CN111620713B - Phosphogypsum-based light heat-preservation floor heating module and preparation method thereof - Google Patents
Phosphogypsum-based light heat-preservation floor heating module and preparation method thereof Download PDFInfo
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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
- C04B28/143—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 the synthetic calcium sulfate being phosphogypsum
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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
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/20—Resistance against chemical, physical or biological attack
- C04B2111/27—Water resistance, i.e. waterproof or water-repellent materials
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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
- C04B2111/00—Mortars, concrete or artificial stone or mixtures to prepare them, characterised by specific function, property or use
- C04B2111/40—Porous or lightweight materials
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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
- C04B2201/20—Mortars, concrete or artificial stone characterised by specific physical values for the density
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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
- C04B2201/30—Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values
- C04B2201/32—Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values for the thermal conductivity, e.g. K-factors
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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
Abstract
The invention belongs to the technical field of building materials, and relates to a phosphogypsum-based light heat-insulation floor heating module and a preparation method thereof, wherein the phosphogypsum-based light heat-insulation floor heating module is prepared from the following raw materials in parts by weight: 80-105 parts of phosphorus building gypsum, 3-10 parts of vitrified micro bubbles, 1-5 parts of polyphenyl granules with the grain diameter less than or equal to 2cm, 3-10 parts of cement, 0.1-3 parts of polypropylene fiber and 0.1-0.5 part of retarder; phosphogypsum-based light heat-preservation floor heating module floor heating mold box with volume weight not higher than 1000kg/m3The compressive strength is not lower than 100Kpa, the breaking load is not lower than 200N, the thermal conductivity is not higher than 0.1W/(m.k), and the material does not contain formaldehyde, and is a novel light and heat-insulating building material.
Description
Technical Field
The invention belongs to the technical field of building materials, and relates to a phosphogypsum-based light heat-preservation floor heating module and a preparation method thereof.
Background
The floor heating module is one of the main optional components at the tail end of the floor heating system and is used for replacing auxiliary materials such as insulation boards, reflection films and staple bolts in the traditional floor heating system. The appearance and the application of the floor heating module greatly simplify the floor heating installation procedure. The type of the floor heating module: the composite material comprises EPS modules, extruded sheet modules, metal and heat insulation material composite modules and cement modules according to material division. Since the birth of the floor heating module, the floor heating module is greatly popular in the market due to the obvious improvement of the floor heating module compared with the traditional floor heating process. The floor heating modules of different forms and different materials have respective advantages and also have various defects, such as high manufacturing cost, relatively weak compressive strength and the like of the composite module. The module made of the plastic cargo material has poor fireproof performance, great fire hazard, short service life and the like. The polystyrene foam plastic has the fatal defects that the heat-resistant temperature is low, the polystyrene foam plastic begins to decompose at 74 ℃, the polystyrene foam plastic is thermally melted and shrunk when the temperature is continuously increased, and the compressive strength of the polystyrene foam plastic is only 0.02-0.03MPa, and the polystyrene foam plastic is easy to collapse when the stress is large or uneven; the cement module has high cost due to the fact that a large amount of resources and energy consumption are consumed in the production process of cement, the hydration rate of the cement is high, a large amount of bubbles are broken before initial setting, and defoaming water, slurry collapse and bleeding segregation are formed.
The phosphogypsum is a solid byproduct generated when phosphorite is treated by sulfuric acid in the production of phosphoric acid, about 4.0-5.0 tons of phosphogypsum are generated per 1 ton of phosphoric acid, and the main component of the phosphogypsum is calcium sulfate dihydrate (CaSO)4·2H2O), and also contains small amount of unreacted phosphorus ore, phosphoric acid, fluoride, organic matter, potassium, sodium, etc. After the phosphogypsum is subjected to purification, calcination and modification, the phosphogypsum can be used for producing gypsum building materials. The phosphogypsum is powder, the appearance is grey white, grey black, grey yellow and the like, the attached water is 10 to 30 percent, and the volume weight is 0.733 to 0.88g/cm3The particle diameter is 5-50um generally, the content of calcium sulfate dihydrate is 70-95%, the annual output of phosphogypsum in China is about 7500 ten thousand tons, the accumulated output is about 6 hundred million tons, the method is one of the by-product gypsum with the largest output, and the ecological environment such as atmosphere, soil, underground water and the like in a stacking area and a nearby area can be seriously damaged due to improper treatment. Patent CN201710383656.X discloses a self-leveling lightweight aggregate, which comprises gypsum, portland cement, mineral powder, a lightweight aggregate, a defoaming agent, methyl cellulose, a pour regulator, a water reducer and a waterproof agent. The self-leveling floor has the beneficial effects that the self-leveling floor recorded by the scheme is low in price, has the effects of light weight and heat preservation and insulation, and can be matched with the construction of floor heating and partition walls; in addition, the paint also has the advantages of good fluidity and convenient construction; patent CN201610751291.7 discloses a foaming heat-conducting gypsum-based self-leveling floor tile material, belongs to the self-leveling floor tile material field. The feed is prepared from the following components in parts by mass: 49-54 parts of semi-hydrated gypsum, 6-10 parts of cement, 28-30 parts of quartz sand, 10-15 parts of heavy calcium powder, 0.5-1.6 parts of redispersible latex powder, 0.32-0.45 part of water reducing agent, 0.02-0.03 part of water-retaining agent, 0.06-0.11 part of retarder, 5-10 parts of expandable polystyrene particles and 0.1-0.5 part of PP fiber, and the floor heating adopts the material of the scheme, so that the material has the advantages of small shrinkage, difficulty in cracking, high temperature rise speed of the floor heating, low later-stage temperature reduction speed and good water resistance; patent CN201610218238.0 discloses a polyurethane-composite fiber fireproof floor heating insulation board, which comprises the following components in parts by weight: 30-40 parts of polyurethane, 15-24 parts of composite fiber, 8-17 parts of desulfurized gypsum powder, 3-11 parts of polybutadiene epoxy resin, and B4-9 parts of cyclohexane methyl imido ester, 13-20 parts of fine sand, 15-24 parts of bauxite, 7-13 parts of vermiculite powder, 3-9 parts of calcium sulfonate, 8-15 parts of cement slag, 2-5 parts of a fire retardant, 4-8 parts of potassium ammonium polyphosphate and 25-35 parts of water, and the scheme also discloses a preparation method of the polyurethane-composite fiber fireproof floor heating insulation board; however, in the prior art, the utilization amount of the phosphogypsum is not high, and the phosphogypsum is lower than the expansion shrinkage rate of cement, which can cause cracks to appear on the cement part and is influenced by the impurities of the phosphogypsum, so that the phosphogypsum has strict requirements on the water reducing agent, and in the document 'technical progress research on gypsum-based self-leveling mortar', the 'special water reducing agent for gypsum must be developed and researched due to the influence of the impurities of the industrial byproduct gypsum of the same kind, which has different using effects of the water reducing agent' is clearly pointed out, which greatly increases the application difficulty of the phosphogypsum, and in addition, the interface bonding force of the gypsum, the cement and the polyphenyl granules is weaker, and the mechanical property of the floor heating module is also influenced. Therefore, the floor heating module made of gypsum still needs to be researched.
Disclosure of Invention
The invention provides a phosphogypsum-based light heat-preservation floor heating module and a preparation method thereof to solve the technical problems.
In order to achieve the above purpose, the invention adopts the following technical scheme:
the phosphogypsum-based light heat-preservation floor heating module is prepared from the following raw materials in parts by weight: 80-105 parts of phosphorus building gypsum, 3-10 parts of vitrified micro bubbles, 1-5 parts of polyphenyl granules with the grain diameter less than or equal to 2cm, 3-10 parts of cement, 0.1-3 parts of polypropylene fiber and 0.1-0.5 part of retarder.
Further, the phosphogypsum-based light heat-preservation floor heating module is prepared from the following raw materials in parts by weight: 100 parts of phosphorus building gypsum, 5 parts of cement, 1.5 parts of polypropylene fiber, 0.15 part of retarder, 6 parts of vitrified micro-beads and 1 part of polyphenyl granules with the grain diameter less than or equal to 2 cm.
Furthermore, the phosphorus building gypsum is a product obtained by calcining phosphogypsum and removing crystal water.
Furthermore, the content of the hemihydrate gypsum in the phosphorus building gypsum exceeds 75 percent, and the balance is dihydrate gypsum (CaSO)4·2H2O) or anhydrous calcium sulfate (CaSO)4) One or two of them.
The cement is Portland cement, and the strength grade is not lower than 42.5.
Further preferably, the cement is replaced by modified cement; the modification method comprises the following steps: mixing lotus leaf powder and 30-50% ethanol solution according to the mass ratio of 1: (2-5) placing the mixture in a reaction kettle, heating the mixture for 10-15min at the temperature of 70-80 ℃, then placing the mixture in the ultrasonic dispersion condition of 130-170W for 10-18min, and then adding water and materials according to the mass ratio of 1: (24-30) mixing and stirring the cement for 5-10min, placing the mixture under the condition of 130-170W for ultrasonic dispersion for 8-10min, separating solid from liquid, and drying the mixture under the condition of 80-100 ℃ of microwave until the surface moisture content is less than or equal to 4%.
After the cement is doped into the mortar, the compression strength and the waterproof performance of the product can be improved, the pH value of slurry can be effectively improved, and the phenomena of mildew and yellowing of the finished product after use are avoided.
According to the invention, the lotus leaf powder is used for modifying the cement, so that the hydration rate of the cement is improved, the chemical shrinkage rate, the plastic shrinkage rate and the water absorption performance of the cement are reduced, meanwhile, the cement and organic matters in lotus leaves are mutually combined, the interface combination between the cement and polyphenyl granules is enhanced, and simultaneously, the workability of slurry and the waterproof performance of a floor heating module are enhanced.
The volume weight of the vitrified micro bubbles is more than or equal to 110kg/m3The cylinder pressure strength is more than or equal to 200kPa, the water absorption is less than or equal to 45 percent, and the surface closed pore rate is more than or equal to 80 percent.
Further preferably, the vitrified microbead is replaced by a modified vitrified microbead; the modification method comprises the following steps: mixing sodium oleate with water according to a mass ratio of 1: (1-3) placing in a reaction kettle, heating until sodium oleate is dissolved, performing ultrasonic dispersion for 8-10min under the condition of 130-: and (32-37) mixing and stirring the vitrified micro bubbles for 5-10min, performing ultrasonic dispersion for 12-16min under the condition of 130-170W, and drying the solid part after solid-liquid separation.
The vitrified micro bubbles and the polyphenyl granules are used as light aggregate with high quality and low price, and the volume weight of the product is reduced and the heat insulation performance of the product is improved after the vitrified micro bubbles and the polyphenyl granules are added.
According to the invention, sodium oleate is used for modifying the vitrified micro bubbles, and the sodium oleate has hydrophobic groups and hydrophilic groups, so that physical and chemical adsorption can be generated with specific atoms on the substances, and the compactness of the vitrified micro bubbles and the proportion of the hydrophilic and hydrophobic groups on the surface are changed, so that when the vitrified micro bubbles are contacted with cement, the foaming performance of the cement can be improved, and a large number of pores are generated in the cement paste. Meanwhile, the sodium oleate modified vitrified small balls have the function of increasing material binding force, the construction efficiency and the heat conductivity coefficient are improved, the heat transfer capacity of the floor heating module is enhanced, and the defects that the vitrified small balls are low in construction efficiency and the heat conductivity coefficient is basically bestant to about 0.07W/(m.K) … … and cannot be applied in a large area in northern areas recorded in the research on the performance optimization and application of the expanded vitrified small ball insulation board are overcome.
The invention utilizes the vitrified micro bubbles, has light weight, excellent physical and chemical properties, outstanding durability, low heat conductivity coefficient, excellent waterproof and high temperature resistance and other properties, and can effectively solve the problems of high water absorption of slurry, reduced later strength of products, hollowing and cracking and the like.
Furthermore, the length of the polypropylene fiber is less than or equal to 3 cm.
Further, the polypropylene fibers are replaced with modified polypropylene fibers; the modification method comprises the following steps: mixing a silane coupling agent and polypropylene fibers according to the weight ratio of 1: (45-50) mixing at 45-50 deg.C for 10-20 min.
The invention can greatly improve the breaking load of the product after being doped with the polypropylene fiber and reduce the damage rate of the product in the transportation and construction.
According to the invention, the silane coupling agent is used for modifying the polypropylene fiber, so that the thermal stability and the water absorption performance of the fiber can be improved, the bonding capability of gypsum, cement and polyphenyl particles is further enhanced, a stable structure is formed, and the mechanical property and the waterproof performance of the floor heating module are effectively improved.
The retarder has a pH value of 8-9.
The particle size of the polyphenyl particles is less than or equal to 2 cm.
Further, the phosphogypsum-based light heat-preservation floor heating module and the preparation method thereof comprise the following steps:
(1) metering: weighing phosphorous building gypsum, cement, vitrified micro bubbles, polyphenyl granules, polypropylene fibers and a retarder according to parts by weight;
(2) mixing and stirring: pouring the weighed phosphorus building gypsum, cement, polypropylene fiber and retarder into a stirrer for mixing, pouring the weighed vitrified micro bubbles and polyphenyl granules into the stirrer for secondary mixing after uniform mixing, and adding water for wet mixing to obtain slurry;
(3) forming and leveling: pouring the slurry into a mold for molding, scraping redundant slurry while vibrating in the molding process, and leveling after the slurry is solidified;
(4) drying: drying the formed and leveled semi-finished product to discharge attached water, thereby obtaining a finished product.
Further, in step (1), the metering error of the retarder should not exceed 0.2%.
Further, a secondary stirring mode is adopted in the step (2), the stirring time is not less than 3min, and the added water accounts for 50-100% of the mass of the dry materials.
Further, in the step (3), the vibration time of the slurry is 1-3 min.
Further, in step (4), the drying temperature does not exceed 100 ℃.
Due to the adoption of the technical scheme, the invention has the following beneficial effects:
phosphogypsum-based light heat-preservation floor heating module floor heating mold box with volume weight not higher than 1000kg/m3The compressive strength is not lower than 100Kpa, the breaking load is not lower than 200N, the thermal conductivity is not higher than 0.1W/(m.k), and the material does not contain formaldehyde, and is a novel light and heat-insulating building material.
(1) The invention adopts the phosphorus building gypsum, the cement, the vitrified micro bubbles, the polyphenyl granules, the fibers and the retarder as raw materials, wherein the raw materials used by the phosphorus building gypsum are industrial wastes which are used as air-hardening cementing materials, and the production cost is lower compared with the cementing materials such as cement, lime and the like which are calcined at high temperature because the low-temperature calcination is adopted, so that the production cost of the floor heating module can be effectively reduced and the production benefit can be improved when the phosphorus building gypsum is used for producing the floor heating module.
(2) The invention takes the phosphorus building gypsum as the main raw material, can improve the utilization rate of industrial waste, and is a new green building material variety which is vigorously popularized by China; the phosphorus building gypsum is used as a non-combustible material, has excellent fireproof performance, and a product processed by the phosphorus building gypsum has natural fireproof advantages and can reduce fire hidden danger after being used; in addition, the phosphorus building gypsum has the characteristics of quick setting and good plasticity, the production period of the floor heating module produced by using the phosphorus building gypsum is short, the efficiency is high, and products in various shapes can be produced according to the mould.
(3) The construction of the floor heating module is quicker than that of similar products, and the construction can be completed synchronously with the floor heating pipe, namely the floor heating pipe is laid while the module is covered.
(4) The floor heating module disclosed by the invention has good heat preservation, heat conduction and mechanical properties and good waterproof performance, and effectively solves the problem that condensed water vapor formed between the floor heating pipe and the floor heating module damages the traditional module after the floor heating is closed, so that the service life of the floor heating module disclosed by the invention is longer.
Detailed Description
The following is a detailed description of the embodiments of the present invention, but the present invention is not limited to these embodiments, and any modifications or substitutions in the basic spirit of the embodiments are included in the scope of the present invention as claimed in the claims.
Example 1
The phosphogypsum-based light heat-preservation floor heating module is prepared from the following raw materials in parts by weight: 100 parts of phosphorus building gypsum, 5 parts of cement, 1.5 parts of fiber, 0.15 part of retarder, 6 parts of vitrified micro bubbles and 1 part of polyphenyl granules;
the phosphorus building gypsum is a product obtained by calcining phosphogypsum and removing part of crystal water, and comprises the following chemical components: semi-hydrated gypsum (CaSO)4·1/2H2O) content of more than or equal to 80%, and dihydrate Gypsum (CaSO)4·2H2O)≤1% and III anhydrous calcium sulfate content of (CaSO)4) Less than or equal to 4 percent; the cement is general cement produced by a cement plant, and the strength grade is 42.5; the volume weight of the vitrified micro bubbles is 120kg/m3The cylinder pressure strength is 210kPa, the water absorption is 48%, and the surface closed porosity is 80%; the fiber is polypropylene fiber, and the length of the fiber is 0.6 cm; the retarder is a special retarder for gypsum, and has a pH value: 9; the particle size of the polyphenyl particles is 1 cm;
a preparation method of a floor heating module produced by taking phosphogypsum as a main raw material comprises the following steps:
(1) metering: weighing the phosphorous building gypsum, the cement, the vitrified micro bubbles, the polyphenyl granules, the fibers and the retarder according to the parts by weight; the metering error of the retarder must not exceed 0.2%;
(2) mixing and stirring: pouring the weighed building gypsum, cement, fiber and retarder into a stirrer for mixing, pouring the weighed vitrified micro bubbles and polyphenyl granules into the stirrer for secondary mixing after uniform mixing, and adding water for wet mixing; in the step (2), a secondary stirring mode is adopted, the stirring time is 3min, and the water addition amount accounts for 70% of the dry material mass;
(3) forming and leveling: pouring the mixed slurry into a mould for forming, scraping redundant slurry while vibrating in the forming process, and leveling after the slurry is solidified; the vibrating time of the slurry is 2 min;
(4) drying: drying the formed and leveled semi-finished product to discharge attached water, thereby obtaining a finished product; the drying temperature is 100 ℃.
Example 2
The phosphogypsum-based light heat-preservation floor heating module is prepared from the following raw materials in parts by weight: 100 parts of phosphorus building gypsum, 5 parts of cement, 1.5 parts of fiber, 0.1 part of retarder and 8 parts of vitrified micro bubbles;
the phosphorus building gypsum is a product obtained by calcining phosphogypsum and removing part of crystal water, and comprises the following chemical components: semi-hydrated gypsum (CaSO)4·1/2H2O) content of more than or equal to 85%, and dihydrate Gypsum (CaSO)4·2H2O) is less than or equal to 3 percent, and the content of anhydrous calcium sulfate III is (CaSO)4) Less than or equal to 4 percent; the cement is general cement produced by a cement plant, and the strength grade is 42.5; the volume weight of the vitrified micro bubbles is 120kg/m3The cylinder pressure strength is 210kPa, the water absorption is 48%, and the surface closed porosity is 80%; the fiber is polypropylene fiber, and the length of the fiber is 0.6 cm; the retarder is a special retarder for gypsum, and the pH value is as follows: 9;
a preparation method of a floor heating module produced by taking phosphogypsum as a main raw material comprises the following steps:
(1) metering: weighing the phosphorous building gypsum, the cement, the vitrified micro bubbles, the polyphenyl granules, the fibers and the retarder according to the parts by weight; the metering error of the retarder must not exceed 0.2%;
(2) mixing and stirring: pouring the weighed building gypsum, cement, fiber and retarder into a stirrer for mixing, pouring the weighed vitrified micro bubbles and polyphenyl granules into the stirrer for secondary mixing after uniform mixing, and adding water for wet mixing; in the step (2), a secondary stirring mode is adopted, the stirring time is 10min, and the added water accounts for 50% of the dry material mass;
(3) forming and leveling: pouring the mixed slurry into a mould for forming, scraping redundant slurry while vibrating in the forming process, and leveling after the slurry is solidified; the vibrating time of the slurry is 1 min;
(4) drying: drying the formed and leveled semi-finished product to discharge attached water, thereby obtaining a finished product; the drying temperature is 88 ℃.
Example 3
The phosphogypsum-based light heat-preservation floor heating module is prepared from the following raw materials in parts by weight: 100 parts of phosphorus building gypsum, 5 parts of cement, 1.5 parts of fiber, 0.1 part of retarder and 6 parts of polyphenyl granules;
the phosphorus building gypsum is a product obtained by calcining phosphogypsum and removing part of crystal water, and comprises the following chemical components: semi-hydrated gypsum (CaSO)4·1/2H2O) content of more than or equal to 85%, and dihydrate Gypsum (CaSO)4·2H2O) is less than or equal to 3 percent, and the content of anhydrous calcium sulfate III is (CaSO)4) Less than or equal to 4 percent; the cement is general cement produced by a cement plantIntensity rating of 42.5; the fiber is polypropylene fiber, and the length of the fiber is 0.6 cm; the retarder is a special retarder for gypsum, and has a pH value: 9;
a preparation method of a floor heating module produced by taking phosphogypsum as a main raw material comprises the following steps:
(1) metering: weighing the phosphorous building gypsum, the cement, the vitrified micro bubbles, the polyphenyl granules, the fibers and the retarder according to the parts by weight; the metering error of the retarder must not exceed 0.2%;
(2) mixing and stirring: pouring the weighed building gypsum, cement, fiber and retarder into a stirrer for mixing, pouring the weighed vitrified micro bubbles and polyphenyl granules into the stirrer for secondary mixing after uniform mixing, and adding water for wet mixing; in the step (2), a secondary stirring mode is adopted, the stirring time is 20min, and the water addition amount accounts for 100% of the dry material mass;
(3) forming and leveling: pouring the mixed slurry into a mould for forming, scraping redundant slurry while vibrating in the forming process, and leveling after the slurry is solidified; the vibrating time of the slurry is 3 min;
(4) drying: drying the formed and leveled semi-finished product to discharge attached water, thereby obtaining a finished product; the drying temperature is 75 ℃.
Example 4
The phosphogypsum-based light heat-preservation floor heating module is prepared from the following raw materials in parts by weight: 100 parts of phosphorus building gypsum, 8 parts of cement, 2 parts of fiber, 0.15 part of retarder, 3 parts of vitrified micro bubbles and 3 parts of polyphenyl granules;
the phosphorus building gypsum is a product obtained by calcining phosphogypsum and removing part of crystal water, and comprises the following chemical components: semi-hydrated gypsum (CaSO)4·1/2H2O) content of more than or equal to 85%, and dihydrate Gypsum (CaSO)4·2H2O) is less than or equal to 2 percent, and III is anhydrous calcium sulfate with the content of (CaSO)4) Less than or equal to 3 percent; the cement is general cement produced by a cement plant, and the strength grade is 42.5; the volume weight of the vitrified micro bubbles is 140kg/m3The cylinder pressure strength is 220kPa, the water absorption is 48 percent, and the surface closed pore rate is 82 percent; the fiber is polypropyleneA fiber having a length of 1 cm; the retarder is a special retarder for gypsum, and the pH value is as follows: 9; the particle size of the polyphenyl particles is 0.5 cm;
a preparation method of a floor heating module produced by taking phosphogypsum as a main raw material comprises the following steps:
(1) metering: weighing the phosphorous building gypsum, the cement, the vitrified micro bubbles, the polyphenyl granules, the fibers and the retarder according to parts by weight; the metering error of the retarder must not exceed 0.2%;
(2) mixing and stirring: pouring the weighed building gypsum, cement, fiber and retarder into a stirrer for mixing, pouring the weighed vitrified micro bubbles and polyphenyl granules into the stirrer for secondary mixing after uniform mixing, and adding water for wet mixing; in the step (2), a secondary stirring mode is adopted, the stirring time is 7min, and the added water accounts for 64 percent of the dry material mass;
(3) forming and leveling: pouring the mixed slurry into a mould for forming, scraping redundant slurry while vibrating in the forming process, and leveling after the slurry is solidified; the vibrating time of the slurry is 1.5 min;
(4) drying: drying the formed and leveled semi-finished product to discharge attached water, thereby obtaining a finished product; the drying temperature is 63 ℃.
Example 5
On the basis of the example 1, modified cement is used for replacing cement; the modification method comprises the following steps: mixing lotus leaf powder and 50% ethanol solution according to the mass ratio of 1: 5, placing the mixture in a reaction kettle, heating the mixture for 15min at the temperature of 80 ℃, then placing the mixture in a 170W condition for ultrasonic dispersion for 18min, and then adding water and materials in a mass ratio of 1: mixing and stirring 30 parts of cement for 10min, performing ultrasonic dispersion for 10min under the condition of 170W, performing solid-liquid separation, and drying under the microwave condition of 100 ℃ until the surface moisture content is less than or equal to 4%.
Example 6
On the basis of the example 1, modified cement is used for replacing cement; the modification method comprises the following steps: mixing lotus leaf powder and an ethanol solution with the mass concentration of 30% according to the mass ratio of 1: 2, placing the mixture in a reaction kettle, heating the mixture for 10min at the temperature of 70 ℃, then placing the mixture in a reaction kettle for ultrasonic dispersion for 10-18min under the condition of 130W, and then adding water and materials in a mass ratio of 1: mixing and stirring the 24 cement for 5min, performing ultrasonic dispersion for 8min under the condition of 130W, performing solid-liquid separation, and drying under the condition of 80 ℃ microwave until the surface moisture content is less than or equal to 4%;
meanwhile, the modified vitrified small balls are used for replacing the vitrified small balls; the modification method comprises the following steps: mixing sodium oleate with water according to a mass ratio of 1: 1, placing the mixture in a reaction kettle, heating until sodium oleate is dissolved, performing ultrasonic dispersion for 8min under the condition of 130W, and then adding water and material in a mass ratio of 1: 32, mixing and stirring the vitrified micro bubbles for 5min, placing the mixture under the condition of 130W for ultrasonic dispersion for 12min, and drying the solid part after solid-liquid separation.
Example 7
On the basis of example 2, the modified vitrified micro bubbles are used for replacing the vitrified micro bubbles; the modification method comprises the following steps: mixing sodium oleate with water according to a mass ratio of 1: 3, placing in a reaction kettle, heating until sodium oleate is dissolved, performing ultrasonic dispersion for 10min under the condition of 170W, and then adding water and material in a mass ratio of 1: 37, stirring for 10min, placing under the condition of 170W, making ultrasonic dispersion for 16min, after solid-liquid separation, drying solid portion.
Example 8
On the basis of example 2, modified vitrified microbeads are used instead; the modification method comprises the following steps: mixing sodium oleate with water according to a mass ratio of 1: 2, placing the mixture in a reaction kettle, heating until sodium oleate is dissolved, performing ultrasonic dispersion for 9min under the condition of 140W, and then adding water and materials in a mass ratio of 1: 34, mixing and stirring the vitrified micro bubbles for 6min, placing the mixture under the condition of 160W for ultrasonic dispersion for 14min, and drying a solid part after solid-liquid separation;
meanwhile, the modified polypropylene fiber is used for replacing the polypropylene fiber; the modification method comprises the following steps: mixing a silane coupling agent and polypropylene fibers according to the weight ratio of 1: 48 mass ratio, and mixing for 10-20min at 47 ℃.
Example 9
On the basis of the example 3, the modified polypropylene fiber is used for replacing the polypropylene fiber; the modification method comprises the following steps: mixing a silane coupling agent and polypropylene fibers according to the weight ratio of 1: 45 mass ratio, and mixing for 10min at 45 ℃.
Example 10
On the basis of example 3, modified cement is used for replacing cement; the modification method comprises the following steps: mixing lotus leaf powder and an ethanol solution with the mass concentration of 40% according to the mass ratio of 1: 4, placing the mixture in a reaction kettle, heating the mixture for 12min at the temperature of 75 ℃, then placing the mixture in a reaction kettle for ultrasonic dispersion for 13min under the condition of 150W, and then adding water and materials in a mass ratio of 1: 27, mixing and stirring the cement for 10min, placing the mixture under the condition of 150W for ultrasonic dispersion for 7min, separating solid from liquid, and placing the mixture under the microwave condition of 90 ℃ for drying until the surface moisture content is less than or equal to 4%;
meanwhile, the modified polypropylene fiber is used for replacing the polypropylene fiber; the modification method comprises the following steps: mixing a silane coupling agent and polypropylene fibers according to the weight ratio of 1: mixing at 50 wt% for 20min at 50 deg.C.
Example 11
On the basis of example 4, modified cement is used to replace cement; the modification method comprises the following steps: mixing lotus leaf powder and an ethanol solution with the mass concentration of 40% according to the mass ratio of 1: 4, placing the mixture in a reaction kettle, heating the mixture for 12min at the temperature of 75 ℃, then placing the mixture in a reaction kettle for ultrasonic dispersion for 13min under the condition of 150W, and then adding water and materials in a mass ratio of 1: 27, mixing and stirring the cement for 10min, placing the mixture under the condition of 150W for ultrasonic dispersion for 7min, separating solid from liquid, and placing the mixture under the microwave condition of 90 ℃ for drying until the surface moisture content is less than or equal to 4%;
replacing the vitrified micro bubbles with modified vitrified micro bubbles; the modification method comprises the following steps: mixing sodium oleate with water according to a mass ratio of 1: 1.8 placing in a reaction kettle, heating until sodium oleate is dissolved, ultrasonically dispersing for 9min under the condition of 155W, and then adding water and material in a mass ratio of 1: 35, mixing and stirring the vitrified micro bubbles for 7min, placing the mixture under the condition of 145W for ultrasonic dispersion for 15min, and drying a solid part after solid-liquid separation;
replacing polypropylene fibers with modified polypropylene fibers; the modification method comprises the following steps: mixing a silane coupling agent and polypropylene fibers according to the weight ratio of 1: 49 mass ratio, and mixing for 13min at 47 ℃.
Comparative example 1
On the basis of the embodiment 1, the difference from the embodiment 1 is that: the feed is prepared from the following raw materials in parts by weight: 79 parts of phosphorus building gypsum, 6 parts of vitrified micro bubbles, 1 part of polyphenyl granules, 2.8 parts of cement, 1.5 parts of fibers and 0.15 part of retarder.
Comparative example 2
On the basis of the embodiment 1, the difference from the embodiment 1 is that: 105 parts of phosphorus building gypsum, 5 parts of cement, 1.5 parts of fiber, 0.15 part of retarder, 10.3 parts of vitrified micro-beads and 5.5 parts of polyphenyl granules.
Comparative example 3
On the basis of the embodiment 2, the difference from the embodiment 2 is that: the polypropylene fibers are replaced by polyvinyl alcohol fibers.
Comparative example 4
On the basis of example 3, the difference from example 3 is that: the polypropylene fibers are replaced by glass fibers.
Comparative example 5
On the basis of the embodiment 4, the difference from the embodiment 4 is that: the vitrified micro bubbles are replaced by expanded perlite.
Comparative example 6
On the basis of example 5, the difference from example 5 is that: the lotus leaf powder is replaced by sodium oleate.
Comparative example 7
On the basis of example 11, the difference from example 11 is that: the lotus leaf powder is replaced by stearic acid.
Experimental example 1
1. Test of Water resistance
The samples obtained in the examples and the comparative examples are soaked in clear water at the temperature of (20 +/-2) DEG C, taken out after 24 hours, wiped to dry the surface moisture, then each group is tested by three samples, the average value is taken, and the calculation formula is as shown in formula 1: wa ═ m2-m1)/m 1; wherein: m1 mass of sample when dried; m2 mass of the sample after 24h of immersion; the results are shown in table 1:
TABLE 1
2. Heat conductivity test
The instrument used for measuring the heat conductivity coefficient in the experiment is a TPMBE-300 flat heat conductivity instrument; the specification and the size of a test piece for testing the heat conductivity coefficient are 200mm multiplied by 50 mm; the starting temperature of a hot plate is 34 ℃, the starting temperature of a cold plate is 8 ℃, and the power is 3.4W; the test results are shown in table 2;
TABLE 2
3. Mechanical Property test
3.1 determination of the flexural Strength: the specification of the sample is 50mm multiplied by 100mm, the sample is placed in the center of a clamp of an anti-bending tester to test the anti-bending strength of the sample, and after the sample is broken, the instrument is stopped and the data displayed on the instrument is recorded; the results are shown in Table 3;
TABLE 3
| Test specimen | Dry folding (N) | Test specimen | Dry folding (N) |
| Example 1 | 255.01 | Example 10 | 267.20 |
| Example 2 | 252.63 | Example 11 | 268.18 |
| Example 3 | 250.75 | Comparative example 1 | 213.73 |
| Example 4 | 249.82 | Comparative example 2 | 202.96 |
| Example 5 | 265.12 | Comparative example 3 | 224.62 |
| Example 6 | 261.07 | Comparative example 4 | 203.54 |
| Example 7 | 266.98 | Comparative example 5 | 194.31 |
| Example 8 | 263.24 | Comparative example 6 | 217.17 |
| Example 9 | 265.19 | Comparative example 7 | 190.49 |
3.2 determination of compressive strength: after the bending strength is measured, 2 half test pieces formed by breaking three test pieces are sequentially placed at the central position of a clamp of the numerical control compression tester, the compression strength of the test pieces starts to be measured, and test data are recorded after the test is finished; the results are shown in Table 4;
TABLE 4
| Test specimen | Dry pressure (MPa) | Test specimen | Dry pressure (MPa) |
| Example 1 | 47.3 | Example 10 | 46.7 |
| Example 2 | 46.2 | Example 11 | 46.6 |
| Example 3 | 46.5 | Comparative example 1 | 32.9 |
| Example 4 | 45.8 | Comparative example 2 | 28.9 |
| Example 5 | 46.6 | Comparative example 3 | 33.5 |
| Example 6 | 45.9 | Comparative example 4 | 30.9 |
| Example 7 | 47.1 | Comparative example 5 | 29.6 |
| Example 8 | 46.8 | Comparative example 6 | 35.7 |
| Example 9 | 46.3 | Comparative example 7 | 42.1 |
Claims (7)
1. The phosphogypsum-based light heat-insulation floor heating module is characterized by being prepared from the following raw materials in parts by weight: 80-105 parts of phosphorus building gypsum, 3-10 parts of vitrified micro bubbles, 1-5 parts of polyphenyl granules with the grain diameter less than or equal to 2cm, 3-10 parts of cement, 0.1-3 parts of polypropylene fiber and 0.1-0.5 part of retarder;
the cement is modified cement; the modification method comprises the following steps: mixing lotus leaf powder and 30-50% ethanol solution according to the mass ratio of 1: (2-5) placing the mixture in a reaction kettle, heating the mixture for 10-15min at the temperature of 70-80 ℃, then placing the mixture in the ultrasonic dispersion condition of 130-170W for 10-18min, and then mixing the mixture according to the mass ratio of water to material of 1: (24-30), adding cement in proportion, mixing and stirring for 5-10min, placing under the condition of 130-170W ultrasonic dispersion for 8-10min, after solid-liquid separation, placing under the condition of 80-100 ℃ microwave drying until the surface moisture content is less than or equal to 4%;
the vitrified micro bubbles are modified vitrified micro bubbles; the modification method comprises the following steps: mixing sodium oleate with water according to a mass ratio of 1: (1-3) placing in a reaction kettle, heating until sodium oleate is dissolved, ultrasonically dispersing for 8-10min under the condition of 130-: (32-37) adding vitrified micro bubbles in proportion, mixing and stirring for 5-10min, placing under the condition of 130-170W ultrasonic dispersion for 12-16min, and drying the solid part after solid-liquid separation;
the polypropylene fiber is a modified polypropylene fiber; the modification method comprises the following steps: mixing a silane coupling agent and polypropylene fibers according to the weight ratio of 1: (45-50) mixing at 45-50 deg.C for 10-20 min.
2. The phosphogypsum-based light heat-preservation floor heating module as claimed in claim 1, which is prepared from the following raw materials in parts by weight: 100 parts of phosphorus building gypsum, 5 parts of cement, 1.5 parts of polypropylene fiber, 0.15 part of retarder, 6 parts of vitrified micro-beads and 1 part of polyphenyl granules with the grain diameter less than or equal to 2 cm.
3. The phosphogypsum-based lightweight heat-preservation floor heating module as claimed in claim 1 or 2, wherein the content of the hemihydrate gypsum in the phosphogypsum building gypsum exceeds 75%, and the balance is one or two of dihydrate gypsum and anhydrous calcium sulfate.
4. The phosphogypsum-based lightweight insulated floor heating module as claimed in claim 1 or 2, characterized in that the vitrified micro bubblesThe volume weight is more than or equal to 110kg/m3The cylinder pressure strength is more than or equal to 200kPa, the water absorption is less than or equal to 45 percent, and the surface closed pore rate is more than or equal to 80 percent.
5. The phosphogypsum-based lightweight insulated floor heating module as claimed in claim 1 or 2, characterized in that the polypropylene fiber has a length of less than or equal to 3 cm.
6. The phosphogypsum-based lightweight insulated floor heating module as claimed in claim 1 or 2, characterized in that the retarder has a pH value of 8-9.
7. The preparation method of the phosphogypsum-based light heat-preservation floor heating module as claimed in any one of claims 1 to 6, is characterized by comprising the following steps:
(1) metering: weighing phosphorous building gypsum, cement, vitrified micro bubbles, polyphenyl granules, polypropylene fibers and a retarder according to parts by weight;
(2) mixing and stirring: pouring the weighed phosphorus building gypsum, cement, polypropylene fiber and retarder into a stirrer for mixing, pouring the weighed vitrified micro bubbles and polyphenyl granules into the stirrer for secondary mixing after uniform mixing, and adding water for wet mixing to obtain slurry;
(3) forming and leveling: pouring the slurry into a mold for molding, scraping redundant slurry while vibrating in the molding process, and leveling after the slurry is solidified;
(4) drying: drying the formed and leveled semi-finished product to discharge attached water, thereby obtaining a finished product.
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| CN113416053A (en) * | 2021-08-03 | 2021-09-21 | 单成敏 | Gypsum-based cement light sound insulation wallboard capable of adsorbing and decomposing formaldehyde |
| CN115849847A (en) * | 2022-11-18 | 2023-03-28 | 贵州开磷集团股份有限公司 | Anti-cracking phosphogypsum-based light material |
| CN116535182A (en) * | 2023-04-28 | 2023-08-04 | 中信建筑设计研究总院有限公司 | Incombustible dry floor heating module and preparation method thereof |
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