CN114853433B - Fluorine gypsum composite cementing material and preparation method thereof - Google Patents
Fluorine gypsum composite cementing material and preparation method thereof Download PDFInfo
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- CN114853433B CN114853433B CN202210385645.6A CN202210385645A CN114853433B CN 114853433 B CN114853433 B CN 114853433B CN 202210385645 A CN202210385645 A CN 202210385645A CN 114853433 B CN114853433 B CN 114853433B
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- 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
- C04B28/14—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 calcium sulfate cements
- C04B28/142—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 calcium sulfate cements containing synthetic or waste calcium sulfate cements
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- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/50—Mortars, concrete or artificial stone characterised by specific physical values for the mechanical strength
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/91—Use of waste materials as fillers for mortars or concrete
Abstract
The invention discloses a fluorogypsum composite cementing material and a preparation method thereof, wherein the fluorogypsum composite cementing material comprises the following components: 65-74% of fluorgypsum, 14-21% of slag powder, 5-12% of ordinary Portland cement, 1-3% of alkaline material, 0.5-1.8% of active excitant, 0.2-2% of redispersible latex powder and 0.1-1% of water-retaining thickener. According to the fluorine gypsum composite cementing material and the preparation method thereof, the fluorine gypsum is modified by adopting a proper additive and a certain process condition, so that the cementing performance of the fluorine gypsum composite cementing material is effectively improved, the mechanical strength of the fluorine gypsum composite cementing material is enhanced, and a new way for comprehensively utilizing the fluorine gypsum is widened.
Description
Technical Field
The invention belongs to the technical field of building materials, and particularly relates to a fluorine gypsum composite cementing material and a preparation method thereof.
Background
The fluorogypsum is a byproduct of the hydrofluoric acid production process, and 3.6 tons of anhydrous fluorogypsum are generated from industrial waste residue which is produced by the reaction of sulfuric acid and fluorite powder and mainly contains calcium sulfate, wherein each 1 ton of hydrofluoric acid is produced, and the production reaction equation is as follows:
H 2 SO 4 +CaF 2 ＝2HF+CaSO 4
when the fluorogypsum is discharged from the reaction furnace, the material temperature is 180-230 ℃, the gas temperature is 800-1000 ℃, the main component of the discharged gypsum is II-type anhydrous calcium sulfate, the discharged gypsum is strong acid, the pH=2-4, and the annual discharge amount exceeds 250 ten thousand tons, so the yield of the fluorogypsum is considerable.
The properties and main component analysis of the fluorogypsum are shown in the following table 1: the solid product of this reaction is gypsum (CaSO) 4 ) Because of containing small amounts of unreacted CaF 2 So is also called fluorgypsum.
TABLE 1 composition of fluorogypsum (%)
| CaO | MgO | Fe 2 O 3 | Al 2 O 3 | SiO 2 | SO 3 | CaF 2 |
| 32-38 | 0.1-3 | 0.05-0.25 | 0.01-3.0 | 0.6-7.0 | 40-60 | 0.5-2.0 |
At present, most of domestic fluorogypsum is only stored or buried in a pumping slag field after lime or carbide slag is neutralized, so that not only is land resources wasted and huge economic pressure is brought to enterprises, but also residual harmful substances in the fluorogypsum in the storage field can be transferred under the action of rain leaching and wind flushing, so that the ground surface and underground water are polluted, and the human health is seriously endangered.
Although the anhydrous gypsum content in the fluorine gypsum is more than 90%, the hydration speed is extremely slow, a large number of thermodynamically unstable crystallization contact points exist for generating dihydrate gypsum crystals, the water resistance is poor, and the softening coefficient is about 0.2-0.3. Research shows that under the action of proper additive, the solubility and dissolution rate of the fluorogypsum can be improved, the chemical reaction kinetics property in the hydration reaction process can be changed, the hydration rate can be accelerated, and the setting time can be shortened, so that the performance of the fluorogypsum can be improved. Therefore, the fluorine gypsum waste residue is modified, and is converted into gypsum building materials and the like for comprehensive utilization, so that the waste is turned into wealth, the environment is protected, the energy and the resources are saved, and the national sustainable development strategy is met.
Disclosure of Invention
Based on the technical problems, the invention provides the fluorine gypsum composite cementing material and the preparation method thereof, and the fluorine gypsum is modified by adopting proper external additives and assisting a certain process condition, so that the gelation performance of the fluorine gypsum composite cementing material is effectively improved, and the mechanical strength of the fluorine gypsum composite cementing material is enhanced, thereby widening a new way of comprehensively utilizing the fluorine gypsum.
The invention provides a fluorine gypsum composite cementing material, which comprises the following raw materials in percentage by weight: 65-74% of fluorgypsum, 14-21% of slag powder, 5-12% of ordinary Portland cement, 1-3% of alkaline material, 0.5-1.8% of active excitant, 0.2-2% of redispersible latex powder and 0.1-1% of water-retaining thickener.
In order to improve the hydration rate of the fluorine gypsum, promote the coagulation of the fluorine gypsum and improve the strength of the cementing material, the slag powder is fully hydrated in an alkaline environment, and the later strength of the cementing material is improved; the ordinary silicate cement can maintain the volume stability of the fluorine gypsum base and improve the early strength of the composite cementing material; the alkaline material ensures the alkaline environment for hydration of the fluorogypsum gel setting material, ensures that the exciting agent can improve the hydration rate of the fluorogypsum-based plastering material and shortens the setting time; the redispersible emulsion powder excites part of active substances in the composite cementing material to generate a hard mould with a net structure, thereby improving the performances of the composite cementing material such as elastic modulus, water resistance, crack resistance, bonding strength and the like; the water retention thickener can improve the water retention and sagging properties of the fluorine gypsum-based plastering material.
In the invention, the fluorogypsum, the slag powder, the ordinary Portland cement, the alkaline material, the activity excitant, the redispersible emulsion powder, the water reducing agent and the water-retaining thickener are matched with each other to cooperatively play a role, so that the fluorogypsum-based plastering material has the advantages of short setting time, high strength, small bulk density, good volume stability, high bonding strength, excellent water-retaining property and the like.
Preferably, the fluorogypsum is dry powder obtained by grinding and crushing fluorogypsum discharged from hydrofluoric acid production;
the grinding and crushing function is to destroy the crystal lattice, increase the lattice distortion and defects, increase the specific surface area and the irregularity of the surface structure, improve the hydration activity of the fluorine gypsum and promote the hardening of the fluorine gypsum.
Preferably, the fineness of the fluorine gypsum is 150-350 meshes.
The hydration process of the fluorogypsum is carried out from outside to inside, so that the hydration speed is low and the activity is low: the anhydrite particles are thinned by grinding and crushing, so that the contact between the fluorogypsum and water is increasedSpecific surface area, increasing dissolution rate of fluorine gypsum, and enabling Ca in slurry 2+ The dissolution rate is increased, so that the activity of the fluorogypsum is effectively stimulated.
Preferably, the slag powder is blast furnace slag powder, and the slag alkalinity is 1.1-1.4.
The blast furnace slag powder with slag alkalinity of 1.1-1.4 has more sufficient hydration reaction in alkaline environment, and can improve the grain composition of the composite cementing material, so that the volume stability of the composite cementing material is enhanced.
Preferably, the alkaline material is at least one of calcium oxide, calcium hydroxide or potassium hydroxide.
The alkaline material of calcium oxide, calcium hydroxide or potassium hydroxide effectively ensures the alkaline environment of hydration of the fluorine gypsum gel setting material.
Preferably, the activity activator is at least one of sodium sulfate, potassium sulfate, aluminum sulfate, potassium thioaluminate or thioaluminate.
The active excitant can generate unstable double salt (salt mCaSO) on the surface of anhydrite 4 ·nH 2 O), accelerating the formation of the supersaturation degree of the fluorine gypsum and reducing the crystallization activation energy, accelerating the crystallization and remarkably improving the hydration rate: the main transformation process is as follows:
mCaSO 4 +salt nH 2 O.fwdarw.salt.mCaSO 4 ·4nH 2 O (double salt)
Salt mCaSO 4 ·4nH 2 O (double salt) →mCaSO 4 ·2H 2 O+ salt- (n-2 m) H 2 O
The double salt is decomposed into dihydrate gypsum and hydrous salt under the existence of water and exciting agent, and the dihydrate gypsum is continuously crystallized, so that the slurry forms a tightly-interlaced crystal structure, and the setting time is shortened. The sulfate excitant can cause a large amount of acicular ettringite (CSH) gel to appear in the system, and cross coexist with a crystal structure network mainly containing gypsum, and when the sulfate excitant is filled in the crystal gaps of the gypsum, a tightly-interlaced crystal structure is formed, so that the water resistance and the strength of the fluorine gypsum product are greatly improved.
Preferably, the redispersible emulsion powder is ethylene-vinyl acetate copolymer rubber powder, acrylic acid rubber powder and styrene-butadiene rubberPowder, polyvinyl alcohol powder or grafted SiO 2 At least one of the polyvinyl acetate powders;
preferably, the redispersible emulsion powder is grafted SiO 2 Polyvinyl acetate powder of (2).
The redispersible emulsion powder is emulsified and dispersed in water, and after the water is evaporated, a polymer film is formed in the mixing material, so that various performances of the cementing material are improved; in the redispersible emulsion powder selected by the invention, siO is grafted 2 SiO is grafted on the surface of the polyvinyl acetate rubber powder 2 ，SiO 2 The hydration property of the adhesive powder enables the adhesive powder to have excellent water dispersion performance, so that the adhesive powder can be more effectively filled among the hydrated particles of the fluorine gypsum after being emulsified and dispersed, and a cross-linked three-dimensional network structure is formed in the interior, so that the particles of the fluorine gypsum slurry are more tightly bonded together, and the flexural strength performance of the obtained composite cementing material is further improved.
Preferably, the grafted SiO 2 The polyvinyl acetate rubber powder is SiO modified by KH570 2 And monomer containing acid vinyl ester are polymerized under the condition of initiator and dispersant.
Preferably, the water-retaining thickener is at least one of methylcellulose, ethylcellulose, hydroxypropyl methylcellulose, hydroxyethyl cellulose, carboxymethyl cellulose or starch ether.
The high polymer water-retaining agent is generally of a three-dimensional network structure, hydrophilic groups of the high polymer water-retaining agent can form hydrogen bonds with water molecules when the high polymer water-retaining agent contacts water, so that the water evaporation of the fluorine gypsum composite cementing material can be effectively solved, the cohesiveness and uniformity of the gypsum material are improved, and the problems of cracking, hollowing and the like are avoided.
The invention also provides a preparation method of the fluorogypsum composite cementing material, which comprises the following steps: adding the fluorogypsum into grinding equipment, adding slag powder and ordinary Portland cement, and grinding uniformly to obtain modified fluorogypsum; adding the modified fluorogypsum, the alkaline material, the activity excitant, the redispersible latex powder and the water-retaining thickener into stirring equipment, and uniformly stirring to obtain the fluorogypsum composite cementing material.
Preferably, the grinding device is a Raymond mill.
Compared with the prior art, the invention has the following beneficial effects:
(1) In the fluorine gypsum composite cementing material, the raw material components play a synergistic effect, so that the fluorine gypsum composite cementing material has the advantages of short setting time, high strength, small bulk density, good volume stability, bonding strength and the like;
(2) In the fluorine gypsum composite cementing material, the components of the raw materials are reasonably proportioned, so that the optimal modification effect is promoted, the hydration rate of the fluorine gypsum composite cementing material is improved, the setting time is shortened, and the compression resistance and the flexural strength are improved;
(3) The preparation method of the fluorine gypsum composite cementing material is simple, does not need operations such as calcination and the like, is suitable for large-scale commercial production, and simultaneously takes the fluorine gypsum as a main raw material, thereby realizing the recycling of solid waste, avoiding the pollution of waste fluorine gypsum to the environment, and having wide application prospects in the fields of building material preparation, waste recycling and environmental protection.
Detailed Description
The present invention will be described in detail by way of specific examples, which should be clearly set forth for the purpose of illustration and are not to be construed as limiting the scope of the present invention.
Example 1
The fluorine gypsum composite cementing material comprises the following components in percentage by weight: 68.6% of fluorgypsum, 18.4% of slag powder, 8.2% of P.042.5 ordinary Portland cement, 2.3% of calcium oxide, 1.1% of potassium sulphoaluminate, 0.9% of ethylene-vinyl acetate copolymer rubber powder and 0.5% of hydroxypropyl methyl cellulose;
the fluorine gypsum is dry powder obtained by grinding and crushing fluorine gypsum discharged from hydrofluoric acid production, and the fineness of the fluorine gypsum is 200 meshes; the slag powder is blast furnace slag powder, and the slag alkalinity is 1.32.
The method for preparing the fluorine gypsum composite cementing material specifically comprises the following steps: adding the fluorogypsum into a Raymond mill, adding slag powder and ordinary Portland cement P.042.5, and grinding uniformly to obtain modified fluorogypsum; and adding the modified fluorogypsum, calcium oxide, potassium thioaluminate, ethylene-vinyl acetate copolymer rubber powder and hydroxypropyl methyl cellulose into stirring equipment, and uniformly stirring to obtain the fluorogypsum composite cementing material.
Example 2
The fluorine gypsum composite cementing material comprises the following components in percentage by weight: 65.4% of fluorgypsum, 20.7% of slag powder, 7.9% of P.042.5 ordinary Portland cement, 3.0% of calcium hydroxide, 1.0% of potassium sulfate, 1.8% of styrene-butadiene rubber powder and 0.2% of starch ether;
the fluorine gypsum is dry powder obtained by grinding and crushing the fluorine gypsum discharged from the production of hydrofluoric acid, and the fineness of the fluorine gypsum is 200 meshes.
The method for preparing the fluorine gypsum composite cementing material specifically comprises the following steps: adding the fluorogypsum into a Raymond mill, adding slag powder and ordinary Portland cement, and grinding uniformly to obtain modified fluorogypsum; and adding the modified fluorogypsum, calcium hydroxide, potassium sulfate, styrene-butadiene rubber powder and starch ether into stirring equipment, and uniformly stirring to obtain the fluorogypsum composite cementing material.
Example 3
The fluorine gypsum composite cementing material comprises the following components in percentage by weight: 73.4% of fluorgypsum, 14.1% of slag powder, 8.8% of P.042.5 ordinary Portland cement, 1.2% of calcium oxide, 1.6% of aluminum sulfate, 0.2% of polyvinyl alcohol rubber powder and 0.7% of hydroxyethyl cellulose;
the fluorine gypsum is dry powder obtained by grinding and crushing fluorine gypsum discharged from hydrofluoric acid production, and the fineness of the fluorine gypsum is 200 meshes; the slag powder is blast furnace slag powder, and the slag alkalinity is 1.32.
The method for preparing the fluorine gypsum composite cementing material specifically comprises the following steps: adding the fluorogypsum into a Raymond mill, adding slag powder and ordinary Portland cement, and grinding uniformly to obtain modified fluorogypsum; and adding the modified fluorogypsum, calcium oxide, aluminum sulfate, polyvinyl alcohol rubber powder and hydroxyethyl cellulose into stirring equipment, and uniformly stirring to obtain the fluorogypsum composite cementing material.
Example 4
The fluorine gypsum composite cementing material comprises the following components in percentage by weight: 68.6% of fluorgypsum, 18.4% of slag powder, 8.2% of P.042.5 ordinary Portland cement, 2.3% of calcium oxide, 1.1% of potassium sulphoaluminate and grafted SiO 2 0.9% of polyvinyl acetate rubber powder and 0.5% of water-retaining thickener;
the fluorine gypsum is dry powder obtained by grinding and crushing fluorine gypsum discharged from hydrofluoric acid production, and the fineness of the fluorine gypsum is 200 meshes; the slag powder is blast furnace slag powder, and the slag alkalinity is 1.32; the grafted SiO 2 The polyvinyl acetate rubber powder is prepared by the following method:
KH570 and nano SiO are mixed according to the weight ratio of 1:4 2 Adding into ethanol-water mixed solvent, and performing ultrasonic treatment under acidic (pH=4) condition for 15min to obtain KH570 modified SiO 2 The method comprises the steps of carrying out a first treatment on the surface of the KH570 modified SiO in the weight ratio of 1:9:2:0.05:0.01 2 Adding vinyl acetate, vinyl versatate, sodium dodecyl benzene sulfonate (emulsifier) and potassium persulfate (initiator) into water, strongly stirring and mixing uniformly in a polymerization kettle, polymerizing at 50 ℃ for 6h, continuously curing for 2h, and spray-drying the obtained copolymer emulsion to obtain the grafted SiO 2 Polyvinyl acetate powder of (2).
The method for preparing the fluorine gypsum composite cementing material specifically comprises the following steps: adding the fluorogypsum into a Raymond mill, adding slag powder and ordinary Portland cement P.042.5, and grinding uniformly to obtain modified fluorogypsum; the modified fluorogypsum, calcium oxide, potassium thioaluminate and grafted SiO are subjected to the reaction of 2 Adding the polyvinyl acetate rubber powder and the hydroxypropyl methylcellulose into stirring equipment, and uniformly stirring to obtain the fluorine gypsum composite cementing material.
Comparative example 1
The fluorine gypsum composite cementing material comprises the following components in percentage by weight: 68.6% of fluorgypsum, 18.4% of slag powder, 8.2% of P.042.5 ordinary Portland cement, 2.3% of calcium oxide, 1.1% of potassium sulphoaluminate, 0.9% of polyvinyl acetate rubber powder and 0.5% of water-retaining thickener;
the fluorine gypsum is dry powder obtained by grinding and crushing fluorine gypsum discharged from hydrofluoric acid production, the fineness of the fluorine gypsum is 200 meshes, the slag powder is blast furnace slag powder, the slag alkalinity is 1.32, and the polyvinyl acetate rubber powder is prepared by adopting the following method:
adding acid vinyl ester, tertiary ethylene carbonate, sodium dodecyl benzene sulfonate (emulsifier) and potassium persulfate (initiator) into water according to the weight ratio of 9:2:0.05:0.01, strongly stirring and uniformly mixing in a polymerization kettle, carrying out polymerization reaction for 6 hours at 50 ℃, continuing curing for 2 hours, and carrying out spray drying on the obtained copolymer emulsion to obtain the polyvinyl acetate rubber powder.
The method for preparing the fluorine gypsum composite cementing material specifically comprises the following steps: adding the fluorogypsum into a Raymond mill, adding slag powder and ordinary Portland cement P.042.5, and grinding uniformly to obtain modified fluorogypsum; and adding the modified fluorogypsum, calcium oxide, potassium thioaluminate, polyvinyl acetate rubber powder and hydroxypropyl methylcellulose into stirring equipment, and uniformly stirring to obtain the fluorogypsum composite cementing material.
Experimental test:
in order to verify the technical performance of the fluorogypsum composite cementing materials in each example and comparative example, the aqueous gel ratio of 0.35 is adopted for stirring uniformly, the obtained slurry is injection molded, the obtained test block is cured in the environment with the temperature of (20+/-2) ℃ and the relative humidity of 50-60%, the flexural strength and the compressive strength of the test block in different ages are tested, the average value is obtained, the results are shown in the table 1, and the strength measurement is carried out according to the GB/T17671-1999 cement mortar strength test method (ISO method):
table 1 results of test on technical properties of products obtained in examples and comparative examples
| Example 1 | Example 2 | Example 3 | Example 4 | Comparative example 1 | |
| Initial setting time (min) | 1h32min | 1h28min | 1h25min | 1h58min | 1h16min |
| Final setting time (min) | 3h41min | 3h27min | 3h49min | 2h43min | 4h17min |
| 24h flexural Strength (MPa) | 1.9 | 1.7 | 1.6 | 2.7 | 1.2 |
| Compressive strength (MPa) for 24h | 5.4 | 7.1 | 6.4 | 10.5 | 4.5 |
| 7d flexural Strength (MPa) | 7.8 | 8.5 | 6.9 | 9.3 | 5.8 |
| 7d compressive Strength (MPa) | 45.3 | 40.4 | 48.2 | 54.2 | 32.9 |
| Tensile bond Strength (MPa) | 1.0 | 0.9 | 0.8 | 1.2 | 0.6 |
As can be seen from the table, the fluorine gypsum composite cementing material has good physical properties, high flexural strength, compression strength and tensile bonding strength and good construction performance.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.
Claims (4)
1. The fluorine gypsum composite cementing material is characterized by comprising the following raw materials in percentage by weight: 65-74% of fluorgypsum, 14-21% of slag powder, 5-12% of ordinary Portland cement, 1-3% of alkaline material, 0.5-1.8% of active excitant, 0.2-2% of redispersible latex powder and 0.1-1% of water-retaining thickener;
the redispersible emulsion powder is grafted SiO 2 Polyvinyl acetate powder;
the grafted SiO 2 The polyvinyl acetate rubber powder is SiO modified by KH570 2 Polymerizing the vinyl acetate monomer with a monomer containing vinyl acetate under the condition of an initiator and a dispersing agent;
the fluorine gypsum is dry powder obtained by grinding and crushing fluorine gypsum discharged from hydrofluoric acid production; the fineness of the fluorogypsum is 150-350 meshes; the alkaline material is at least one of calcium oxide, calcium hydroxide or potassium hydroxide; the activity excitant is at least one of sodium sulfate, potassium sulfate, aluminum sulfate or potassium thioaluminate; the water-retaining thickener is at least one of methyl cellulose, ethyl cellulose, hydroxypropyl methyl cellulose, hydroxyethyl cellulose, carboxymethyl cellulose or starch ether.
2. The fluorogypsum composite cementitious material of claim 1, wherein the slag powder is blast furnace slag powder and the slag basicity is 1.1-1.4.
3. A method of preparing the fluorogypsum composite gel material according to claim 1 or 2, comprising: adding the fluorogypsum into grinding equipment, adding slag powder and ordinary Portland cement, and grinding uniformly to obtain modified fluorogypsum; adding the modified fluorogypsum, the alkaline material, the activity excitant, the redispersible latex powder and the water-retaining thickener into stirring equipment, and uniformly stirring to obtain the fluorogypsum composite cementing material.
4. A method for preparing a fluorogypsum composite cementitious material in accordance with claim 3, wherein said grinding apparatus is a raymond mill.
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