CN111116046A - Preparation method of high-strength flame-retardant waterproof glass wool - Google Patents
Preparation method of high-strength flame-retardant waterproof glass wool Download PDFInfo
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- CN111116046A CN111116046A CN201911354013.8A CN201911354013A CN111116046A CN 111116046 A CN111116046 A CN 111116046A CN 201911354013 A CN201911354013 A CN 201911354013A CN 111116046 A CN111116046 A CN 111116046A
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C13/00—Fibre or filament compositions
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03B—MANUFACTURE, SHAPING, OR SUPPLEMENTARY PROCESSES
- C03B37/00—Manufacture or treatment of flakes, fibres, or filaments from softened glass, minerals, or slags
- C03B37/01—Manufacture of glass fibres or filaments
- C03B37/04—Manufacture of glass fibres or filaments by using centrifugal force, e.g. spinning through radial orifices; Construction of the spinner cups therefor
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
- C03C1/002—Use of waste materials, e.g. slags
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C14/00—Glass compositions containing a non-glass component, e.g. compositions containing fibres, filaments, whiskers, platelets, or the like, dispersed in a glass matrix
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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
- C04B30/00—Compositions for artificial stone, not containing binders
- C04B30/02—Compositions for artificial stone, not containing binders containing fibrous 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
- C04B2111/20—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
- C04B2111/20—Resistance against chemical, physical or biological attack
- C04B2111/28—Fire resistance, i.e. materials resistant to accidental fires or high temperatures
Abstract
The invention belongs to the technical field of building material preparation, and particularly relates to a preparation method of high-strength flame-retardant waterproof glass wool. Firstly, bagasse and wheat straw are mixed and crushed, solid products, cullet, calcite and other raw materials are mixed and ground, high-temperature treatment is carried out to prepare glass liquid, the glass liquid is put into a glass wool centrifuge for treatment and drying to obtain the high-strength flame-retardant waterproof glass wool; the aluminum ions are introduced into the plant fibers, the mechanical strength of the glass wool is improved, meanwhile, the aluminum simple substance is dispersed in the glass wool by utilizing the fiber components, the flame retardant property of the glass wool is enhanced under the high temperature condition, the fiber components and the carbohydrate are carbonized, the waterproof property and the mechanical strength are improved, and the application prospect is wide.
Description
Technical Field
The invention belongs to the technical field of building material preparation, and particularly relates to a preparation method of high-strength flame-retardant waterproof glass wool.
Background
CN201410853918.0 discloses a glass wool ceiling, it includes glass wool board layer, glass fiber mat layer, gypsum coating layer, and the glass wool board layer adds the centrifugal glass wool fibre that adds the environmental protection resin binder and makes, and the mass ratio of centrifugal glass wool fibre and environmental protection resin binder, gypsum coating is: 85-93: 7-15: 2-3; the preparation method comprises the steps of uniformly spraying the environment-friendly resin binder on the surface of centrifugal glass cotton fiber in an atomized state, collecting cotton by a cotton collector, compressing, conveying, curing in a curing furnace to obtain a glass cotton plate, then pasting the glass fiber felt on the glass cotton plate, and spraying a compressed gypsum coating according to different decorative patterns; compared with the prior art, the scheme can prepare the glass wool ceiling with rich and various shapes according to the requirements of customers, the ceiling not only has good heat preservation, heat insulation, sound absorption and fire prevention effects, but also does not drop dust, does not release formaldehyde, does not damage the health of users, has light weight, can reduce the load requirements on buildings, and is more convenient to carry and install.
The glass wool belongs to an inorganic heat-insulating material, is an important member in the field of heat-insulating materials, not only has the excellent properties of non-combustibility, small heat conductivity coefficient, good chemical stability and the like, but also can be compounded with other materials or deeply processed, thereby expanding the application field of products. As the glass wool product is more and more widely applied to industries such as building, metallurgy, petroleum, chemical industry, national defense and military industry and the like and high and new technology industries, the glass wool product plays an important role in the national economic development.
However, glass wool is relatively brittle and generally has low mechanical strength, and cellulose breakage is likely to occur after long-term use. Meanwhile, the glass wool is a heat-insulating material with a small heat conductivity coefficient, and compared with other raw materials, the glass wool is adhered with an adhesive on the surface, and the adhesive is easy to generate stickiness when being heated and even cause the deformation of the glass wool, so that when the glass wool is used as a heat-insulating layer, the heat conductivity coefficient of the glass wool is greatly reduced in order not to influence the use effect and the service life of the glass wool, the stability of the glass wool under a high-temperature condition is further improved, and the glass wool has important value.
Glass wool is an artificial inorganic fiber, belonging to one category of glass fibers. The glass wool is made up by using natural ore of quartz sand, limestone and dolomite as main raw material, and adding some chemical raw materials of soda ash and borax, etc. and melting them into glass, fiberizing the molten glass, and adding environment-protecting formula adhesive using thermosetting resin as main component. The glass wool has the characteristics of good molding, small volume density, thermal conductivity , heat preservation and insulation, good sound absorption performance, corrosion resistance, stable chemical performance and the like; typical porous sound absorbing materials have good sound absorbing properties. The common pure glass wool has poor flame-retardant and heat-insulating effects, cannot meet the requirements of modern society on the flame-retardant and heat-insulating effects of the glass wool, and limits the wide application of the glass wool. Therefore, it is necessary to further improve the flame retardant property of the existing glass wool to meet the use requirement of the glass wool.
The glass wool is used as a heat-insulating attractive heat-insulating material and is widely applied to the fields of petroleum, chemical engineering, construction, heat preservation, sound absorption, heat insulation and the like, the high-density glass wool board in the market is mainly a product which is prepared by taking phenolic resin in the traditional process as a binder and has the thickness of 48kg/cm3 multiplied by 50mm, 64kg/cm3 multiplied by 50mm and the like specified in the national standard GB/T13350, the board generally has the thickness of not more than 50mm, the requirements of customers in high-density, high-area-density and high-thickness board products in high-cold regions, coastal defense regions and the like cannot be met, meanwhile, a certain formaldehyde release amount still exists in the original phenolic adhesive board product after curing, a certain potential safety hazard is realized, the requirements of the current world on the environment are not higher and higher, and the popularization and application of the.
The glass wool belongs to one category of glass fiber and is artificial inorganic fiber, the glass wool is a material for forming a cotton shape by fiberizing molten glass, the chemical components belong to glass, the glass wool is inorganic fiber and has the advantages of good forming property, small volume density, low thermal conductivity, heat insulation, good sound absorption performance, corrosion resistance and stable chemical performance, however, the existing glass wool roll does not have the waterproof function and can not meet the using requirement in use.
At present, glass wool exists: high brittleness, general mechanical performance, poor impact resistance, general waterproofness and the like.
Therefore, the invention of the excellent glass wool has positive significance to the technical field of building material preparation.
Disclosure of Invention
The technical problems to be solved by the invention are as follows: aiming at the defects that the existing glass wool is large in brittleness and poor in impact resistance and durability caused by general mechanical strength, and meanwhile, the glass wool is poor in flame retardant property and general in waterproof property, the preparation method of the high-strength flame retardant waterproof glass wool is provided.
In order to solve the technical problems, the invention adopts the technical scheme that:
a preparation method of high-strength flame-retardant waterproof glass wool is characterized by comprising the following specific preparation steps:
(1) putting the cullet, calcite, forsterite, borax and solid products into a planetary ball mill, grinding for 2-3 h under the conditions that the rotating speed is 100-120 r/min and the ball-to-material ratio is 10:1, putting the ground materials into a muffle furnace, filling argon into the muffle furnace, raising the temperature in the muffle furnace to 400-450 ℃, and standing at a constant temperature for 60-80 min;
(2) continuously raising the temperature in the muffle furnace to 1300-1400 ℃, heating at high temperature for 15-20 min to obtain glass liquid, putting the glass liquid into a glass wool centrifuge for centrifugal treatment to obtain a centrifugal product, putting the centrifugal product into a drying box, and drying for 3-4 h at the temperature of 110-120 ℃ to obtain the high-strength flame-retardant waterproof glass wool;
the specific preparation steps of the solid product are as follows:
(1) placing the oxidation reaction liquid in a reaction kettle, filling nitrogen into the reaction kettle to increase the air pressure in the reaction kettle to 0.6-1.0 MPa, increasing the temperature in the reaction kettle to 160-180 ℃, stirring for 30-40 min at the constant temperature and constant pressure by using a stirring device at the rotating speed of 300-400 r/min to prepare a thermal reaction mixed liquid, putting the thermal reaction mixed liquid and a sulfuric acid solution with the mass fraction of 10-20% into a beaker, and stirring for 50-60 min at the rotating speed of 300-500 r/min by using a stirrer to prepare an acidic mixed liquid;
(2) putting the acidic mixed solution and aluminum chloride into a reaction kettle, stirring for 50-60 min at a rotating speed of 500-600 r/min by using a stirrer, standing for 3-4 h after stirring to prepare a mixed dispersion liquid, adding simple substance iron powder into the reaction kettle, stirring for 50-70 min at a rotating speed of 500-600 r/min by using the stirrer, filtering after stirring to obtain filter residues, and cleaning the filter residues for 3-5 times by using distilled water to prepare a solid product;
the oxidation reaction liquid comprises the following specific preparation steps:
(1) putting bagasse and wheat straw into an oven, drying for 3-4 hours at the temperature of 60-70 ℃, putting into a crusher to crush to obtain a mixed material after drying, putting the mixed material and 6-10% by mass of hydrochloric acid into a beaker, stirring for 60-80 min at the rotating speed of 400-500 r/min by using a stirrer, putting the beaker into a microwave oven after stirring, and performing microwave treatment for 10-12 min under the power of 600-800W to obtain mixed slurry;
(2) putting a beaker into an ice water bath kettle, dropwise adding a sodium hydroxide solution with the mass fraction of 10-15% into the beaker to adjust the pH value, raising the water bath temperature to 80-100 ℃, reacting at a constant temperature for 40-50 min to obtain a reaction mixed solution, adding sodium hypochlorite powder into the beaker, and stirring with a stirrer at the rotating speed of 500-600 r/min for 30-40 min to obtain an oxidation reaction solution.
Preferably, the weight parts of the cullet are 82-86 parts, the weight parts of the calcite are 2-4 parts, the weight parts of the forsterite are 3-5 parts, the weight parts of the borax are 8-10 parts, and the weight parts of the solid product are 15-19 parts.
The mass ratio of the thermal reaction mixed solution to the sulfuric acid solution with the mass fraction of 10-20% in the specific preparation step (1) of the solid product is 1: 5.
The mass ratio of the acidic mixed solution to the aluminum chloride in the specific preparation step (2) of the solid product is 50: 1.
The mass of the simple substance iron powder added into the reaction kettle in the specific preparation step (2) of the solid product is 3-5% of the mass of the mixed dispersion liquid.
The specific preparation step (1) of the oxidation reaction solution is that the mass ratio of the bagasse to the wheat straw is 5: 1.
The mass ratio of the mixed material in the step (1) to hydrochloric acid with the mass fraction of 6-10% is 1: 10.
Specifically, in the step (2), a sodium hydroxide solution with the mass fraction of 10-15% is added dropwise into the beaker to adjust the pH value to 11-13.
Specifically preparing the oxidation reaction liquid, wherein the mass of the sodium hypochlorite powder added into the beaker in the step (2) is 2-4% of the mass of the reaction mixture.
The beneficial technical effects of the invention are as follows:
(1) the invention firstly mixes and crushes bagasse and wheat straw, the crushing is mixed with hydrochloric acid and is carried out microwave treatment to prepare mixed serous fluid, then alkali liquor is dripped into the mixed serous fluid to carry out high temperature reaction, sodium hypochlorite is added after the reaction to prepare oxidation reaction liquid, then the oxidation reaction liquid is carried out high temperature and high pressure reaction, sulfuric acid is dripped to prepare acid mixed liquid, then aluminum chloride is added into the acid mixed liquid to be mixed, iron powder is added to react, after the reaction, the solid product is obtained by filtering and washing, finally the solid product, cullet, calcite and other raw materials are mixed and ground, the high temperature treatment is carried out to prepare glass liquid, the glass liquid is treated and dried in a glass cotton centrifuge to obtain the high-strength flame-retardant waterproof glass cotton, the bagasse and the wheat straw are soaked by hydrochloric acid and are treated by high temperature, the fiber components are further decomposed and the carbon chains are broken by high-temperature and high-pressure treatment to generate fiber components with smaller molecular weight and shorter carbon chains, the saccharide components are hydrolyzed to generate micromolecular saccharide organic components, and then sodium hypochlorite is used for carrying out oxidation treatment on the fiber molecules to graft a large number of carboxyl groups on the surfaces of the fibers, so that the bonding effect among the components in the glass cotton is increased by the carboxyl and the saccharide components, the toughness and the mechanical strength of the glass cotton are effectively enhanced by combining the good toughness and the mechanical property of the fibers, the brittleness of the glass cotton is reduced, the impact resistance of the glass cotton is improved, and the durability of the glass cotton is enhanced;
(2) the invention introduces aluminum ions into plant fibers, utilizes carboxyl groups generated by oxidation reaction to form complexation to further enhance the adsorption effect on the aluminum ions, and utilizes iron powder to generate displacement effect on the aluminum ions, thereby generating aluminum simple substance components in the fibers, enhancing the mechanical strength and mechanical property of the fibers to further enhance the mechanical strength of the glass wool, simultaneously dispersing the aluminum simple substance in the glass wool by utilizing the fiber components, generating an aluminum oxide protective film under the condition of high temperature to isolate air, enhancing the flame retardant property of the glass wool, and carrying out carbonization treatment on the fiber components and carbohydrate compounds, forming covalent bonds between the fiber components and the carbohydrate components and surrounding components in the carbonization process, enhancing the bonding degree, improving the compactness of each component in the glass wool before, enhancing the waterproof property and the mechanical strength, and having wide application prospect.
Detailed Description
Putting bagasse and wheat straw into an oven according to a mass ratio of 5:1, drying for 3-4 h at a temperature of 60-70 ℃, crushing in a crusher after drying to obtain a mixed material, putting the mixed material and 6-10% hydrochloric acid according to a mass ratio of 1:10 into a beaker, stirring for 60-80 min at a rotating speed of 400-500 r/min by using a stirrer, putting the beaker into a microwave oven after stirring, and performing microwave treatment for 10-12 min under a power of 600-800W to obtain mixed slurry; placing the beaker in an ice water bath kettle, dropwise adding a sodium hydroxide solution with the mass fraction of 10-15% into the beaker to adjust the pH value to 11-13, raising the water bath temperature to 80-100 ℃, reacting at a constant temperature for 40-50 min to prepare a reaction mixed solution, adding sodium hypochlorite powder with the mass fraction of 2-4% of the reaction mixed solution into the beaker, and stirring with a stirrer at the rotating speed of 500-600 r/min for 30-40 min to prepare an oxidation reaction solution; placing the oxidation reaction liquid into a reaction kettle, filling nitrogen into the reaction kettle to increase the air pressure in the reaction kettle to 0.6-1.0 MPa, increasing the temperature in the reaction kettle to 160-180 ℃, stirring for 30-40 min at a constant temperature and a constant pressure by using a stirring device at a rotating speed of 300-400 r/min to prepare a thermal reaction mixed liquid, putting the thermal reaction mixed liquid and a sulfuric acid solution with a mass fraction of 10-20% into a beaker according to a mass ratio of 1:5, and stirring for 50-60 min at a rotating speed of 300-500 r/min by using a stirrer to prepare an acidic mixed liquid; putting the acidic mixed solution and aluminum chloride into a reaction kettle according to the mass ratio of 50:1, stirring for 50-60 min at the rotating speed of 500-600 r/min by using a stirrer, standing for 3-4 h to prepare a mixed dispersion liquid, adding simple substance iron powder accounting for 3-5% of the mass of the mixed dispersion liquid into the reaction kettle, stirring for 50-70 min at the rotating speed of 500-600 r/min by using the stirrer, filtering to obtain filter residues, and cleaning the filter residues for 3-5 times by using distilled water to prepare a solid product; putting 82-86 parts of cullet, 2-4 parts of calcite, 3-5 parts of forsterite, 8-10 parts of borax and 15-19 parts of the solid product into a planetary ball mill, grinding for 2-3 hours under the conditions that the rotating speed is 100-120 r/min and the ball-to-material ratio is 10:1, putting the ground mixture into a muffle furnace, filling argon into the muffle furnace, raising the temperature in the muffle furnace to 400-450 ℃, and standing for 60-80 minutes at constant temperature; and continuously raising the temperature in the muffle furnace to 1300-1400 ℃, heating at a high temperature for 15-20 min to prepare glass liquid, putting the glass liquid into a glass wool centrifuge for centrifugal treatment to obtain a centrifugal product, putting the centrifugal product into a drying box, and drying for 3-4 h at the temperature of 110-120 ℃ to obtain the high-strength flame-retardant waterproof glass wool.
Example 1
Preparation of mixed slurry:
putting bagasse and wheat straw into an oven according to a mass ratio of 5:1, drying for 3h at 60 ℃, crushing in a crusher after drying to obtain a mixed material, putting the mixed material and 6% hydrochloric acid into a beaker according to a mass ratio of 1:10, stirring for 60min at a rotating speed of 400r/min by using a stirrer, putting the beaker into a microwave oven after stirring, and performing microwave treatment for 10min under the condition that the power is 600W to obtain mixed slurry;
preparation of an oxidation reaction solution:
placing the beaker in an ice water bath kettle, dropwise adding a sodium hydroxide solution with the mass fraction of 10% into the beaker to adjust the pH value to 11, raising the temperature of the water bath to 80 ℃, reacting at a constant temperature for 40min to obtain a reaction mixed solution, adding sodium hypochlorite powder with the mass fraction of 2% of the reaction mixed solution into the beaker, and stirring for 30min at the rotating speed of 500r/min by using a stirrer to obtain an oxidation reaction solution;
preparing an acidic mixed solution:
placing the oxidation reaction liquid in a reaction kettle, filling nitrogen into the reaction kettle to increase the air pressure in the reaction kettle to 0.6MPa, increasing the temperature in the reaction kettle to 160 ℃, stirring for 30min at a constant temperature and a constant pressure by using a stirring device at a rotating speed of 300r/min to prepare a thermal reaction mixed liquid, putting the thermal reaction mixed liquid and a sulfuric acid solution with a mass fraction of 10% into a beaker according to a mass ratio of 1:5, and stirring for 50min at a rotating speed of 300r/min by using a stirrer to prepare an acidic mixed liquid;
preparation of solid product:
putting the acidic mixed solution and aluminum chloride into a reaction kettle according to the mass ratio of 50:1, stirring for 50min at the rotating speed of 500r/min by using a stirrer, standing for 3h after stirring to prepare mixed dispersion liquid, adding simple substance iron powder accounting for 3% of the mass of the mixed dispersion liquid into the reaction kettle, stirring for 50min at the rotating speed of 500r/min by using the stirrer, filtering after stirring to obtain filter residue, and cleaning the filter residue for 3 times by using distilled water to prepare a solid product;
preparing high-strength flame-retardant waterproof glass wool:
putting 82 parts of cullet, 2 parts of calcite, 3 parts of forsterite, 8 parts of borax and 15 parts of the solid product into a planetary ball mill, grinding for 2 hours under the conditions that the rotating speed is 100r/min and the ball-to-material ratio is 10:1, putting the ground mixture into a muffle furnace, filling argon into the muffle furnace, raising the temperature in the muffle furnace to 400 ℃, and standing at a constant temperature for 60 minutes;
and continuously raising the temperature in the muffle furnace to 1300 ℃, heating at high temperature for 15min to obtain glass liquid, putting the glass liquid into a glass wool centrifuge for centrifugal treatment to obtain a centrifugal product, putting the centrifugal product into a drying box, and drying for 3h at the temperature of 110 ℃ to obtain the high-strength flame-retardant waterproof glass wool.
Example 2
Preparation of mixed slurry:
putting bagasse and wheat straw into an oven according to a mass ratio of 5:1, drying for 3.5h at 65 ℃, crushing in a crusher after drying to obtain a mixed material, putting the mixed material and 8% hydrochloric acid into a beaker according to a mass ratio of 1:10, stirring for 70min at a rotating speed of 450r/min by using a stirrer, putting the beaker into a microwave oven after stirring, and performing microwave treatment for 11min under the condition that the power is 700W to obtain mixed slurry;
preparation of an oxidation reaction solution:
placing the beaker in an ice water bath kettle, dropwise adding a sodium hydroxide solution with the mass fraction of 12.5% into the beaker to adjust the pH value to 12, raising the temperature of the water bath to 90 ℃, reacting at a constant temperature for 45min to obtain a reaction mixed solution, adding sodium hypochlorite powder with the mass fraction of 3% of the reaction mixed solution into the beaker, and stirring at the rotating speed of 550r/min for 35min by using a stirrer to obtain an oxidation reaction solution;
preparing an acidic mixed solution:
placing the oxidation reaction liquid in a reaction kettle, filling nitrogen into the reaction kettle to increase the air pressure in the reaction kettle to 0.8MPa, increasing the temperature in the reaction kettle to 170 ℃, stirring for 35min at a constant temperature and a constant pressure by using a stirring device at a rotating speed of 350r/min to prepare a thermal reaction mixed liquid, putting the thermal reaction mixed liquid and a sulfuric acid solution with the mass fraction of 15% into a beaker according to a mass ratio of 1:5, and stirring for 55min at a rotating speed of 400r/min by using a stirrer to prepare an acidic mixed liquid;
preparation of solid product:
putting the acidic mixed solution and aluminum chloride into a reaction kettle according to the mass ratio of 50:1, stirring for 55min at the rotating speed of 550r/min by using a stirrer, standing for 3.5h after stirring to obtain a mixed dispersion liquid, adding simple substance iron powder accounting for 4% of the mass of the mixed dispersion liquid into the reaction kettle, stirring for 60min at the rotating speed of 550r/min by using the stirrer, filtering after stirring to obtain filter residue, and cleaning the filter residue for 4 times by using distilled water to obtain a solid product;
preparing high-strength flame-retardant waterproof glass wool:
putting 84 parts of cullet, 3 parts of calcite, 4 parts of forsterite, 9 parts of borax and 17 parts of the solid product into a planetary ball mill, grinding for 2.5 hours under the conditions that the rotating speed is 110r/min and the ball-to-material ratio is 10:1, putting the ground mixture into a muffle furnace, filling argon into the muffle furnace, raising the temperature in the muffle furnace to 425 ℃, and standing at constant temperature for 70 minutes;
and continuously raising the temperature in the muffle furnace to 1350 ℃, heating at high temperature for 17.5min to obtain glass liquid, putting the glass liquid into a glass wool centrifuge for centrifugal treatment to obtain a centrifugal product, putting the centrifugal product into a drying box, and drying for 3.5h at the temperature of 115 ℃ to obtain the high-strength flame-retardant waterproof glass wool.
Example 3
Preparation of mixed slurry:
putting bagasse and wheat straw into an oven according to a mass ratio of 5:1, drying for 4h at 70 ℃, putting into a crusher after drying, crushing to obtain a mixed material, putting the mixed material and 10% hydrochloric acid into a beaker according to a mass ratio of 1:10, stirring for 80min at a rotating speed of 500r/min by using a stirrer, putting the beaker into a microwave oven after stirring, and performing microwave treatment for 12min under the condition that the power is 800W to obtain mixed slurry;
preparation of an oxidation reaction solution:
placing the beaker in an ice water bath kettle, dropwise adding a sodium hydroxide solution with the mass fraction of 15% into the beaker to adjust the pH value to 13, raising the temperature of the water bath to 100 ℃, reacting at a constant temperature for 50min to obtain a reaction mixed solution, adding sodium hypochlorite powder with the mass fraction of 4% of the reaction mixed solution into the beaker, and stirring at the rotating speed of 600r/min for 40min by using a stirrer to obtain an oxidation reaction solution;
preparing an acidic mixed solution:
placing the oxidation reaction liquid in a reaction kettle, filling nitrogen into the reaction kettle to increase the air pressure in the reaction kettle to 1.0MPa, increasing the temperature in the reaction kettle to 180 ℃, stirring for 40min at a constant temperature and a constant pressure by using a stirring device at a rotating speed of 400r/min to prepare a thermal reaction mixed liquid, putting the thermal reaction mixed liquid and a sulfuric acid solution with the mass fraction of 20% into a beaker according to the mass ratio of 1:5, and stirring for 60min at a rotating speed of 500r/min by using a stirrer to prepare an acidic mixed liquid;
preparation of solid product:
putting the acidic mixed solution and aluminum chloride into a reaction kettle according to the mass ratio of 50:1, stirring for 60min at the rotating speed of 600r/min by using a stirrer, standing for 4h after stirring to prepare mixed dispersion liquid, adding simple substance iron powder accounting for 5% of the mass of the mixed dispersion liquid into the reaction kettle, stirring for 70min at the rotating speed of 600r/min by using the stirrer, filtering after stirring to obtain filter residue, and cleaning the filter residue for 5 times by using distilled water to prepare a solid product;
preparing high-strength flame-retardant waterproof glass wool:
putting 86 parts of cullet, 4 parts of calcite, 5 parts of forsterite, 10 parts of borax and 19 parts of the solid product into a planetary ball mill, grinding for 3 hours under the conditions that the rotating speed is 120r/min and the ball-to-material ratio is 10:1, putting into a muffle furnace after grinding, filling argon into the muffle furnace, raising the temperature in the muffle furnace to 450 ℃, and standing at constant temperature for 80 minutes;
and continuously raising the temperature in the muffle furnace to 1400 ℃, heating at high temperature for 20min to obtain glass liquid, putting the glass liquid into a glass wool centrifuge for centrifugal treatment to obtain a centrifugal product, putting the centrifugal product into a drying box, and drying for 4h at the temperature of 120 ℃ to obtain the high-strength flame-retardant waterproof glass wool.
Comparative example 1 was prepared substantially the same as example 1 except for the lack of an acidic mixture.
Comparative example 2 was prepared essentially the same as example 1 except for the absence of solid product.
Comparative example 3 glass wool from Guangzhou company.
The glass wool of the present invention and the glass wool of the comparative example were respectively subjected to performance tests, and the test results are shown in table 1:
the detection method comprises the following steps:
the compressive strength was measured according to the JC/T978-005 standard.
Notched impact strength: the glass wool prepared in the examples and comparative examples was used to prepare a specimen having a length of 110mm and a width of 10mm, a notch having a V-shape with an angle of 45 DEG and a radius of 0.4mm was placed in the middle of the specimen, and the specimen was tested by a simple beam pendulum impact tester having a pendulum impact energy of 45J, an impact velocity of 3.6m/s and a span of 60mm, and the notch impact strength was measured.
The limiting oxygen index is measured with reference to the standard of GB 206-80.
And (3) testing the waterproofness: the glass wool in the examples and comparative examples was formed into a 150 cm-high cylinder, and water was poured into the cylinder at a height of 100cm, and after 4 hours, it was observed whether or not water leaked from the glass wool sheet.
TABLE 1 measurement results of glass wool Properties
| Test items | Example 1 | Example 2 | Example 3 | Comparative example 1 | Comparative example 2 | Comparative example 3 |
| Compressive strength (MPa) | 45 | 48 | 51 | 33 | 36 | 39 |
| Notched bar impact Strength (MPa) | 36 | 38 | 41 | 23 | 26 | 30 |
| Limiting Oxygen Index (LOI) | 34.78 | 36.45 | 38.56 | 28.67 | 30.12 | 32.24 |
| Water-proof property | Without leakage | Without leakage | Without leakage | Apparent penetration | Slight penetration | Slight penetration |
As can be seen from the table 1, the high-strength flame-retardant waterproof glass wool prepared by the invention has the advantages of high mechanical strength, excellent impact resistance and durability, good flame retardance and waterproof performance, and wide application prospect.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, but rather as the subject matter of the invention is to be construed in all aspects and as broadly as possible, and all changes, equivalents and modifications that fall within the true spirit and scope of the invention are therefore intended to be embraced therein.
Claims (9)
1. A preparation method of high-strength flame-retardant waterproof glass wool is characterized by comprising the following specific preparation steps:
(1) putting the cullet, calcite, forsterite, borax and solid products into a planetary ball mill, grinding for 2-3 h under the conditions that the rotating speed is 100-120 r/min and the ball-to-material ratio is 10:1, putting the ground materials into a muffle furnace, filling argon into the muffle furnace, raising the temperature in the muffle furnace to 400-450 ℃, and standing at a constant temperature for 60-80 min;
(2) continuously raising the temperature in the muffle furnace to 1300-1400 ℃, heating at high temperature for 15-20 min to obtain glass liquid, putting the glass liquid into a glass wool centrifuge for centrifugal treatment to obtain a centrifugal product, putting the centrifugal product into a drying box, and drying for 3-4 h at the temperature of 110-120 ℃ to obtain the high-strength flame-retardant waterproof glass wool;
the specific preparation steps of the solid product are as follows:
(1) placing the oxidation reaction liquid in a reaction kettle, filling nitrogen into the reaction kettle to increase the air pressure in the reaction kettle to 0.6-1.0 MPa, increasing the temperature in the reaction kettle to 160-180 ℃, stirring for 30-40 min at the constant temperature and constant pressure by using a stirring device at the rotating speed of 300-400 r/min to prepare a thermal reaction mixed liquid, putting the thermal reaction mixed liquid and a sulfuric acid solution with the mass fraction of 10-20% into a beaker, and stirring for 50-60 min at the rotating speed of 300-500 r/min by using a stirrer to prepare an acidic mixed liquid;
(2) putting the acidic mixed solution and aluminum chloride into a reaction kettle, stirring for 50-60 min at a rotating speed of 500-600 r/min by using a stirrer, standing for 3-4 h after stirring to prepare a mixed dispersion liquid, adding simple substance iron powder into the reaction kettle, stirring for 50-70 min at a rotating speed of 500-600 r/min by using the stirrer, filtering after stirring to obtain filter residues, and cleaning the filter residues for 3-5 times by using distilled water to prepare a solid product;
the oxidation reaction liquid comprises the following specific preparation steps:
(1) putting bagasse and wheat straw into an oven, drying for 3-4 hours at the temperature of 60-70 ℃, putting into a crusher to crush to obtain a mixed material after drying, putting the mixed material and 6-10% by mass of hydrochloric acid into a beaker, stirring for 60-80 min at the rotating speed of 400-500 r/min by using a stirrer, putting the beaker into a microwave oven after stirring, and performing microwave treatment for 10-12 min under the power of 600-800W to obtain mixed slurry;
(2) putting a beaker into an ice water bath kettle, dropwise adding a sodium hydroxide solution with the mass fraction of 10-15% into the beaker to adjust the pH value, raising the water bath temperature to 80-100 ℃, reacting at a constant temperature for 40-50 min to obtain a reaction mixed solution, adding sodium hypochlorite powder into the beaker, and stirring with a stirrer at the rotating speed of 500-600 r/min for 30-40 min to obtain an oxidation reaction solution.
2. The preparation method of the high-strength flame-retardant waterproof glass wool according to claim 1, characterized in that: preferably, the weight parts of the cullet are 82-86 parts, the weight parts of the calcite are 2-4 parts, the weight parts of the forsterite are 3-5 parts, the weight parts of the borax are 8-10 parts, and the weight parts of the solid product are 15-19 parts.
3. The preparation method of the high-strength flame-retardant waterproof glass wool according to claim 1, characterized in that: the mass ratio of the thermal reaction mixed solution to the sulfuric acid solution with the mass fraction of 10-20% in the specific preparation step (1) of the solid product is 1: 5.
4. The preparation method of the high-strength flame-retardant waterproof glass wool according to claim 1, characterized in that: the mass ratio of the acidic mixed solution to the aluminum chloride in the specific preparation step (2) of the solid product is 50: 1.
5. The preparation method of the high-strength flame-retardant waterproof glass wool according to claim 1, characterized in that: the mass of the simple substance iron powder added into the reaction kettle in the specific preparation step (2) of the solid product is 3-5% of the mass of the mixed dispersion liquid.
6. The preparation method of the high-strength flame-retardant waterproof glass wool according to claim 1, characterized in that: the specific preparation step (1) of the oxidation reaction solution is that the mass ratio of the bagasse to the wheat straw is 5: 1.
7. The preparation method of the high-strength flame-retardant waterproof glass wool according to claim 1, characterized in that: the mass ratio of the mixed material in the step (1) to hydrochloric acid with the mass fraction of 6-10% is 1: 10.
8. The preparation method of the high-strength flame-retardant waterproof glass wool according to claim 1, characterized in that: specifically, in the step (2), a sodium hydroxide solution with the mass fraction of 10-15% is added dropwise into the beaker to adjust the pH value to 11-13.
9. The preparation method of the high-strength flame-retardant waterproof glass wool according to claim 1, characterized in that: specifically preparing the oxidation reaction liquid, wherein the mass of the sodium hypochlorite powder added into the beaker in the step (2) is 2-4% of the mass of the reaction mixture.
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| CN201911354013.8A CN111116046A (en) | 2019-12-25 | 2019-12-25 | Preparation method of high-strength flame-retardant waterproof glass wool |
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| CN201911354013.8A CN111116046A (en) | 2019-12-25 | 2019-12-25 | Preparation method of high-strength flame-retardant waterproof glass wool |
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| CN201911354013.8A Withdrawn CN111116046A (en) | 2019-12-25 | 2019-12-25 | Preparation method of high-strength flame-retardant waterproof glass wool |
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