CN109020414B - Composite cement-based adsorption material and preparation method thereof - Google Patents
Composite cement-based adsorption material and preparation method thereof Download PDFInfo
- Publication number
- CN109020414B CN109020414B CN201811232151.4A CN201811232151A CN109020414B CN 109020414 B CN109020414 B CN 109020414B CN 201811232151 A CN201811232151 A CN 201811232151A CN 109020414 B CN109020414 B CN 109020414B
- Authority
- CN
- China
- Prior art keywords
- parts
- graphene oxide
- cement
- carboxylated graphene
- micro bubbles
- 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.)
- Active
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/02—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing hydraulic cements other than calcium sulfates
- C04B28/04—Portland cements
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
- B01J20/106—Perlite
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
- B01J20/205—Carbon nanostructures, e.g. nanotubes, nanohorns, nanocones, nanoballs
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
-
- 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
- C04B20/00—Use 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
- C04B20/02—Treatment
- C04B20/023—Chemical treatment
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/20—Heavy metals or heavy metal compounds
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/00017—Aspects relating to the protection of the environment
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/00474—Uses not provided for elsewhere in C04B2111/00
- C04B2111/00767—Uses not provided for elsewhere in C04B2111/00 for waste stabilisation purposes
- C04B2111/00784—Uses not provided for elsewhere in C04B2111/00 for waste stabilisation purposes for disposal only
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Analytical Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Inorganic Chemistry (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Nanotechnology (AREA)
- Crystallography & Structural Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- General Chemical & Material Sciences (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The invention discloses a composite cement-based adsorption material and a preparation method thereof, relating to the technical field of sewage treatment; the feed comprises the following raw materials in parts by weight: 200-240 parts of carboxylated graphene oxide, 30-60 parts of vitrified micro bubbles, 0.5-0.8 part of foaming agent, 3-5 parts of water reducing agent, 2-3 parts of air entraining agent, 600-650 parts of cement and 10-18 parts of sand; filling the vitrified micro bubbles with carboxylated graphene oxide through dispersion and suction, and then stirring, foaming, maintaining and drying to obtain a cement-based adsorbing material; the carboxylated graphene oxide cement-based composite material prepared by the invention can fully utilize the structural characteristics of the carboxylated graphene oxide and the vitrified micro bubbles after combination, has the high-quality performances of strong adsorption performance, good mechanical property, high strength, durability and good impermeability, can effectively adsorb metal ions in sewage, and can be widely applied to places in direct contact with industrial wastewater, such as sewage pipes, wastewater treatment pools and the like.
Description
Technical Field
The invention relates to the technical field of sewage treatment, in particular to a composite cement-based adsorption material for adsorbing metal ions in industrial sewage and a preparation method thereof.
Background
With the rapid development of the industrial field, environmental problems have become a major factor hindering economic development and social construction in our country, and water pollution is an important influencing factor of environmental problems. According to statistics, industrial sewage accounts for 70% of water resource pollution, and harmful toxic substances in the sewage have high metal ion concentration, so that the harm is large. In recent years, the country has relatively lagged behind the treatment of industrial sewage. Therefore, the treatment of industrial sewage is at present imminent.
At present, the common industrial sewage treatment methods include a physical chemical method, an advanced oxidation method and an electrochemical method. The physical and chemical method is widely adopted, and has the advantages of simple equipment, safe and convenient operation, convenient automatic control, mature process, low cost and the like. The physical method is mainly used for treating harmful substances in the wastewater, so that the aim of deep purification is fulfilled. However, there are also situations that are difficult to solve, for which simple physical processing methods cannot solve the problem. Therefore, the development of a metal ion adsorbing material with large adsorption capacity and high cost performance is always a hot point of research.
Disclosure of Invention
The invention overcomes the defects in the prior art, provides the light cement-based composite adsorption material with strong adsorption performance, good mechanical property, high strength, durability and good impermeability, and can be widely applied to places such as sewage pipes and wastewater treatment pools which are directly contacted with industrial wastewater. The invention is realized by the following technical scheme.
The composite cement-based adsorption material comprises the following raw materials in parts by weight: 200-240 parts of carboxylated graphene oxide, 30-60 parts of vitrified micro bubbles, 0.5-0.8 part of foaming agent, 3-5 parts of water reducing agent, 2-3 parts of air entraining agent, 600-650 parts of cement and 10-18 parts of sand.
The carboxylated graphene oxide is carboxylated by chloroacetic acid, so that epoxy groups and hydroxyl groups on the surface of the graphene oxide are partially substituted by carboxyl groups.
A preparation method of a composite cement-based adsorption material comprises the following steps:
a) preparing materials: 200-240 parts of carboxylated graphene oxide, 30-60 parts of vitrified micro bubbles, 0.5-0.8 part of foaming agent, 3-5 parts of water reducing agent, 2-3 parts of air entraining agent, 600-650 parts of cement, 10-18 parts of sand and 200-230 parts of water level are weighed accurately.
b) Dispersing: and adding the carboxylated graphene oxide into the water, and performing ultrasonic treatment to obtain a carboxylated graphene oxide dispersion liquid.
c) Suction: and (3) immersing the vitrified micro bubbles into the carboxylated graphene oxide dispersion liquid for 3-5 hours, stirring at a constant speed, taking out the vitrified micro bubbles, and performing steam curing in a steam curing chamber to obtain the steam cured vitrified micro bubbles.
d) Mixing: mixing and stirring the sand, the cement and the steam-cured vitrified micro bubbles, adding the air entraining agent for stirring, and then adding the water reducing agent for stirring to obtain the mixed fluid of the cement-based material.
e) Foaming: and mixing the foaming agent into the mixed fluid, stirring, pouring, forming and drying.
Further, the ultrasonic treatment of the step b) is 30-40 min.
Further, the vitrified micro bubbles are immersed into the carboxylated graphene oxide dispersion liquid for 3-5 hours, then the mixture is stirred at a constant speed, then the vitrified micro bubbles are taken out to be steamed and cured in a steam curing chamber, the vitrified micro bubbles are immersed into the carboxylated graphene oxide dispersion liquid again after the steam curing, and the steam curing vitrified micro bubbles are obtained after the steam curing.
Further, the uniform stirring time in the step c) is 30-50 s.
Further, the steam curing temperature in the step c) is 80-90 ℃, and the steam curing time is 2-3 h.
Further, heating the steam cured vitrified small balls for 1-2 hours at 150-180 ℃ to ensure that the cavities of the vitrified small balls are filled with carboxylated graphene oxide.
Further, the foaming is to mix a foaming agent into the mixed fluid, mix and stir for 120-150 seconds, stir at a high speed for 60-90 seconds, and pour and mold.
Further, in the step e), the cast material is placed into a standard curing chamber which is maintained at the room temperature of 18-22 ℃ and the humidity of more than or equal to 95%, curing is carried out for 25-30 days, and then the adsorbing material is dried at the normal temperature.
The carboxylated graphene oxide composite cement-based adsorption material with the strength of more than 1.2Mpa and the adsorption efficiency of more than or equal to 95 percent can be obtained.
On the basis of the above preparation method, preferred preparation conditions are: the carboxyl content of the carboxylated graphene oxide can reach 50% by adding 30% of chloroacetic acid, the thickness of a lamella is less than 1nm, and the length and the width of the lamella are less than 100nm, so that the solubility and the biological performance of the graphene oxide are improved.
The preferable density of the vitrified micro bubbles is 100kg/m3And vitrified micro bubbles with the granularity of 1mm, the water absorption rate of 30 percent and the cylinder pressure strength of 1 MPa.
The cement can adopt 42.5 common Portland cement, and the mechanical property of the formed cement-based material can be guaranteed.
The foaming agent is preferably sodium dodecyl benzene sulfonate foaming agent.
The water reducing agent is preferably a polycarboxylic acid water reducing agent, belongs to a high-efficiency water reducing agent and is powdery.
The air entraining agent is preferably a rosin resin air entraining agent.
The fineness of the sand is 2.5-2.8, the mud content is less than 1%, and the water content is less than 3%.
The vitrified micro bubbles adopted by the invention are irregular spherical particles, have small particle size and larger specific surface area, and can fully contact with sewage, thereby improving the adsorption rate. The interior of the glass fiber reinforced plastic composite material is of a cavity structure, the surface of the glass fiber reinforced plastic composite material is vitrified and sealed, the wave absorbing performance is good, and the water absorption rate is low.
The carboxylated graphene oxide belongs to a nano material, and has a monolithic layer structure with high specific surface area and unique chemical activity. The surface of the carboxylated graphene oxide contains oxygen-containing functional groups such as hydroxyl, epoxy, carboxyl and the like, the functional groups endow the carboxylated graphene oxide with excellent chemical activity and wettability, the surface of the carboxylated graphene oxide is negatively charged, nanoscale dispersion can be formed in water, the carboxylated graphene oxide has strong adsorption capacity, and metal ions in sewage can be sufficiently adsorbed.
The carboxylated graphene oxide composite cement-based material prepared by the invention mainly contains oxygen-containing functional groups such as hydroxyl, epoxy, carboxyl and the like on the surface of the carboxylated graphene oxide, and the functional groups endow the carboxylated graphene oxide with excellent chemical activity and wettability, and enable the surface of the carboxylated graphene oxide to be negatively charged, so that nanoscale dispersion can be formed in water, the carboxylated graphene oxide composite cement-based material has strong adsorption capacity, can sufficiently adsorb metal ions in sewage, has the metal ion removal rate of more than 98%, and has the characteristics of large adsorption capacity and high adsorption rate.
A large amount of carboxylated graphene oxide can be stored in the cavity inside the vitrified micro bubbles, so that the adsorption capacity of metal ions is maximized, and meanwhile, the microwave absorbing performance of the vitrified micro bubbles can weaken electromagnetic waves in sewage. The addition of the foaming agent can generate a plurality of micropores in the cement-based composite material, thereby increasing the adsorption capacity of the material. And the sodium dodecyl benzene sulfonate foaming agent belongs to a surfactant foaming agent, and surface ions are anions and can react with metal ions in sewage to achieve the effect of adsorbing the metal ions. The carboxylated graphene oxide has extremely excellent physical and chemical properties, so that the effect of desorption and desorption of metal ions is remarkable, the cyclic use can be realized, and the environment is protected.
Compared with the prior art, the invention has the beneficial effects that.
According to the invention, the vitrified microsphere foamed cement-based material is used as a basic support material of the carboxylated graphene oxide adsorption material, the porous characteristic of the material can improve the adsorption efficiency, and the material has the advantages of simple preparation, low cost and the like. The carboxylated graphene oxide cement-based composite material prepared by the method can fully utilize the characteristics of high specific surface area, unique chemical activity single-chip layer structure, hydroxyl, epoxy, carboxyl and other oxygen-containing functional groups on the surface and the like after the carboxylated graphene oxide and the vitrified micro bubbles are combined, realize the adsorption of metal ions in industrial sewage, and has the advantages of large adsorption capacity, high speed, easy preparation, mature process and easy regeneration.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects to be solved by the present invention more clearly apparent, the present invention is further described in detail with reference to the embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention. The technical solutions of the present invention are described in detail below with reference to examples, but the scope of protection is not limited thereto.
Example 1
The composite cement-based adsorption material is operated according to the following steps:
1) preparing materials: accurately weighing carboxylated graphene oxide, vitrified micro bubbles, a sodium dodecyl benzene sulfonate foaming agent, a polycarboxylic acid water reducing agent, a rosin air entraining agent, cement, sand and water according to the weight ratio of =210:40:0.6:3.5:2.5:630:16:220, and placing in a classified manner.
2) Dispersing: adding the carboxylated graphene oxide into water, and carrying out ultrasonic treatment for 30 minutes to obtain a carboxylated graphene oxide dispersion liquid.
3) Suction: and (2) immersing the vitrified microsphere into the carboxylated graphene oxide dispersion liquid for 3 hours, uniformly stirring for 50 seconds, performing steam curing in a steam curing chamber at 90 ℃ for 2 hours, immersing the vitrified microsphere subjected to steam curing in the carboxylated graphene oxide dispersion liquid for 3 hours for the second time, uniformly stirring for 60 seconds, performing steam curing in the steam curing chamber at 90 ℃ for 2 hours, and then treating the vitrified microsphere adsorbed with the carboxylated graphene oxide at 150 ℃ for 1 hour to ensure that the cavity of the vitrified microsphere is filled with the carboxylated graphene oxide.
4) Mixing: the sand, the cement and the treated vitrified micro bubbles are put into the mixer and stirred for 30 seconds, so that the cement fully wraps the sand, the weighed rosin air entraining agent is added into the mixer and stirred for 120 seconds, and then the polycarboxylic acid water reducing agent is added into the mixer and stirred for 90 seconds, so that the mixed fluid of the cement-based material is obtained.
5) Foaming: and (3) mixing the foaming agent into the mixed fluid of the stirred cement-based material, stirring for 150 seconds, scraping cement paste on the inner wall of the stirring pot, stirring at a high speed for 90 seconds, and pouring and forming.
6) And (5) maintenance: the cast test piece is placed into a standard curing room with the room temperature maintained at 20 ℃ and the humidity of 95 percent, and cured for 28 days under the condition.
7) And (3) drying: the test piece was dried at room temperature. The carboxylated graphene oxide composite cement-based adsorption material with the strength of 1.2MPa and the adsorption efficiency of 95% is obtained.
8) Placing the mixture in a closed container at room temperature to carry out Cu treatment2+The adsorption time of (2) was 28 days.
Example 2
The composite cement-based adsorption material is operated according to the following steps:
1) preparing materials: accurately weighing carboxylated graphene oxide, vitrified micro bubbles, a fatty alcohol-polyoxyethylene ether sodium sulfate foaming agent, a polycarboxylic acid water reducing agent, a saponin air entraining agent, cement, sand and water according to the weight ratio of =200:60:0.5:5:3:600:10:200, and placing in classification.
2) Dispersing: and adding the carboxylated graphene oxide into water, and carrying out ultrasonic treatment for 40 minutes to obtain a carboxylated graphene oxide dispersion liquid.
3) Suction: and (2) immersing the vitrified microsphere into the carboxylated graphene oxide dispersion liquid for 5 hours, uniformly stirring for 30 seconds, performing steam curing in a steam curing chamber at 80 ℃ for 3 hours, immersing the vitrified microsphere subjected to steam curing in the carboxylated graphene oxide dispersion liquid for 5 hours, uniformly stirring for 30 seconds, performing steam curing in a steam curing chamber at 90 ℃ for 2 hours, and then treating the vitrified microsphere adsorbed with the carboxylated graphene oxide at 180 ℃ for 1.5 hours to ensure that the cavity of the vitrified microsphere is filled with the carboxylated graphene oxide.
4) Mixing: the sand, the cement and the treated vitrified micro bubbles are firstly put into and stirred for 60 seconds, so that the cement fully wraps the sand, then the weighed saponin air entraining agent is added into the mixture and stirred for 90 seconds, and then the polycarboxylic acid water reducing agent is added into the mixture and stirred for 120 seconds, so that the mixed fluid of the cement-based material is obtained.
5) Foaming: and (3) mixing the foaming agent into the mixed fluid of the stirred cement-based material, stirring for 120 seconds, scraping cement paste on the inner wall of the stirring pot, stirring at a high speed for 60 seconds, and pouring and forming.
6) And (5) maintenance: the cast test piece is placed into a standard curing chamber which is maintained at the room temperature of 18 ℃ and the humidity of 98 percent, and is cured for 25 days under the condition.
7) And (3) drying: the test piece was dried at room temperature. The carboxylated graphene oxide composite cement-based adsorption material with the strength of 1.3MPa and the adsorption efficiency of 98% is obtained.
8) Placing the mixture in a closed container at room temperature to carry out Cr precipitation2+The adsorption time of (2) was 28 days.
Example 3
The composite cement-based adsorption material is operated according to the following steps:
1) preparing materials: accurately weighing carboxylated graphene oxide, vitrified micro bubbles, a sodium dodecyl sulfate foaming agent, a polycarboxylic acid water reducing agent, a rosin air entraining agent, cement, sand and water according to the weight ratio of =240:30:0.8:3:2:650:18:230, and placing in classification.
2) Dispersing: adding the carboxylated graphene oxide into water, and carrying out ultrasonic treatment for 35 minutes to obtain a carboxylated graphene oxide dispersion liquid.
3) Suction: and (2) immersing the vitrified microsphere into the carboxylated graphene oxide dispersion liquid for 4 hours, uniformly stirring for 40 seconds, performing steam curing in a steam curing chamber at 85 ℃ for 2.5 hours, immersing the vitrified microsphere subjected to steam curing in the carboxylated graphene oxide dispersion liquid for a second time for 4 hours, uniformly stirring for 30 seconds, performing steam curing in a steam curing chamber at 90 ℃ for 3 hours, and then treating the vitrified microsphere adsorbed with the carboxylated graphene oxide at 160 ℃ for 1.5 hours to ensure that the cavity of the vitrified microsphere is filled with the carboxylated graphene oxide.
4) Mixing: the sand, the cement and the treated vitrified micro bubbles are firstly put into and stirred for 50 seconds, so that the cement fully wraps the sand, then the weighed rosin air entraining agent is added into the mixture and stirred for 90 seconds, and then the polycarboxylic acid water reducing agent is added into the mixture and stirred for 100 seconds, so that the mixed fluid of the cement-based material is obtained.
5) Foaming: and (3) mixing the foaming agent into the mixed fluid of the stirred cement-based material, stirring for 130 seconds, scraping cement paste on the inner wall of the stirring pot, stirring at a high speed for 80 seconds, and pouring and forming.
6) And (5) maintenance: the cast test piece is placed into a standard curing chamber which is maintained at the room temperature of 22 ℃ and the humidity of 97 percent, and is cured for 28 days under the condition.
7) And (3) drying: the test piece was dried at room temperature. The obtained carboxylated graphene oxide composite cement-based adsorption material has the strength of 1.25MPa and the adsorption efficiency of 96%.
8) Putting the mixture in a closed container at room temperature to carry out Ni reaction2+The adsorption time of (2) was 28 days.
Example 4
The composite cement-based adsorption material is operated according to the following steps:
1) preparing materials: the carboxylated graphene oxide, the vitrified micro bubbles, the sodium dodecyl benzene sulfonate foaming agent, the polycarboxylic acid water reducing agent, the saponin air entraining agent, the cement, the sand and the water are accurately weighed according to the weight ratio of =230:50:0.5:4.5:3:640:17:230, and are placed in a classified manner.
2) Dispersing: adding the carboxylated graphene oxide into water, and carrying out ultrasonic treatment for 30 minutes to obtain a carboxylated graphene oxide dispersion liquid.
3) Suction: and (2) immersing the vitrified micro bubbles into the carboxylated graphene oxide dispersion liquid for 5 hours, uniformly stirring for 40 seconds, performing steam curing in a steam curing chamber at 90 ℃ for 2 hours, immersing the vitrified micro bubbles subjected to steam curing in the carboxylated graphene oxide dispersion liquid for 3 hours, uniformly stirring for 60 seconds, performing steam curing in the steam curing chamber at 90 ℃ for 2 hours, and then treating the vitrified micro bubbles adsorbed with the carboxylated graphene oxide at 150 ℃ for 2 hours to ensure that the cavities of the vitrified micro bubbles are filled with the carboxylated graphene oxide.
4) Mixing: the sand, the cement and the treated vitrified micro bubbles are firstly put into and stirred for 50 seconds, so that the cement fully wraps the sand, then the weighed saponin air entraining agent is added into the mixture and stirred for 110 seconds, and then the polycarboxylic acid water reducing agent is added into the mixture and stirred for 110 seconds, so as to obtain the mixed fluid of the cement-based material.
5) Foaming: and (3) mixing the foaming agent into the mixed fluid of the stirred cement-based material, stirring for 150 seconds, scraping cement paste on the inner wall of the stirring pot, stirring at a high speed for 90 seconds, and pouring and forming.
6) And (5) maintenance: the cast test piece is placed into a standard curing room with the room temperature maintained at 22 ℃ and the humidity of 95 percent, and cured for 28 days under the condition.
7) And (3) drying: the test piece was dried at room temperature. The obtained carboxylated graphene oxide composite cement-based adsorption material with the strength of 1.2MPa and the adsorption efficiency of 97 percent.
8) Placing the mixture in a closed container at room temperature for Pb precipitation2+The adsorption time of (2) was 28 days.
Test results
The metal ion concentrations in the above five examples were measured by ICP to calculate the removal rates, which are shown in Table 1.
TABLE 1 test results of removal rate of metal ions (%) -of cement-based materials
Test sample (carboxylated graphene oxide, vitrified micro bubbles and perlite cement-based material) to Cu2+、Cr2+、Ni2+、Pb2+The removal rates of the inorganic composite material are 93.52%, 96.25%, 88.39% and 93.69%, the adsorption effect is obvious, and the removal rates are respectively 22.67%, 28.59%, 19.23% and 26.72% higher than that of a blank sample (a cement-based material which does not participate in carboxylated graphene oxide, vitrified micro-beads and perlite).
While the invention has been described in further detail with reference to specific preferred embodiments thereof, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention as defined by the appended claims.
Claims (9)
1. The composite cement-based adsorption material is characterized by comprising the following raw materials in parts by weight: 200-240 parts of carboxylated graphene oxide, 30-60 parts of vitrified micro bubbles, 0.5-0.8 part of foaming agent, 3-5 parts of water reducing agent, 2-3 parts of air entraining agent, 600-650 parts of cement and 10-18 parts of sand; the preparation method of the composite cement-based adsorption material comprises the following steps:
a) preparing materials: weighing 200-240 parts of carboxylated graphene oxide, 30-60 parts of vitrified micro bubbles, 0.5-0.8 part of foaming agent, 3-5 parts of water reducing agent, 2-3 parts of air entraining agent, 600-650 parts of cement, 10-18 parts of sand and 200-230 parts of water level;
b) dispersing: adding the carboxylated graphene oxide into the water, and performing ultrasonic treatment to obtain a carboxylated graphene oxide dispersion liquid;
c) suction: immersing the vitrified micro bubbles into the carboxylated graphene oxide dispersion liquid for 3-5 hours, stirring at a constant speed, taking out the vitrified micro bubbles, and performing steam curing in a steam curing chamber to obtain steam cured vitrified micro bubbles;
d) mixing: mixing and stirring the sand, the cement and the steam-cured vitrified micro bubbles, adding the air entraining agent for stirring, and then adding the water reducing agent for stirring to obtain a mixed fluid of a cement-based material;
e) foaming: and mixing the foaming agent into the mixed fluid, stirring, pouring, forming and drying.
2. The composite cement-based adsorption material according to claim 1, wherein the carboxylated graphene oxide is carboxylated by chloroacetic acid, so that epoxy groups and hydroxyl groups on the surface of the graphene oxide are partially substituted by carboxyl groups.
3. The composite cement-based adsorption material according to claim 1, wherein the sonication in step b) is performed for 30-40 min.
4. The composite cement-based adsorption material according to claim 1, wherein the vitrified micro bubbles are immersed in the carboxylated graphene oxide dispersion liquid for 3-5 hours, then stirred at a constant speed, taken out and steamed in a steaming chamber, and after steaming, the vitrified micro bubbles are immersed in the carboxylated graphene oxide dispersion liquid again to repeat the steps, so that the steamed vitrified micro bubbles are obtained after steaming.
5. The composite cement-based adsorption material according to claim 1 or 4, wherein the uniform stirring time in step c) is 30-50 s.
6. The composite cement-based adsorption material according to claim 1 or 4, wherein the steam curing temperature in step c) is 80-90 ℃ and the steam curing time is 2-3 h.
7. The composite cement-based adsorption material according to claim 1 or 4, wherein the steam cured vitrified micro bubbles are heated at 150-180 ℃ for 1-2 h.
8. The composite cement-based adsorption material as claimed in claim 1, wherein the foaming is performed by mixing a foaming agent into the mixed fluid, mixing and stirring for 120-150 seconds, then stirring at high speed for 60-90 seconds, and casting.
9. The preparation method of the composite cement-based adsorption material according to claim 1, wherein in the step e), the cast material is placed in a standard curing chamber which is maintained at room temperature of 18-22 ℃ and humidity of more than or equal to 95%, curing is carried out for 25-30 days, and then the adsorption material is dried at normal temperature.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811232151.4A CN109020414B (en) | 2018-10-22 | 2018-10-22 | Composite cement-based adsorption material and preparation method thereof |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811232151.4A CN109020414B (en) | 2018-10-22 | 2018-10-22 | Composite cement-based adsorption material and preparation method thereof |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN109020414A CN109020414A (en) | 2018-12-18 |
| CN109020414B true CN109020414B (en) | 2021-03-26 |
Family
ID=64613651
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811232151.4A Active CN109020414B (en) | 2018-10-22 | 2018-10-22 | Composite cement-based adsorption material and preparation method thereof |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109020414B (en) |
Families Citing this family (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110559997A (en) * | 2019-09-29 | 2019-12-13 | 东莞理工学院城市学院 | Cement-based adsorbent and preparation method and application thereof |
| CN112430035B (en) * | 2020-11-25 | 2022-04-29 | 江南大学 | Graphene oxide-pervious concrete composite material and preparation method thereof |
| CN114230730A (en) * | 2021-12-28 | 2022-03-25 | 重庆建研科之杰新材料有限公司 | Concrete slump retaining agent and preparation method and application thereof |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2015040211A (en) * | 2013-08-20 | 2015-03-02 | 尾池工業株式会社 | Graphene dispersion composition, and carbon-containing resin laminated body |
| CN106000315A (en) * | 2016-07-20 | 2016-10-12 | 陕西科技大学 | Method for preparing light cement-based graphene oxide composite adsorption material |
-
2018
- 2018-10-22 CN CN201811232151.4A patent/CN109020414B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2015040211A (en) * | 2013-08-20 | 2015-03-02 | 尾池工業株式会社 | Graphene dispersion composition, and carbon-containing resin laminated body |
| CN106000315A (en) * | 2016-07-20 | 2016-10-12 | 陕西科技大学 | Method for preparing light cement-based graphene oxide composite adsorption material |
Non-Patent Citations (1)
| Title |
|---|
| 羧基化氧化石墨烯的制备及其电化学性能;王正玮等;《云南民族大学学报:自然科学版》;20130228;第22卷(第2期);第86-90页 * |
Also Published As
| Publication number | Publication date |
|---|---|
| CN109020414A (en) | 2018-12-18 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109020414B (en) | Composite cement-based adsorption material and preparation method thereof | |
| CN103833285B (en) | The preparation method of high-strength light photocatalytic cements base composite mortar and products thereof | |
| CN108484115B (en) | Porous material prepared by utilizing solid waste | |
| CN112125550B (en) | Method for reinforcing recycled aggregate of waste concrete through open carbonization | |
| CN105289469A (en) | Geopolymer based porous adsorption material and preparation method thereof | |
| CN110041035B (en) | C30 high-impermeability concrete with low consumption of rubber materials and preparation method thereof | |
| CN106830667B (en) | Modification method of hollow glass beads and application thereof | |
| CN115321885A (en) | Polymer modified cement-based repair mortar for marine concrete and preparation method thereof | |
| CN113426421B (en) | Foamed geopolymer adsorption material and preparation method and application thereof | |
| CN109574583B (en) | High-strength concrete and preparation method thereof | |
| CN113800856A (en) | Concrete drain pipe with good anti-permeability performance and production process thereof | |
| CN109928688A (en) | A kind of method and non-sintered brick preparing non-sintered brick using river bottom mud | |
| CN108264253B (en) | preparation method of pervious concrete with heavy metal ion removing capacity | |
| CN116239362A (en) | Light foam concrete baking-free ceramsite and preparation method thereof | |
| CN109354448B (en) | Method for preparing light foam concrete by using municipal solid waste incineration slag | |
| CN115448659B (en) | Solid waste stainless steel slag recycled concrete based on early carbonization and early dry-wet cycle coupling effect and preparation method thereof | |
| CN114507036B (en) | Inactivated and sterilized basalt fiber modified concrete with high corrosion resistance and preparation method thereof | |
| CN114394785A (en) | Method for improving antimicrobial corrosion resistance of concrete sewage pipeline | |
| CN108906054A (en) | A kind of forming method using Fenton iron cement preparation ozone oxidation nbsCOD catalyst | |
| CN113968688A (en) | Modification method of recycled concrete aggregate, concrete composition and application thereof | |
| CN112430037A (en) | Light environment-friendly concrete and preparation method thereof | |
| CN112321184A (en) | Preparation method of recycled aggregate for prefabricated building | |
| TWI445871B (en) | Light weight and thermal insulation composition aggregates and fabrication method thereof | |
| Gu et al. | Bio-inspired polydopamine modification of recycled carbon fibers for improving the performance of recycled carbon fiber reinforced mortars | |
| CN115784671B (en) | Method for preparing baking-free bricks from tailings in machine-made sand production process |
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 | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |