CN114656199A - Preparation method of high-strength and weather-resistant oyster shell geopolymer - Google Patents

Preparation method of high-strength and weather-resistant oyster shell geopolymer Download PDF

Info

Publication number
CN114656199A
CN114656199A CN202210308089.2A CN202210308089A CN114656199A CN 114656199 A CN114656199 A CN 114656199A CN 202210308089 A CN202210308089 A CN 202210308089A CN 114656199 A CN114656199 A CN 114656199A
Authority
CN
China
Prior art keywords
oyster shell
geopolymer
strength
weather
caustic soda
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
CN202210308089.2A
Other languages
Chinese (zh)
Inventor
华颖
卢金山
华峰
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Nanchang Hangkong University
Original Assignee
Nanchang Hangkong University
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Nanchang Hangkong University filed Critical Nanchang Hangkong University
Priority to CN202210308089.2A priority Critical patent/CN114656199A/en
Publication of CN114656199A publication Critical patent/CN114656199A/en
Withdrawn legal-status Critical Current

Links

Images

Classifications

    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B28/00Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
    • C04B28/006Compositions 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 mineral polymers, e.g. geopolymers of the Davidovits type
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B28WORKING CEMENT, CLAY, OR STONE
    • B28BSHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
    • B28B11/00Apparatus or processes for treating or working the shaped or preshaped articles
    • B28B11/24Apparatus or processes for treating or working the shaped or preshaped articles for curing, setting or hardening
    • B28B11/245Curing concrete articles
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B12/00Cements not provided for in groups C04B7/00 - C04B11/00
    • C04B12/005Geopolymer cements, e.g. reaction products of aluminosilicates with alkali metal hydroxides or silicates
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B14/00Use of inorganic materials as fillers, e.g. pigments, for mortars, concrete or artificial stone; Treatment of inorganic materials specially adapted to enhance their filling properties in mortars, concrete or artificial stone
    • C04B14/02Granular materials, e.g. microballoons
    • C04B14/26Carbonates
    • C04B14/28Carbonates of calcium
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B20/00Use of materials as fillers for mortars, concrete or artificial stone according to more than one of groups C04B14/00 - C04B18/00 and characterised by shape or grain distribution; Treatment of materials according to more than one of the groups C04B14/00 - C04B18/00 specially adapted to enhance their filling properties in mortars, concrete or artificial stone; Expanding or defibrillating materials
    • C04B20/02Treatment
    • C04B20/023Chemical treatment
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B7/00Hydraulic cements
    • C04B7/32Aluminous cements
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2111/00Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
    • C04B2111/00017Aspects relating to the protection of the environment
    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B2201/00Mortars, concrete or artificial stone characterised by specific physical values
    • C04B2201/50Mortars, concrete or artificial stone characterised by specific physical values for the mechanical strength

Landscapes

  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Ceramic Engineering (AREA)
  • Structural Engineering (AREA)
  • Organic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Environmental & Geological Engineering (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Geology (AREA)
  • Civil Engineering (AREA)
  • Inorganic Chemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Mechanical Engineering (AREA)
  • Curing Cements, Concrete, And Artificial Stone (AREA)

Abstract

The application relates to a preparation method of a high-strength and weather-resistant oyster shell geopolymer, which comprises the following steps: crushing oyster shells, and ball-milling into 80-mesh oyster shell powder; adding oyster shell powder into caustic soda aqueous solution, and placing the mixture into a reaction kettle for hydrothermal treatment; after hydrothermal treatment, adding granite powder slag, water glass solution and organosilane coupling agent into caustic soda aqueous solution of oyster shell powder, and mechanically mixing uniformly to obtain mixed slurry; pouring the mixed slurry into a mold, vibrating and degassing, placing the mold in a drying box for pressurized maintenance, and curing at room temperature after the maintenance is finished to obtain the oyster shell geopolymer. According to the invention, the geopolymer is prepared by taking oyster shells as raw materials, the porosity is reduced and the compressive strength is improved by improving the interfacial adhesion property of oyster shell particles and aluminosilicate gel, and the infiltration and diffusion of external water are prevented by hydrophobization of the pore surfaces, so that the efflorescence of the geopolymer is inhibited, and the engineering application property of the geopolymer is greatly improved.

Description

Preparation method of high-strength and weather-resistant oyster shell geopolymer
Technical Field
The application relates to the technical field of solid waste recycling, in particular to a preparation method of a high-strength and weather-resistant oyster shell geopolymer.
Background
The geopolymer is a three-dimensional network gel formed by polymerizing inorganic silicon-oxygen tetrahedron and aluminum-oxygen tetrahedron, and has a bonding structure of organic high polymer, so that the geopolymer has the characteristics of both the organic high polymer and portland cement. The geopolymer has the characteristics of high early strength and quick setting time; the compressive strength of the geopolymer is about 30 MPa even if the geopolymer is subjected to heat treatment at 400-800 ℃ for 1 h, and the geopolymer can be used as a refractory material. The research and application development prospect of geopolymers of Sun Daoduo, Wang Patrio and Hupu states that the compressive strength of geopolymers prepared by alkali-activated metakaolin at 25 ℃ for 4 hours can reach 87.5 MPa, and the strength in 7 days can reach 137.6 MPa. Mixing slag with building waste residue or laterite in a certain proportion as a raw material, mixing the raw material with NaOH and sodium silicate solution, curing at 80 ℃ for 24 hours, and curing at room temperature for 7 days to prepare the slag-based geopolymer. The invention patent CN201911285672.0 discloses a geopolymer-based concrete of coal mine wastes and a preparation method thereof, wherein an alkaline dry powder excitant is selected, only powder with the grain diameter less than 0.03 mm is used when the alkaline dry powder excitant is prepared, and the production rate is lower and the energy consumption is high.
Caustic soda is generally used as an alkali activator in the preparation of geopolymers, and aluminosilicate solid waste residues are dissolved by the caustic soda in the curing process and gradually dehydrated to form a glass phase with higher bonding strength. In the practical engineering application process, external water and carbon dioxide gas penetrate through the gas pore passage, permeate into the geopolymer, react with residual caustic soda to generate sodium carbonate, and severe efflorescence of efflorescence occurs, so that the mechanical strength of the geopolymer is greatly reduced, and the engineering application of the geopolymer is severely restricted.
A large amount of oysters are cultured in coastal areas of China, the oysters are main marine cultured aquatic products, and the yield of the oysters in China reaches 523 ten thousand tons in 2019. More than 60% of oysters are inedible oyster shells, so that a large amount of oyster shells are accumulated near a coastline, precious land resources are occupied, and the environmental sanitation and the ecological system around a storage yard are influenced. Oyster shell contains more than 90% of calcium carbonate with calcite structure and organic matter components such as polysaccharide, glycoprotein and pearl protein, and only a small amount of oyster shell is used for soil improvement, food additives and medicines at present, and most oyster shell is not effectively utilized. Oyster shell is used as a raw material, a certain amount of aluminosilicate waste residue is added, and alkali is adopted to activate geological polymerization reaction, so that the oyster shell geopolymer can be prepared. The method not only solves the problem of shell resource utilization and protects the ecological environment, but also is expected to be widely applied to building dams, ditches and sidewalks as the geopolymer is a green environment-friendly building material, thereby generating good economic and social benefits.
However, hydrophobic organic matters in the oyster shells seriously interfere with geological polymerization reaction, so that the interfacial adhesion performance between oyster shell powder particles and aluminosilicate gel generated by the geological polymerization reaction is reduced; the porosity of the geopolymer is obviously increased by the bubbles generated by the hydrolysis of organic matters in the process of geopolymerization reaction, the compressive strength of the geopolymer is reduced, and the efflorescence of the geopolymer is accelerated by the high porosity caused by the bubbles, so that the engineering application value of the oyster shell geopolymer is reduced.
Disclosure of Invention
The invention aims to provide a preparation method of a high-strength and weather-resistant oyster shell geopolymer. Oyster shell is used as a main raw material, granite powder slag is added to serve as an aluminosilicate raw material, an organosilane coupling agent serves as a pore surface hydrophobing agent, alkali-activated geological polymerization reaction is adopted, the granite powder slag is converted into aluminosilicate gel, and oyster shell powder particles are bonded through the aluminosilicate gel, so that the oyster shell geopolymer is prepared. By improving the interfacial adhesion property of the oyster shell powder particles and the aluminosilicate gel, the porosity of the oyster shell geopolymer is reduced, the compressive strength is improved, and by hydrophobization of the pores, permeation and diffusion of external water are prevented, the efflorescence of the geopolymer is inhibited, the engineering application property of the geopolymer is greatly improved, and the engineering application of the oyster shell waste residues in the field of green building materials is promoted.
The technical scheme adopted by the invention is as follows: a preparation method of a high-strength and weather-resistant oyster shell geopolymer comprises the following steps:
step S1: crushing oyster shells, and ball-milling into 80-mesh oyster shell powder;
step S2: adding the oyster shell powder obtained in the step S1 into a caustic soda aqueous solution, and placing the mixture into a reaction kettle for hydrothermal treatment, wherein the weight ratio of the oyster shell powder to the caustic soda aqueous solution is 3: 1-4: 1;
step S3: after hydrothermal treatment, adding granite powder slag, water glass solution and organosilane coupling agent into caustic soda aqueous solution of oyster shell powder, and mechanically mixing uniformly to obtain mixed slurry;
step S4: and (5) pouring the mixed slurry obtained in the step (S3) into a mould for vibration degassing, placing the mould into a drying box for pressurized maintenance, and curing at room temperature for 28 days after the maintenance is finished to obtain the oyster shell geopolymer.
Further, the concentration of the caustic soda aqueous solution in the step S2 is 8-10 mol/L.
Further, the hydrothermal treatment temperature in step S2 is 110-150 ℃, and the hydrothermal treatment time is 10-30 min.
Further, in the step S3, the mass ratio of the oyster shell powder to the granite powder slag is 3: 1-5: 1.
Further, SiO in the water glass solution in step S32And Na2The molar ratio of O is 1: 1-2.5: 1; the mass ratio of the water glass solution to the caustic soda aqueous solution is 1: 1-3: 1.
Further, in step S3, the organic silane coupling agent is n-octyltriethoxysilane, and the addition amount of the organic silane coupling agent is 2% by mass of the granite powder slag.
Further, in the step S4, the curing pressure is 0.2-0.5 MPa, the curing temperature is 80-100 ℃, and the curing time is 10-24 hours.
The invention has the beneficial effects that:
(1) by adopting an oyster shell powder hydrothermal treatment technology, when hydrothermal treatment is carried out in a caustic soda aqueous solution, hydrophobic organic matters in oyster shells are hydrolyzed and removed under the alkali catalysis, so that the interfacial adhesion property of oyster shell powder particles and aluminosilicate gel is remarkably improved, and the compressive strength of a geopolymer is improved;
(2) the pressurized curing method is adopted for curing, compared with the normal-pressure curing, the aluminosilicate gel slides in the pressurized curing process, the pore space is filled, the large pores in the mixed slurry are eliminated, the porosity is obviously reduced, and the compactness of the oyster shell geopolymer is improved, so that the compressive strength of the oyster shell geopolymer is improved;
(3) in the preparation process, an organosilane coupling agent is added, and under the action of alkali catalysis, the silane coupling agent is hydrolyzed to generate hydrophobic alkyl groups which are distributed on the surfaces of air holes to form hydrophobic pores. The low porosity and the hydrophobic pores formed by pressurized curing effectively prevent the permeation and diffusion of external water, thereby inhibiting the efflorescence of the oyster shell geopolymer;
(4) the invention takes oyster shell as main raw material, adopts oyster shell hydrothermal treatment technology, pressurized maintenance technology and air pore hydrophobic modification technology of organosilane coupling agent to prepare high-strength and weather-resistant oyster shell geopolymer; the oyster shell geopolymer is used as a green environment-friendly building material, can replace high-energy-consumption cement concrete, saves a large amount of energy, greatly reduces greenhouse gas emission in the building material industry, and has wide market application prospect.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present application, and it is obvious for those skilled in the art that other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a flow chart of a preparation method of examples 1 to 3 of the present invention;
FIG. 2 shows FESEM appearance of oyster shell geopolymer prepared in example 1 of the present invention;
FIG. 3 shows FESEM appearance of oyster shell geopolymer prepared in example 2 of the present invention;
FIG. 4 shows FESEM appearance of oyster shell geopolymer prepared in example 3 of the present invention.
Detailed Description
In order that the above objects, features and advantages of the present invention can be more clearly understood, a more particular description of the invention will be rendered by reference to the appended drawings. In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention, however, the present invention may be practiced in other ways than those specifically described herein, and thus the present invention is not limited to the specific embodiments disclosed below.
Unless defined otherwise, technical or scientific terms used herein shall have the ordinary meaning as understood by one of ordinary skill in the art to which this application pertains. The use of "first," "second," and similar terms in the description and claims of this patent application do not denote any order, quantity, or importance, but rather the terms are used to distinguish one element from another. Also, the use of the terms "a" or "an" and the like do not denote a limitation of quantity, but rather denote the presence of at least one.
As shown in figure 1, the preparation method of the high-strength and weather-resistant oyster shell geopolymer comprises the following steps:
step S1: crushing oyster shells, and ball-milling into 80-mesh oyster shell powder;
step S2: adding the oyster shell powder obtained in the step S1 into caustic soda aqueous solution, and placing the oyster shell powder into a reaction kettle for hydrothermal treatment to reduce protein on the surface of powder particles; wherein the weight ratio of the oyster shell powder to the caustic soda aqueous solution is 3: 1-4: 1, the concentration of the caustic soda aqueous solution is 8-10 mol/L, the hydrothermal treatment temperature is 110-150 ℃, and the hydrothermal treatment time is 10-30 min;
step S3: after hydrothermal treatment, adding granite powder slag, water glass solution and organosilane coupling agent into caustic soda aqueous solution of oyster shell powder, and mechanically mixing uniformly to obtain mixed slurry; wherein the weight ratio of oyster shell powder to granite powder slag is 3: 1-5: 1, and SiO in the water glass solution2And Na2The molar ratio of O is 1: 1-2.5: 1; the mass ratio of the water glass solution to the caustic soda aqueous solution is 1: 1-3: 1, and the organosilane coupling agent isThe addition amount of the n-octyl triethoxysilane and the organosilane coupling agent is 2 percent of the mass of the granite powder slag;
step S4: pouring the mixed slurry obtained in the step S3 into a mold, vibrating and degassing, and placing the mold into a drying box for pressurized curing, wherein the curing pressure is 0.2-0.5 MPa, the curing temperature is 80-100 ℃, and the curing time is 10-24 hours; curing for 28 days at room temperature after curing to obtain the oyster shell geopolymer.
Example 1
Crushing and ball-milling oyster shells, sieving the crushed and ball-milled oyster shells with a 80-mesh sieve, adding oyster shell powder into 8 mol/L aqueous caustic soda solution, wherein the mass ratio of the oyster shell powder to the aqueous caustic soda solution is 4:1, placing the oyster shell powder and the aqueous caustic soda solution into a reaction kettle for hydrothermal treatment, wherein the hydrothermal treatment temperature is 110 ℃, and the hydrothermal treatment time is 10 min; then adding granite powder slag, water glass solution and organic silane coupling agent, wherein the mass ratio of the oyster shell powder to the granite powder slag is 4:1, and SiO is contained in the water glass solution2And Na2The molar ratio of O is 1:1, the mass ratio of the water glass solution to the caustic soda aqueous solution is 1:1, the organosilane coupling agent is n-octyl triethoxysilane, and the addition amount of the organosilane coupling agent is 2 percent of the mass of the granite powder slag; and (3) injecting the slurry into a mold after uniform mixing, placing the mold in a drying oven for pressurized curing, wherein the curing pressure is 0.2 MPa, the curing temperature is 80 ℃, the curing time is 10 h, and curing is carried out for 28 days at room temperature after curing is finished to obtain the oyster shell geopolymer.
The microscopic morphology of the oyster shell geopolymer prepared in example 1 was observed by using a field emission scanning electron microscope (hereinafter abbreviated as FESEM). As shown in fig. 2, the geopolymer has relatively large pores inside, with an average pore size of about 6.6
Figure DEST_PATH_IMAGE002A
m, the compressive strength of the oyster shell geopolymer prepared in example 1 is 49.7 MPa through the test of a ceramic bending tester.
The oyster shell geopolymer prepared in example 1 is placed in a 150mL distilled water beaker, the preservative film is covered and then placed in a drying oven for weathering experiments, the weathering temperature is 50 ℃, the weathering time is 48h, the weathered oyster shell geopolymer is dried, the weight loss rate is 12.3%, and the compressive strength of the oyster shell geopolymer is 26.5 MPa as tested by a ceramic bending tester.
Example 2
Crushing and ball-milling oyster shells, sieving the crushed and ball-milled oyster shells with a 80-mesh sieve, adding oyster shell powder into 9 mol/L aqueous caustic soda solution, wherein the mass ratio of the oyster shell powder to the aqueous caustic soda solution is 3.5:1, placing the oyster shell powder and the aqueous caustic soda solution into a reaction kettle for hydrothermal treatment, wherein the hydrothermal treatment temperature is 130 ℃, and the hydrothermal treatment time is 20 min; then adding granite powder slag, a water glass solution and an organic silane coupling agent, wherein the mass ratio of the oyster shell powder to the granite powder slag is 4:1, and SiO is contained in the water glass solution2And Na2The O molar ratio is 1.5:1, the mass ratio of the water glass solution to the caustic soda aqueous solution is 2:1, the organosilane coupling agent is n-octyl triethoxysilane, and the addition amount of the organosilane coupling agent is 2% of the mass of the granite powder slag; and (3) injecting the slurry into a mold after uniform mixing, placing the mold in a drying oven for pressurized curing, wherein the curing pressure is 0.2 MPa, the curing temperature is 90 ℃, the curing time is 24h, and curing is carried out for 28 days at room temperature after curing is finished to obtain the oyster shell geopolymer.
The microscopic morphology of the oyster shell geopolymer prepared in example 2 was observed by FESEM. As shown in FIG. 3, the geopolymer had a significant reduction in internal porosity with an average pore size of about 4.2
Figure DEST_PATH_IMAGE002AA
m, the compressive strength of the oyster shell geopolymer prepared in example 2 was measured to be 76.8 MPa by a ceramic bending tester.
The oyster shell geopolymer prepared in example 2 is placed in a 150mL distilled water beaker, the preservative film is covered and then placed in a drying oven for weathering experiments, the weathering temperature is 50 ℃, the weathering time is 48h, the weathered oyster shell geopolymer is dried, the weight loss rate is 8.4%, and the compressive strength of the oyster shell geopolymer is 61.7 MPa as tested by a ceramic bending tester.
Example 3
Crushing and ball-milling oyster shells, sieving the crushed oyster shells with a 80-mesh sieve, adding oyster shell powder into 10 mol/L caustic soda aqueous solution,the weight ratio of oyster shell powder to caustic soda aqueous solution is 3:1, and the oyster shell powder and the caustic soda aqueous solution are placed in a reaction kettle for hydrothermal treatment, wherein the hydrothermal treatment temperature is 150 ℃, and the hydrothermal treatment time is 30 min; then adding granite powder slag, water glass solution and organic silane coupling agent, wherein the mass ratio of the oyster shell powder to the granite powder slag is 4:1, and SiO is contained in the water glass solution2And Na2The O molar ratio is 2.5:1, the mass ratio of the water glass solution to the caustic soda aqueous solution is 3:1, the organosilane coupling agent is n-octyl triethoxysilane, and the addition amount of the organosilane coupling agent is 2 percent of the mass of the granite powder slag; and injecting the slurry into a mold after uniform mixing, placing the mold in a drying box for pressurized curing, wherein the curing pressure is 0.5 MPa, the curing temperature is 95 ℃, the curing time is 24h, and curing is carried out at room temperature for 28 days after the curing is finished, so as to obtain the oyster shell geopolymer.
The microscopic morphology of the oyster shell geopolymer prepared in example 3 was observed using FESEM. As shown in fig. 4, the geopolymer internal porosity was further reduced with an average pore size of about 2.8
Figure DEST_PATH_IMAGE002AAA
m, the compressive strength of the oyster shell geopolymer prepared in example 3 was measured to be 95.3 MPa by a ceramic bending tester.
The oyster shell geopolymer prepared in example 3 is placed in a 150mL distilled water beaker, the preservative film is covered and then placed in a drying oven for weathering experiments, the weathering temperature is 50 ℃, the weathering time is 48h, the weathered oyster shell geopolymer is dried, the weight loss rate is 3.5%, and the compressive strength of the oyster shell geopolymer tested by a ceramic bending tester is 90.8 MPa.
According to the embodiment of the invention, on the basis of a conventional geopolymer preparation technology, oyster shells are taken as main raw materials, granite powder slag, a water glass solution and an organosilane coupling agent serving as a pore surface hydrophobizing agent are added after hydrothermal treatment of an aqueous solution of caustic soda, and the prepared oyster shell geopolymer has good interfacial adhesion property, low porosity and hydrophobic pores by adopting a pressurized maintenance mode, so that the high-strength and weather-resistant oyster shell geopolymer is obtained. From examples 1 to 3, it is clear that the oyster shell geopolymer prepared by adding the silane coupling agent and pressure curing has higher compressive strength and better weathering resistance. The invention not only effectively utilizes oyster shell, but also the prepared oyster shell geopolymer has higher strength, the phenomenon of saltpetering in the use process is obviously improved, the invention is suitable for the production of green environment-friendly building materials, can replace high-energy-consumption cement concrete, saves a large amount of energy, greatly reduces the emission of greenhouse gas in the building material industry, and has wide market application prospect.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (7)

1. A preparation method of a high-strength and weather-resistant oyster shell geopolymer is characterized by comprising the following steps:
step S1: crushing oyster shells, and ball-milling into 80-mesh oyster shell powder;
step S2: adding the oyster shell powder obtained in the step S1 into a caustic soda aqueous solution, and placing the mixture into a reaction kettle for hydrothermal treatment, wherein the weight ratio of the oyster shell powder to the caustic soda aqueous solution is 3: 1-4: 1;
step S3: after hydrothermal treatment, adding granite powder slag, water glass solution and organosilane coupling agent into caustic soda aqueous solution of oyster shell powder, and mechanically mixing uniformly to obtain mixed slurry;
step S4: and (5) pouring the mixed slurry obtained in the step (S3) into a mould, vibrating and degassing, putting into a drying oven for pressurized maintenance, and curing at room temperature for 28 days after the maintenance is finished to obtain the oyster shell geopolymer.
2. The preparation method of the high-strength and weather-resistant oyster shell geopolymer according to claim 1, wherein the concentration of the caustic soda aqueous solution in step S2 is 8-10 mol/L.
3. The preparation method of the high-strength and weather-resistant oyster shell geopolymer according to claim 2, wherein the hydrothermal treatment temperature in step S2 is 110-150 ℃, and the hydrothermal treatment time is 10-30 min.
4. The preparation method of the high-strength and weather-resistant oyster shell geopolymer as claimed in claim 1, wherein the weight ratio of oyster shell powder to granite powder slag in step S3 is 3: 1-5: 1.
5. The method for preparing high-strength and weather-resistant oyster shell geopolymer according to claim 4, wherein in step S3, SiO in water glass solution2And Na2The molar ratio of O is 1: 1-2.5: 1; the mass ratio of the water glass solution to the caustic soda aqueous solution is 1: 1-3: 1.
6. The preparation method of the high-strength and weather-resistant oyster shell geopolymer as claimed in claim 5, wherein the organosilane coupling agent in step S3 is n-octyltriethoxysilane, and the addition amount of the organosilane coupling agent is 2% of the granite powder slag.
7. The preparation method of the high-strength and weather-resistant oyster shell geopolymer as claimed in claim 1, wherein in step S4, the curing pressure is 0.2-0.5 MPa, the curing temperature is 80-100 ℃, and the curing time is 10-24 h.
CN202210308089.2A 2022-03-26 2022-03-26 Preparation method of high-strength and weather-resistant oyster shell geopolymer Withdrawn CN114656199A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN202210308089.2A CN114656199A (en) 2022-03-26 2022-03-26 Preparation method of high-strength and weather-resistant oyster shell geopolymer

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN202210308089.2A CN114656199A (en) 2022-03-26 2022-03-26 Preparation method of high-strength and weather-resistant oyster shell geopolymer

Publications (1)

Publication Number Publication Date
CN114656199A true CN114656199A (en) 2022-06-24

Family

ID=82034071

Family Applications (1)

Application Number Title Priority Date Filing Date
CN202210308089.2A Withdrawn CN114656199A (en) 2022-03-26 2022-03-26 Preparation method of high-strength and weather-resistant oyster shell geopolymer

Country Status (1)

Country Link
CN (1) CN114656199A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115925336A (en) * 2022-11-25 2023-04-07 河北工业大学 Efflorescence-resistant high-content steel slag geopolymer mortar and preparation method thereof

Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103086414A (en) * 2013-01-31 2013-05-08 南昌航空大学 Method for preparing high-purity calcite calcium carbonate micropowder through shell hydro-thermal treatment
CN105683331A (en) * 2013-10-30 2016-06-15 贝克休斯公司 Proppants with improved strength
US20190203099A1 (en) * 2018-01-02 2019-07-04 Saudi Arabian Oil Company Composition of encapsulated chemical additives and methods for preparation of the same
CN111592287A (en) * 2020-05-21 2020-08-28 南昌航空大学 Preparation method of calcium carbonate type waste residue geopolymer
CN112079593A (en) * 2020-07-30 2020-12-15 浙江大学 Siloxane modified super-hydrophobic geopolymer anticorrosive material and preparation method thereof
CN112079585A (en) * 2020-07-30 2020-12-15 浙江大学 Super-hydrophobic geopolymer prepared by microcellular foaming and preparation method thereof
CN112390576A (en) * 2020-11-11 2021-02-23 武汉工程大学 Potassium titanate whisker modified high-strength high-hydrophobicity porous geopolymer thermal insulation material and preparation method and application thereof
CN113480242A (en) * 2021-06-30 2021-10-08 深圳信息职业技术学院 Geopolymer water permeable brick and preparation method and application thereof

Patent Citations (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103086414A (en) * 2013-01-31 2013-05-08 南昌航空大学 Method for preparing high-purity calcite calcium carbonate micropowder through shell hydro-thermal treatment
CN105683331A (en) * 2013-10-30 2016-06-15 贝克休斯公司 Proppants with improved strength
US20190203099A1 (en) * 2018-01-02 2019-07-04 Saudi Arabian Oil Company Composition of encapsulated chemical additives and methods for preparation of the same
CN111592287A (en) * 2020-05-21 2020-08-28 南昌航空大学 Preparation method of calcium carbonate type waste residue geopolymer
CN112079593A (en) * 2020-07-30 2020-12-15 浙江大学 Siloxane modified super-hydrophobic geopolymer anticorrosive material and preparation method thereof
CN112079585A (en) * 2020-07-30 2020-12-15 浙江大学 Super-hydrophobic geopolymer prepared by microcellular foaming and preparation method thereof
CN112390576A (en) * 2020-11-11 2021-02-23 武汉工程大学 Potassium titanate whisker modified high-strength high-hydrophobicity porous geopolymer thermal insulation material and preparation method and application thereof
CN113480242A (en) * 2021-06-30 2021-10-08 深圳信息职业技术学院 Geopolymer water permeable brick and preparation method and application thereof

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115925336A (en) * 2022-11-25 2023-04-07 河北工业大学 Efflorescence-resistant high-content steel slag geopolymer mortar and preparation method thereof

Similar Documents

Publication Publication Date Title
CN114436601B (en) Recycled aggregate self-compacting concrete and preparation method thereof
CN111978056A (en) Modified material of low-quality aggregate and treatment method
CN107337414B (en) Carbonized baking-free brick prepared from marine waste sludge and preparation method thereof
CN107814530B (en) High-strength recycled concrete porous brick
CN113429141B (en) Cementing material and preparation method and application thereof
CN112079593B (en) Siloxane modified super-hydrophobic geopolymer anticorrosive material and preparation method thereof
CN111170698B (en) Regenerated glass fiber reinforced plastic anti-crack thermal insulation mortar and preparation and construction methods thereof
CN107244859A (en) A kind of civil engineering heat insulating type concrete and preparation method thereof
CN110922134A (en) Cement-based capillary crystalline waterproof coating and preparation method thereof
CN112010602A (en) High-strength recycled aggregate concrete and preparation method thereof
CN106927735B (en) Fly ash based geopolymer rice hull thermal insulation mortar and method for constructing building exterior wall thermal insulation mortar layer
CN109942235A (en) Room temperature conserves ground polymers concrete of high-strength high anti-carbonation properties and preparation method thereof
CN108558324A (en) A kind of impervious regeneration concrete
CN109734369A (en) A kind of foam air-entrained concrete building block and preparation method thereof prepared using iron tailings as raw material normal temperature and pressure
CN112573884A (en) High-toughness alkali slag granite powder aerated concrete block and preparation method thereof
CN114656199A (en) Preparation method of high-strength and weather-resistant oyster shell geopolymer
CN112723807B (en) Seawater-mixed underwater undispersed concrete and preparation method thereof
CN111333392A (en) Seawater mixed culture coral reef sand C120UHPC and preparation method thereof
CN112851166A (en) Method for preparing high-strength baking-free ceramsite by adopting mine stripping soil
CN107417292B (en) Preparation method of lime-sand brick
KR101218654B1 (en) Geopolymer Composition and manufacturing method thereof
CN114956698A (en) Preparation method of novel carbonized and regenerated pressed brick
CN110606767B (en) Lightweight aggregate concrete and preparation process thereof
CN114956707A (en) Concrete for frame structure house and preparation method thereof
CN107555930B (en) High-strength water-blocking aerated concrete building block and preparation method thereof

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
WW01 Invention patent application withdrawn after publication
WW01 Invention patent application withdrawn after publication

Application publication date: 20220624