CN108585872A - A kind of preparation method of energy-saving floor tile - Google Patents

A kind of preparation method of energy-saving floor tile Download PDF

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CN108585872A
CN108585872A CN201810412203.XA CN201810412203A CN108585872A CN 108585872 A CN108585872 A CN 108585872A CN 201810412203 A CN201810412203 A CN 201810412203A CN 108585872 A CN108585872 A CN 108585872A
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floor tile
temperature
energy
ludox
obtains
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沈春霞
何伟仁
陈可
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Foshan Nine Mo Science And Technology Information Consulting Co Ltd
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Foshan Nine Mo Science And Technology Information Consulting Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/515Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics
    • C04B35/56Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides
    • C04B35/565Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on non-oxide ceramics based on carbides or oxycarbides based on silicon carbide
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    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/63Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
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    • C04CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/63Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
    • C04B35/6303Inorganic additives
    • C04B35/6316Binders based on silicon compounds
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    • C04BLIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
    • C04B35/00Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/622Forming processes; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/626Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B
    • C04B35/63Preparing or treating the powders individually or as batches ; preparing or treating macroscopic reinforcing agents for ceramic products, e.g. fibres; mechanical aspects section B using additives specially adapted for forming the products, e.g.. binder binders
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    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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    • C09K5/00Heat-transfer, heat-exchange or heat-storage materials, e.g. refrigerants; Materials for the production of heat or cold by chemical reactions other than by combustion
    • C09K5/02Materials undergoing a change of physical state when used
    • EFIXED CONSTRUCTIONS
    • E04BUILDING
    • E04FFINISHING WORK ON BUILDINGS, e.g. STAIRS, FLOORS
    • E04F15/00Flooring
    • E04F15/02Flooring or floor layers composed of a number of similar elements
    • E04F15/08Flooring or floor layers composed of a number of similar elements only of stone or stone-like material, e.g. ceramics, concrete; of glass or with a top layer of stone or stone-like material, e.g. ceramics, concrete or glass
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    • C04B2235/32Metal oxides, mixed metal oxides, or oxide-forming salts thereof, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
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    • C04B2235/30Constituents and secondary phases not being of a fibrous nature
    • C04B2235/34Non-metal oxides, non-metal mixed oxides, or salts thereof that form the non-metal oxides upon heating, e.g. carbonates, nitrates, (oxy)hydroxides, chlorides
    • C04B2235/349Clays, e.g. bentonites, smectites such as montmorillonite, vermiculites or kaolines, e.g. illite, talc or sepiolite

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Abstract

The invention discloses a kind of preparation methods of energy-saving floor tile, belong to construction material preparing technical field.Floor tile precast body is after sintering, polyurethane is pyrolyzed to form loose and porous structure, hot phase-change microcapsule in paraffin colloidal sol is distributed in pore structure, and heat-absorbing energy-accumulating can be melted at summer, when weather turns cool, curing exotherm heats up, reduce the electricity consumption of the registers such as room conditioning, floor tile liquid phase is essentially from Ludox in the present invention, gel is dehydrated and particle agglomeration occurs amorphous silica in Ludox first in temperature-rise period, to promote the flowing of powder, diffusion, firing, it can also be reacted with other oxides in matrix when high temperature, silicon carbide aoxidizes at high temperature, its surface generates amorphous state oxide layer, this oxide layer activity is very high, it can be reacted with the impurity in matrix and generate low melting point phase acceleration of sintering, reduce the sintering temperature of floor tile, reduce the energy consumption of production floor tile, it has a extensive future.

Description

A kind of preparation method of energy-saving floor tile
Technical field
The invention discloses a kind of preparation methods of energy-saving floor tile, belong to construction material preparing technical field.
Background technology
A kind of floor decorative material of floor tile, also known as floor tile.It is fired with clay.Specification is a variety of.Matter heavily fortified point, unit weight Small, pressure resistance is wear-resisting, can be moisture-proof.Some has decoration function through glazing treatment.It is chiefly used in the ground of public building and civil buildings And flooring.The kind of floor tile has all-body tile, glazed tile, entire body polishing brick and tile, pattern permeating tile, oozes colored polished bricks etc., these floors Brick is not all anti-skidding, especially there is old man and child in family, has to do anti-skidding test in purchase, in order to avoid go out to ask Topic.Common floor tile has:Full-glazed tile, vitrified tile, polished bricks, matt brick, glazed tile, stamp brick, anti-skid brick, extraordinary acid-proof Brick.
Floor is the indispensable ornament materials of modern house, can be divided into timber floor, bamboo flooring, plastic floor, compoundly Plate etc., timber floor generally layer of transparent paint on the surface thereof, to show the lines of wood, meanwhile, so that timber floor is become smooth, The disadvantage is that can slowly ooze out, be detrimental to health containing chemical substances such as formaldehyde in the colored varnish, not only price is high for plastic floor, The gas being pernicious to people also is easy tod produce when temperature is high, composite floor board generally uses gluing, has containing formaldehyde etc. in glue Evil substance, can slowly release and be detrimental to health.In numerous floor decorative materials, floor tile becomes the head of consumer Choosing.
It is key link that current China, which promotes building energy conservation, Development of Green Building, for example according to local climatic characteristic, is adopted With advanced Building technology and material, system adjustment, maximum limit are carried out to natural causes such as the sound, light, heat that act on building Degree ground reduces the energy consumption of building and heating and refrigeration.With the fast development of society, worldwide energy shortage problem day is increasingly Play, sustainable development view are more rooted in the hearts of the people, it is energy saving oneself by China and global common concern, building is to use energy Rich and influential family, there is nearly 30% energy consumption in the whole world on building, in China, building energy consumption oneself be more than national total energy consumption 1/4, but build, the energy saving temperature controlling temperature poor performance of special floor tile low to the utilization ratio of the energy, and sintering production Plate brick energy consumption is higher, therefore, from the strategy of sustainable development and energy development strategy, how to meet user's comfort level On the basis of, utilization ratio of the building to the energy is improved, preferably utilizes natural energy resources, while reducing to external influence, that is, The problem of building energy conservation.
Therefore, a kind of energy utilization rate is high, energy saving temperature controlling is good floor tile is invented to construction material preparing technical field With positive effect.
Invention content
Present invention mainly solves the technical issues of, for current China's building energy consumption, oneself is more than national total energy consumption 1/4, and be in increasing trend, but, the energy saving temperature controlling poor performance of special floor tile low to the utilization ratio of the energy is built, and The higher defect of sintering production floor tile energy consumption provides a kind of preparation method of energy-saving floor tile.
In order to solve the above-mentioned technical problem, the technical solution adopted in the present invention is:
A kind of preparation method of energy-saving floor tile, it is characterised in that specifically preparation process is:
(1)10~12mL emulsifier op-10s are placed in conical flask, 200~220mL hydrochloric acid is poured into conical flask, it is to be emulsified After agent is completely dissolved, 40~45mL atoleines are added into conical flask, conical flask are placed in water-bath, heat temperature raising, uses Magnetic stirring apparatus emulsifying, obtains oil-in-water emulsion;
(2)Oil-in-water emulsion is transferred in the three-necked flask with blender and constant pressure funnel, blender stirring is started, Non-hydrate sodium metasilicate solution is added dropwise to three-necked flask with constant pressure funnel, is stirred to react 2~3h, cooled to room temperature goes out Material, obtains solidliquid mixture;
(3)Solidliquid mixture vacuum filtration machine is filtered, removal filtrate obtains filtering filter residue, right successively with petroleum ether and warm water After suction filtration residue washing 3~5 times, it is transferred in baking oven, is dried to obtain the i.e. hot phase-change microcapsule of white powder;
(4)It counts, 60~65 parts of carborundum powders, 30~35 parts of schmigels, 10~15 parts of kaolin powder is put into small in parts by weight Batch mixing in type batch mixer, obtains mixed powder, and 8~10 parts of Ludox, 80~100 parts of deionized waters are added into mixed powder, It is uniformly mixed and obtains mixed slurry, the sodium hydroxide solution being added into mixed slurry adjusts pH, and planet ball is transferred to after standing Ball milling in grinding machine, after ball milling, into planetary ball mill n-butanol is added stands defoaming, obtains silicon carbide floor tile slurry;
(5)Polyurethane foam is cut into batten, is immersed in sodium hydroxide solution, heat temperature raising hydrolysis takes out batten and is put into clear water In wash by rubbing with the hands, hot phase-change microcapsule and Ludox are mixed to get paraffin colloidal sol, batten are put into colloidal sol and is impregnated by naturally dry, It is put into after taking-up in air dry oven and obtains floor tile precast body after drying;
(6)Floor tile precast body is put into bar shaped steel die, silicon carbide floor tile slurry is filled into mold, then to mold Mold is put into the heating of high temperature resistance furnace Program by interior addition 10~12g zinc stearate powders vertically, and heat preservation continues to heat up, and protects Temperature is sintered, and is demoulded after cooled to room temperature and is obtained energy-saving floor tile.
Step(1)The mass fraction of the hydrochloric acid is 5%, and temperature is 80~85 DEG C after heat temperature raising, and speed of agitator is 800~1000r/min, emulsifying time are 30~35min.
Step(2)250~the 300r/min of speed of agitator, constant pressure funnel drop rate are 2~3mL/min, Non-hydrate sodium metasilicate liquid quality fraction is 40%.
Step(3)The warm water temperature be 50~55 DEG C, baking oven set temperature be 40~50 DEG C, drying time be 12~ 15h。
Step(4)The mixing time is 5~8min, and Ludox mass fraction is 40%, sodium hydroxide solution quality point Number is 40%, and it is 10.0~10.5 to adjust pH with sodium hydroxide solution, and control corundum ball is 10 ︰ 1, ball with mixed slurry mass ratio The mill rotating speed time is 400~500r/min, and additions n-butanol weight is mixed slurry weight 2%, foam time for 40~ 50min。
Step(5)The batten size is 10mm × 10mm × 50mm, and sodium hydroxide solution mass fraction is 15%, is added Temperature is 60~65 DEG C after heat heating, and hydrolysis time is 40~45min, and the mass fraction of Ludox is 35%, hot phase-change microcapsule It is 1 ︰ 10 with Ludox mixing quality ratio, it is 4~5h that batten, which is put into dip time in colloidal sol, sets air dry oven temperature as 80 ~90 DEG C, drying time is 2~3h.
Step(6)The cavity dimension of the bar shaped steel die is 20mm × 20mm × 100mm, and carbon is filled into mold For SiClx floor tile slurry to the 2/3~3/4 of mold volumes, programmed rate is 2 DEG C/min, after heating temperature be 500~ 600 DEG C, soaking time is 30~45min, and temperature is 1000~1100 DEG C after continuing heating, and the heat preservation sintering time is 3~4h.
The beneficial effects of the invention are as follows:
(1)The present invention by emulsifier op-10 with hydrochloric acid be acidified dissolving after in a heated state emulsifying obtain oil-in-water emulsion, Oil-in-water emulsion and non-hydrate sodium metasilicate solution hybrid reaction, reaction product are dried to obtain hot phase-change microcapsule through being filtered, washed, Carborundum powder, schmigel, kaolin powder are mixed and be put into Ludox, with obtaining silicon carbide through dilution, alkalization, ball milling, defoaming Polyurethane foam batten is put into the paraffin colloidal sol that silica cladding paraffin microcapsule is mixed with Ludox by plate brick slurry It impregnates, be dried to obtain floor tile precast body, floor tile precast body is put into bar shaped steel die, and insert silicon carbide floor tile Slurry, fired to obtain energy-saving floor tile, after sintering, polyurethane is pyrolyzed to form loose and porous structure floor tile precast body, stone Hot phase-change microcapsule in wax colloidal sol is distributed in pore structure, is played closure exit orifice after the sintering of silicon carbide floor tile slurry, is played The effect for improving rate of closed hole, makes the heat-insulating property of floor tile improve, the enclosed construction of hot phase-change microcapsule makes paraffin be not easy to ooze Go out cement plate, and heat-absorbing energy-accumulating can be melted at summer, curing exotherm heats up when weather turns cool, is built compared to regular-type foam The heat storage capacity for building material greatly increases, and the electricity consumption of the registers such as room conditioning is reduced, to improve the energy saving control of floor tile Warm nature energy;
(2)Amorphous silica of the floor tile liquid phase in Ludox, Ludox is in temperature-rise period in the present invention Gel is dehydrated and occurs particle agglomeration first, so that Si-OH keys is become Si-O bonds and closes, generates preliminary densification and be turned into With, so that green body in floor tile sintering procedure is kept some strength and shape in middle low temperature, on the other hand, amorphous silicon di-oxide With very high activity a variety of crystalline state and variant, wherein alpha-quartz, β-quartz, α-can be formed with the variation of saturated vapor pressure Cristobalite, α-tridymite etc. are thermodynamically stable phase, and when saturated vapor pressure reaches certain value, these stable solid phases can be changed into Liquid phase, to promote the flowing, diffusion, firing of powder, when high temperature, can also react with other oxides in matrix, generate eutectic Point eutectic, to play the role of making up gap, promote densification, the intensity height of carborundum, creep resistance are strong, in the base Skeleton is served as, the densification for forming the second phase product is sintered under middle cryogenic conditions, improves Mechanical Properties of Products, silicon carbide It aoxidizes at high temperature, surface generates amorphous state oxide layer, this oxide layer activity is very high, can react life with the impurity in matrix At low melting point phase acceleration of sintering, the sintering temperature of floor tile is reduced, the energy consumption of production floor tile is reduced, has a extensive future.
Specific implementation mode
10~12mL emulsifier op-10s are placed in conical flask, 200~220mL mass fractions are poured into conical flask is 5% hydrochloric acid after to be emulsified dose is completely dissolved, 40~45mL atoleines is added into conical flask, conical flask is placed in water-bath In, 80~85 DEG C are heated to, with magnetic stirring apparatus with rotating speed 30~35min of emulsifying of 800~1000r/min, is obtained To oil-in-water emulsion;Oil-in-water emulsion is transferred in the three-necked flask with blender and constant pressure funnel, stirring is started Device is stirred with the rotating speed of 250~300r/min, is dripped to three-necked flask with the drop rate of 2~3mL/min with constant pressure funnel It is 40% non-hydrate sodium metasilicate solution to add 200mL mass fractions, is stirred to react 2~3h, cooled to room temperature, and discharging obtains Solidliquid mixture;Solidliquid mixture vacuum filtration machine is filtered, removal filtrate obtains filtering filter residue, with petroleum ether and 50~55 DEG C warm water successively to filtering residue washing 3~5 times after, be transferred in the baking oven that set temperature is 40~50 DEG C, dry 12~ 15h obtains the i.e. hot phase-change microcapsule of white powder;It counts in parts by weight, by 60~65 parts of carborundum powders, 30~35 parts of corundum Powder, 10~15 parts of kaolin powder are put into 5~8min of batch mixing in small-sized batch mixer, obtain mixed powder, 8 are added into mixed powder Ludox that~10 parts of mass fractions are 40%, 80~100 parts of deionized waters, are uniformly mixed and obtain mixed slurry, to mixed slurry The middle sodium hydroxide solution that mass fraction is added and is 40%, it is 10.0~10.5 to adjust pH, and planet ball is transferred to after standing 2~3h In grinding machine, control corundum ball is 10 ︰ 1 with mixed slurry mass ratio, and rotational speed of ball-mill is 400~500r/min, 1~2h of ball milling, ball The n-butanol for continuing to be added mixed slurry weight 2% after mill into planetary ball mill stands 40~50min of defoaming, obtains carbon SiClx floor tile slurry;Polyurethane foam is cut into the batten that size is 10mm × 10mm × 50mm, it is 15% to immerse mass fraction Sodium hydroxide solution in, be heated to 60~65 DEG C, hydrolyze 40~45min, take out batten and be put into clear water and washes by rubbing with the hands, it is natural It dries, is that 1 ︰ 10 is mixed to get paraffin colloidal sol in mass ratio by the Ludox that hot phase-change microcapsule and mass fraction are 35%, by sample Item is put into 4~5h of dipping in colloidal sol, is put into after taking-up in the air dry oven that set temperature is 80~90 DEG C and is obtained after dry 2~3h To floor tile precast body;By floor tile precast body be put into cavity dimension be 20mm × 20mm × 100mm bar shaped steel dies in, to In mold fill silicon carbide floor tile slurry to mold volumes 2/3~3/4 when, then into mold add 10~12g stearic acid Mold is put into high temperature resistance furnace by zinc powder vertically, is warming up to 500~600 DEG C with the rate program of 2 DEG C/min, heat preservation 30 ~45min is continuously heating to 1000~1100 DEG C, 3~4h of heat preservation sintering, is demoulded after cooled to room temperature and obtain energy-saving floor Brick.
10mL emulsifier op-10s are placed in conical flask, the hydrochloric acid that 200mL mass fractions are 5% is poured into conical flask, After to be emulsified dose is completely dissolved, 40mL atoleines are added into conical flask, conical flask is placed in water-bath, is heated to 80 DEG C, with magnetic stirring apparatus with the rotating speed emulsifying 30min of 800r/min, obtain oil-in-water emulsion;Oil-in-water emulsion is turned It moves in the three-necked flask with blender and constant pressure funnel, starts blender, stirred with the rotating speed of 250r/min, with perseverance Press dropping funel molten for 40% non-hydrate sodium metasilicate to three-necked flask dropwise addition 200mL mass fractions with the drop rate of 2mL/min Liquid, is stirred to react 2h, cooled to room temperature, and discharging obtains solidliquid mixture;Solidliquid mixture vacuum filtration machine is taken out Filter, removal filtrate obtain filtering filter residue, with petroleum ether and 50 DEG C of warm water successively to filtering residue washing 3 times after, be transferred to and set In the baking oven that constant temperature degree is 40 DEG C, dry 12h obtains the i.e. hot phase-change microcapsule of white powder;It counts in parts by weight, by 60 parts of carbon SiClx powder, 30 parts of schmigels, 10 parts of kaolin powder are put into batch mixing 5min in small-sized batch mixer, mixed powder are obtained, to mixed powder Ludox, the 80 parts of deionized waters that 8 parts of mass fractions are 40% are added in material, is uniformly mixed and obtains mixed slurry, to mixed slurry The middle sodium hydroxide solution that mass fraction is added and is 40%, it is 10.0 to adjust pH, is transferred in planetary ball mill after standing 2h, is controlled Corundum ball processed is 10 ︰ 1, rotational speed of ball-mill 400r/min, ball milling 1h with mixed slurry mass ratio, is continued to planet after ball milling The n-butanol that mixed slurry weight 2% is added in ball mill stands defoaming 40min, obtains silicon carbide floor tile slurry;By poly- ammonia Ester foam is cut into the batten that size is 10mm × 10mm × 50mm, immerses in the sodium hydroxide solution that mass fraction is 15%, heating 60 DEG C are warming up to, 40min is hydrolyzed, taking-up batten, which is put into clear water, to be washed by rubbing with the hands, naturally dry, by hot phase-change microcapsule and mass fraction Ludox for 35% is that 1 ︰ 10 is mixed to get paraffin colloidal sol in mass ratio, and batten is put into colloidal sol and impregnates 4h, is put into after taking-up In the air dry oven that set temperature is 80 DEG C floor tile precast body is obtained after dry 2h;Floor tile precast body is put into die cavity ruler Very little is that silicon carbide floor tile slurry is filled into mold to mold volumes in 20mm × 20mm × 100mm bar shaped steel dies When 2/3, then 10g zinc stearate powders are added into mold, mold is put into high temperature resistance furnace vertically, with the speed of 2 DEG C/min Rate temperature programming keeps the temperature 30min, is continuously heating to 1000 DEG C, heat preservation sintering 3h, is demoulded after cooled to room temperature to 500 DEG C Obtain energy-saving floor tile.
11mL emulsifier op-10s are placed in conical flask, the hydrochloric acid that 210mL mass fractions are 5% is poured into conical flask, After to be emulsified dose is completely dissolved, 42mL atoleines are added into conical flask, conical flask is placed in water-bath, is heated to 82 DEG C, with magnetic stirring apparatus with the rotating speed emulsifying 32min of 900r/min, obtain oil-in-water emulsion;Oil-in-water emulsion is turned It moves in the three-necked flask with blender and constant pressure funnel, starts blender, stirred with the rotating speed of 270r/min, with perseverance Press dropping funel molten for 40% non-hydrate sodium metasilicate to three-necked flask dropwise addition 200mL mass fractions with the drop rate of 2mL/min Liquid, is stirred to react 2.5h, cooled to room temperature, and discharging obtains solidliquid mixture;Solidliquid mixture vacuum filtration machine is taken out Filter, removal filtrate obtain filtering filter residue, with petroleum ether and 52 DEG C of warm water successively to filtering residue washing 4 times after, be transferred to and set In the baking oven that constant temperature degree is 45 DEG C, dry 14h obtains the i.e. hot phase-change microcapsule of white powder;It counts in parts by weight, by 62 parts of carbon SiClx powder, 32 parts of schmigels, 12 parts of kaolin powder are put into batch mixing 7min in small-sized batch mixer, mixed powder are obtained, to mixed powder Ludox, 80~100 parts of deionized waters that 9 parts of mass fractions are 40% are added in material, is uniformly mixed and obtains mixed slurry, to mixed The sodium hydroxide solution for being added that mass fraction is 40% in slurry is closed, it is 10.2 to adjust pH, and planetary ball mill is transferred to after standing 2.5h In machine, corundum ball and mixed slurry mass ratio are controlled for 10 ︰ 1, rotational speed of ball-mill 450r/min, ball milling 1.5h, after ball milling The n-butanol for continuing to be added mixed slurry weight 2% into planetary ball mill stands defoaming 45min, obtains silicon carbide floor tile slurry Material;Polyurethane foam is cut into the batten that size is 10mm × 10mm × 50mm, it is molten to immerse the sodium hydroxide that mass fraction is 15% In liquid, 62 DEG C are heated to, hydrolyzes 42min, taking-up batten, which is put into clear water, to be washed by rubbing with the hands, naturally dry, by hot phase-change microcapsule The Ludox for being 35% with mass fraction is that 1 ︰ 10 is mixed to get paraffin colloidal sol in mass ratio, and batten is put into colloidal sol and is impregnated 4.5h is put into the air dry oven that set temperature is 85 DEG C after taking-up and obtains floor tile precast body after dry 2.5h;By floor It is that silicon carbide floor is filled into mold in 20mm × 20mm × 100mm bar shaped steel dies that brick precast body, which is put into cavity dimension, Brick slurry to mold volumes 2/3 when, then into mold add 11g zinc stearate powders, mold is put into high temperature resistance vertically In stoves, 550 DEG C are warming up to the rate program of 2 DEG C/min, 40min is kept the temperature, is continuously heating to 1050 DEG C, heat preservation sintering 3.5h, Demoulding obtains energy-saving floor tile after cooled to room temperature.
12mL emulsifier op-10s are placed in conical flask, the hydrochloric acid that 220mL mass fractions are 5% is poured into conical flask, After to be emulsified dose is completely dissolved, 45mL atoleines are added into conical flask, conical flask is placed in water-bath, is heated to 85 DEG C, with magnetic stirring apparatus with the rotating speed emulsifying 35min of 1000r/min, obtain oil-in-water emulsion;Oil-in-water emulsion is turned It moves in the three-necked flask with blender and constant pressure funnel, starts blender, stirred with the rotating speed of 300r/min, with perseverance Press dropping funel molten for 40% non-hydrate sodium metasilicate to three-necked flask dropwise addition 200mL mass fractions with the drop rate of 3mL/min Liquid, is stirred to react 3h, cooled to room temperature, and discharging obtains solidliquid mixture;Solidliquid mixture vacuum filtration machine is taken out Filter, removal filtrate obtain filtering filter residue, with petroleum ether and 55 DEG C of warm water successively to filtering residue washing 5 times after, be transferred to and set In the baking oven that constant temperature degree is 50 DEG C, dry 15h obtains the i.e. hot phase-change microcapsule of white powder;It counts in parts by weight, by 65 parts of carbon SiClx powder, 35 parts of schmigels, 15 parts of kaolin powder are put into batch mixing 8min in small-sized batch mixer, mixed powder are obtained, to mixed powder Ludox, the 100 parts of deionized waters that 10 parts of mass fractions are 40% are added in material, is uniformly mixed and obtains mixed slurry, to mixing slurry The sodium hydroxide solution that mass fraction is 40% is added in material, it is 10.5 to adjust pH, is transferred in planetary ball mill after standing 3h, It is 10 ︰ 1, rotational speed of ball-mill 500r/min, ball milling 2h that corundum ball, which is controlled, with mixed slurry mass ratio, is continued to row after ball milling The n-butanol that mixed slurry weight 2% is added in celestial body grinding machine stands defoaming 50min, obtains silicon carbide floor tile slurry;It will gather Urethane foam is cut into the batten that size is 10mm × 10mm × 50mm, immerses in the sodium hydroxide solution that mass fraction is 15%, adds Heat is warming up to 65 DEG C, hydrolyzes 45min, and taking-up batten, which is put into clear water, to be washed by rubbing with the hands, naturally dry, by hot phase-change microcapsule and quality point Number is that 1 ︰ 10 is mixed to get paraffin colloidal sol in mass ratio for 35% Ludox, and batten is put into colloidal sol and impregnates 5h, is put after taking-up Enter in the air dry oven that set temperature is 90 DEG C and obtains floor tile precast body after dry 3h;Floor tile precast body is put into die cavity Size is that silicon carbide floor tile slurry is filled into mold to mold volumes in 20mm × 20mm × 100mm bar shaped steel dies 3/4 when, then into mold add 12g zinc stearate powders, mold is put into high temperature resistance furnace vertically, with 2 DEG C/min's Rate program is warming up to 600 DEG C, keeps the temperature 45min, is continuously heating to 1100 DEG C, heat preservation sintering 4h, is taken off after cooled to room temperature Mould obtains energy-saving floor tile.
The energy-saving floor tile that comparative example is produced with Hebei company is as a comparison case to energy-saving floor tile produced by the present invention Performance detection is carried out with the energy-saving floor tile in comparative example, testing result is as shown in table 1:
Test method:
Bulk density test is detected using bulk density tester;
Compressive resistance test is detected using compressive resistance test machine;
Abrasive size test is detected using abrasive grain machinery instrument, and abrasive size is bigger, and wear-resisting property is higher;
Wear-resisting revolution test method:According to national standards, the floor tile in example 1~3 and comparative example is surveyed with 180 mesh sand paper Examination, every 500 conversion, one, sand paper, measures last wear-resisting revolution;
Two-dimensional electrostatic fields test is detected by GB/T11718-2009 methods;
Temperature control performance is tested:When summer outdoor temperature is at 30~37 DEG C, measure indoor temperature, when winter makes outdoor temperature -7~ At 0 DEG C, indoor temperature is measured.
1 floor tile performance measurement result of table
High according to the energy-saving floor tile intensity produced by the present invention of data among the above, wear-resisting property is good, while also having automatic Adjust room temperature effect, when summer outdoor temperature is at 30~37 DEG C, indoor temperature can be maintained at 20 DEG C hereinafter, for the temperature difference compared with Big winter can also maintain room temperature at 18 DEG C or more, have good temperature control performance, high to the utilization rate of the energy, and low energy consumption, tool Have broad application prospects.

Claims (7)

1. a kind of preparation method of energy-saving floor tile, it is characterised in that specifically preparation process is:
(1)10~12mL emulsifier op-10s are placed in conical flask, 200~220mL hydrochloric acid is poured into conical flask, it is to be emulsified After agent is completely dissolved, 40~45mL atoleines are added into conical flask, conical flask are placed in water-bath, heat temperature raising, uses Magnetic stirring apparatus emulsifying, obtains oil-in-water emulsion;
(2)Oil-in-water emulsion is transferred in the three-necked flask with blender and constant pressure funnel, starts blender and stirs It mixes, non-hydrate sodium metasilicate solution is added dropwise to three-necked flask with constant pressure funnel, is stirred to react 2~3h, cooled to room temperature, Discharging, obtains solidliquid mixture;
(3)Solidliquid mixture vacuum filtration machine is filtered, removal filtrate obtains filtering filter residue, right successively with petroleum ether and warm water After suction filtration residue washing 3~5 times, it is transferred in baking oven, is dried to obtain the i.e. hot phase-change microcapsule of white powder;
(4)It counts, 60~65 parts of carborundum powders, 30~35 parts of schmigels, 10~15 parts of kaolin powder is put into small in parts by weight Batch mixing in type batch mixer, obtains mixed powder, and 8~10 parts of Ludox, 80~100 parts of deionized waters are added into mixed powder, It is uniformly mixed and obtains mixed slurry, the sodium hydroxide solution being added into mixed slurry adjusts pH, and planet ball is transferred to after standing Ball milling in grinding machine, after ball milling, into planetary ball mill n-butanol is added stands defoaming, obtains silicon carbide floor tile slurry;
(5)Polyurethane foam is cut into batten, is immersed in sodium hydroxide solution, heat temperature raising hydrolysis takes out batten and is put into clear water In wash by rubbing with the hands, hot phase-change microcapsule and Ludox are mixed to get paraffin colloidal sol, batten are put into colloidal sol and is impregnated by naturally dry, It is put into after taking-up in air dry oven and obtains floor tile precast body after drying;
(6)Floor tile precast body is put into bar shaped steel die, silicon carbide floor tile slurry is filled into mold, then to mold Mold is put into the heating of high temperature resistance furnace Program by interior addition 10~12g zinc stearate powders vertically, and heat preservation continues to heat up, and protects Temperature is sintered, and is demoulded after cooled to room temperature and is obtained energy-saving floor tile.
2. a kind of preparation method of energy-saving floor tile according to claim 1, it is characterised in that:Step(1)The salt The mass fraction of acid is 5%, and temperature is 80~85 DEG C after heat temperature raising, and speed of agitator is 800~1000r/min, when emulsifying Between be 30~35min.
3. a kind of preparation method of energy-saving floor tile according to claim 1, it is characterised in that:Step(2)Described stirs 250~300r/min of mix rotating speed, constant pressure funnel drop rate are 2~3mL/min, non-hydrate sodium metasilicate liquid quality fraction It is 40%.
4. a kind of preparation method of energy-saving floor tile according to claim 1, it is characterised in that:Step(3)The temperature Coolant-temperature gage is 50~55 DEG C, and baking oven set temperature is 40~50 DEG C, and drying time is 12~15h.
5. a kind of preparation method of energy-saving floor tile according to claim 1, it is characterised in that:Step(4)Described is mixed The material time is 5~8min, and Ludox mass fraction is 40%, and sodium hydroxide solution mass fraction is 40%, uses sodium hydroxide solution It is 10.0~10.5 to adjust pH, and control corundum ball is 10 ︰ 1 with mixed slurry mass ratio, and the rotational speed of ball-mill time is 400~500r/ Min, addition n-butanol weight are mixed slurry weight 2%, and foam time is 40~50min.
6. a kind of preparation method of energy-saving floor tile according to claim 1, it is characterised in that:Step(5)The sample Size is 10mm × 10mm × 50mm, and sodium hydroxide solution mass fraction is 15%, and temperature is 60~65 DEG C after heat temperature raising, Hydrolysis time is 40~45min, and the mass fraction of Ludox is 35%, and hot phase-change microcapsule is 1 ︰ with Ludox mixing quality ratio 10, it is 4~5h that batten, which is put into colloidal sol dip time, set air dry oven temperature as 80~90 DEG C, drying time for 2~ 3h。
7. a kind of preparation method of energy-saving floor tile according to claim 1, it is characterised in that:Step(6)The item The cavity dimension of shape steel die is 20mm × 20mm × 100mm, and silicon carbide floor tile slurry to mold is filled into mold and is held Long-pending 2/3~3/4, programmed rate be 2 DEG C/min, after heating temperature be 500~600 DEG C, soaking time be 30~ 45min, temperature is 1000~1100 DEG C after continuing heating, and the heat preservation sintering time is 3~4h.
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Application publication date: 20180928