content of calcium hydroxide is calculated by the mass fraction W of calcium hydroxide 1 Calculating according to the formula (1):
v- -number of volumes of standard titration solution of hydrochloric acid consumed to titrate the test solution in milliliters (mL);
V 0 -the value of the volume of hydrochloric acid standard titration solution consumed for titrating the blank test solution in milliliters (mL);
c-the exact value of the concentration of the hydrochloric acid standard titration solution, the unit is mol per liter (mol/L);
m- -number of sample masses in grams (g);
m- -calcium hydroxide [ Ca (OH) 2 ]The number of molar masses is in grams per mole (g/mol) alone (M = 37.05).
The diatomite mainly comprises SiO 2 The mass percentage range is 90-100%, siO in the diatomite used in the following examples 2 The proportion is 99 percent.
Example 1
A preparation method of a modified oyster shell antibacterial calcium silicate board comprises the following steps: grinding 800g of cleaned Concha Ostreae into fine powder, sieving with 2000 mesh sieve, soaking in 1L (0.2 mol/L) Cu (NO) 3 ) 2 ·3H 2 Stirring O solution for 12h, drying the solid obtained after filtration in an oven at 60 ℃ for 12h, transferring the solid into a muffle furnace at 950 ℃ for calcination for 5h, cooling the solid to room temperature, repeatedly calcining the solid in the muffle furnace at 950 ℃ for 5h to obtain CuO/CaO powder, soaking 160g of the calcined CuO/CaO powder in 200ml of water, and stirring the powder for 2h to obtain CuO/Ca (OH) 2 Powder is dried; 38 parts of calcined hydrated oyster shell powder CuO/Ca (OH) 2 (38 parts are Ca (OH) 2 The mass is calculated according to the following examples, 38 parts of diatomite powder, 4 parts of wood fiber and 20 parts of commonCharging Portland cement (P.O.42.5) and deionized water 30wt% of the powder, stirring, molding under 40MPa for 10min, pre-curing at room temperature for 12 hr, transferring into a cement autoclave, autoclaving at 180 deg.C for 10 hr, and air drying at ventilation position for 7 d.
Example 2
The other steps are the same as example 1 except that 800g of ground and sieved oyster shell powder is soaked in 1LCu (NO) 3 ) 2 ·3H 2 The concentration of the O solution is changed from 0.2mol/L to 0.6mol/L.
Example 3
The other steps are the same as example 1 except that 800g of 1LCu (NO) soaked by ground and sieved oyster shell powder 3 ) 2 ·3H 2 The concentration of the O solution is changed from 0.2mol/L to 1mol/L.
Example 4
The other steps are the same as example 1 except that 800g of ground and sieved oyster shell powder is soaked in 1L (0.2 mol/L) of Cu (NO) 3 ) 2 ·3H 2 The O solution was changed to Cu (NO) soaked in 5L (0.2 mol/L) 3 ) 2 ·3H 2 In O solution; changing 38 parts of calcined hydrated oyster shell powder and 38 parts of diatomite powder into 35 parts of calcined hydrated oyster shell powder and 41 parts of diatomite powder;
example 5
The other steps are the same as the example 1, except that 38 parts of oyster shell powder obtained by hydration after calcination and 38 parts of diatomite powder are changed into 42 parts of oyster shell powder obtained by hydration after calcination and 34 parts of diatomite powder;
example 6
The other steps are the same as the embodiment 1, except that the uniformly stirred slurry is subjected to compression molding under the pressure of 40MPa, and the compression molding is changed into the compression molding under the pressure of 30 MPa;
comparative example 1
The other steps are the same as the embodiment 1, except that the uniformly stirred slurry is subjected to compression molding under the pressure of 40MPa, and the compression molding is changed into the compression molding under the pressure of 50 MPa;
example 7
The other steps are the same as example 1 except that 800g of ground and sieved oyster shell powder is soaked in 1L (0.2 mol/L) of Cu (NO) 3 ) 2 ·3H 2 The O solution was changed to Cu (NO) soaked in 5L (0.2 mol/L) 3 ) 2 ·3H 2 In O solution; the autoclave curing in the cement autoclave at 180 ℃ is changed into the autoclave curing at 160 ℃;
example 8
The other steps are the same as the embodiment 1, except that the autoclave curing in the cement autoclave at 180 ℃ is changed into the autoclave curing in the cement autoclave at 200 ℃;
comparative example 2
The other steps are the same as the example 1, except that the autoclave curing in the cement autoclave at 180 ℃ is changed into the autoclave curing at 140 ℃;
example 9
The other steps are the same as the example 1, except that the autoclave curing time is changed from 10 hours to 8 hours;
example 10
The other steps are the same as the example 1, except that the autoclave curing time is changed from 10 hours in the cement autoclave to 12 hours in the cement autoclave;
comparative example 3
The other steps are the same as the example 1, except that the autoclave curing time is changed from 10 hours in the cement autoclave to 6 hours in the cement autoclave;
table 1 shows the results of the tests of the flexural strength, the fire resistance and the wet swell ratio of the examples and comparative examples,
| reference numerals | Flexural strength (MPa) | Fire resistance rating | Wet swelling Rate (%) |
| Test standard | JC/T564.1-2018 | GB8624-2012 | GB/T7019-2014 |
| Example 1 | 8.31 | A | 0.21 |
| Example 2 | 6.66 | A | 0.22 |
| Example 3 | 5.84 | A | 0.21 |
| Example 4 | 4.73 | A | 0.25 |
| Example 5 | 5.55 | A | 0.18 |
| Example 6 | 4.21 | A | 0.23 |
| Example 7 | 5.05 | A | 0.23 |
| Example 8 | 5.83 | A | 0.21 |
| Example 9 | 4.84 | A | 0.22 |
| Example 10 | 5.85 | A | 0.21 |
| Comparative example 1 | 3.69 | A | 0.20 |
| Comparative example 2 | 3.93 | A | 0.22 |
| Comparative example 3 | 3.89 | A | 0.23 |
As is clear from the test results, cu (NO) in the immersion liquid was added 3 ) 2 ·3H 2 The increase of the O content reduces the rupture strength along with the increase of the O content, and the change of the wet expansion rate is not obvious; with CuO/Ca (OH) 2 The increase in the mass ratio of calcium hydroxide to silica in diatomaceous earth (Ca/Si ratio) of the powder, the tendency of the flexural strength to increase first and then decrease, is probably attributable to Ca (OH) at a Ca/Si ratio of 1 2 And SiO 2 Most fully, the wet expansion rate follows SiO 2 The increase of the content shows a downward trend; the increase of the forming pressure causes the flexural strength to increase and then decrease, which is probably attributed to the fact that the porosity of the calcium silicate board decreases and the compactness increases with the increase of the pressure. The flexural strength is also increased. But the continuous increase of the density can cause the brittleness of the material to be enhanced, the breaking strength is worsened along with the material, when the forming pressure reaches 50MPa, the breaking strength does not meet the minimum standard of the breaking strength in JC/T564.1-2018 fiber reinforced calcium silicate boards any more, and meanwhile, the wet expansion rate shows a descending trend along with the increase of the forming pressure; the increase of the autoclave curing temperature causes the flexural strength to show a trend of changing stably after rising, and after the temperature reaches 160 ℃, the conditions of the flexural strength, the fireproof performance, the wet expansion rate and the like of the calcium silicate plate all meet the national standard. But after 180 ℃, the properties tend to be stable, probably due to the fact that the presence of too much tobermorite or even tobermorite intergrowths with better single crystallinity do not continue to have an influence on the flexural strength of the calcium silicate board; similarly, the performance of the calcium silicate board continuously autoclaved and cured after the curing time reaches 10 hours tends to be stable, and the wet expansion rate of the calcium silicate board is in a stable state. In addition, all examples and comparative examples of the experiment meet the fire resistance requirements described by JC/T564.1-2018 fiber reinforced calcium silicate boards.
Table 2 shows the immersion of Cu (NO) at different concentrations 3 ) 2 ·3H 2 The rate of inhibiting escherichia coli and staphylococcus aureus by the modified oyster shell antibacterial calcium silicate board of the O solution,
test results show that the modified oyster shell antibacterial calcium silicate board has obvious antibacterial effect on escherichia coli and staphylococcus aureus, the antibacterial effect of the calcium silicate board is improved along with the increase of the concentration of the soaking solution, and in example 3, when 800g of oyster shell powder is soaked in 1L (1 mol/L) Cu (NO) 3 ) 2 ·3H 2 After the modified oyster shell antibacterial calcium silicate board prepared from the raw material in the O solution is modified, the bacteriostasis rates of the modified oyster shell antibacterial calcium silicate board on escherichia coli and staphylococcus aureus can respectively reach 93.14% and 100% (the test results are shown in table 2).
The invention is not the best known technology.
Claims (5)
1. A preparation method of a modified oyster shell antibacterial calcium silicate board is characterized by comprising the following steps:
(1) Cleaning Concha Ostreae, oven drying, grinding into fine powder, soaking in Cu (NO) 3 ) 2 ·3H 2 Stirring in O solution for 2-12h, filtering, and oven drying to obtain Cu (NO) 3 ) 2 ·3H 2 O/CaCO 3 Powder;
wherein each 800g of oyster shell powder is soaked in 1-5L Cu (NO) 3 ) 2 ·3H 2 In O solution; cu (NO) 3 ) 2 ·3H 2 O solution with concentration of 0.2-1 mol/L, oyster shell and Cu (NO) 3 ) 2 ·3H 2 O/CaCO 3 Drying the powder in an oven at 60-80 deg.C for 6-12h;
(2) Drying the solid, placing the dried solid in a muffle furnace for calcination, calcining for 5-10h at 800-950 ℃, calcining for 1-3 times, and naturally cooling to room temperature to obtain CuO/CaO powder;
wherein 1-3420g Cu (NO) can be calcined in a muffle furnace volume of 27L 3 ) 2 ·3H 2 O/CaCO 3 Powder;
(3) Adding water into the solid for hydration, filtering, and oven drying the obtained solid in a vacuum oven at 60-80 deg.C for 8-12h to obtain CuO/Ca (OH) 2 Powder;
wherein, the hydration procedure of CuO/CaO is as follows: adding 18g to 100g of water into every 80g of calcined CuO/CaO powder and stirring for 2 to 5 hours;
(4) Mixing CuO/Ca (OH) 2 Mixing the powder with diatomite, adding fiber and ordinary portland cement to obtain mixed powder, adding water, and stirring to obtain slurry;
wherein the mass of the fiber is 0-5% of the mass of the mixed powder; the mass of the cement is 20-40% of the mass of the mixed powder; the mass of the water is 20-40% of the mass of the mixed powder; when the proportion of the substance is 0, the substance is not added, and the mixing and stirring of the slurry are carried out for 10-20min by adopting a pulverizer;
CuO/Ca(OH) 2 the mass ratio of the calcium hydroxide powder to the silicon dioxide in the diatomite is 0.83-1.2:1;
(5) Loading the mixed slurry into a stainless steel mold, performing compression molding on the stainless steel mold under a press machine, and performing pre-curing at room temperature;
(6) Putting the pre-cured plate into a cement autoclave for autoclave curing;
(7) Drying the autoclaved plate at room temperature for 7-14 days to obtain the modified oyster shell antibacterial calcium silicate plate.
2. The method for preparing a modified oyster shell antibacterial calcium silicate board according to claim 1, wherein the pulverizing fineness of oyster shell powder in step (1) is 100-3000 mesh.
3. The method for preparing a modified oyster shell antibacterial calcium silicate board according to claim 1, wherein the fiber in step (4) is wood fiber, and the cement is portland cement.
4. The method for preparing the modified oyster shell antibacterial calcium silicate board as claimed in claim 1, wherein in the step (5), the mold pressing pressure of a press is 30-40MPa, the mold pressing time is 10-20min, and the pre-curing time is 8-12h.
5. The method for preparing a modified oyster shell antibacterial calcium silicate board as claimed in claim 1, wherein in step (6), the steam curing temperature is 160-200 ℃, the pressure is 0.5-1.9MPa, and the steam curing time is 8-12h.
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| CN117361915A (en) * | 2023-08-16 | 2024-01-09 | 浙江大学 | Method for preparing hydrothermal curing body based on relative content of active calcium and active silicon |
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| KR20020039408A (en) * | 2000-11-21 | 2002-05-27 | 이승헌 | A filler manufacturing method for cement by using the shells of oysters and filler made thereby |
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