CN114956866B - Preparation method of low-temperature sintered colored sand - Google Patents
Preparation method of low-temperature sintered colored sand Download PDFInfo
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- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
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- C04B41/45—Coating or impregnating, e.g. injection in masonry, partial coating of green or fired ceramics, organic coating compositions for adhering together two concrete elements
- C04B41/52—Multiple coating or impregnating multiple coating or impregnating with the same composition or with compositions only differing in the concentration of the constituents, is classified as single coating or impregnation
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- 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
- C04B41/00—After-treatment of mortars, concrete, artificial stone or ceramics; Treatment of natural stone
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Abstract
The invention relates to a preparation method of low-temperature sintered colored sand, which specifically comprises the following steps: white or light-colored quartz sand is used as a base material, the surface of the base material is subjected to primary sintering to form a smooth silica gel primer, the silica gel primer contains a high-temperature color developing agent, the color can be developed under the high-temperature sintering condition, then the surface of the silica gel primer is subjected to slurry spraying by adopting a gel-like coloring slurry and then is sintered again, and finally, the color is fixed by a steam method, so that the wear-resistant colored sand with bright color is prepared.
Description
Technical Field
The invention relates to a preparation method of low-temperature sintered colored sand, belonging to the technical field of composite material preparation.
Background
The color sand is divided into natural color sand and artificial color sand, is a common building material, is processed from various natural color ores, has the characteristics of soft color tone, strong stereoscopic impression, simple processing technology and the like, but has the problems of ore source difference and the like, so that products in different batches have larger color difference and less color varieties, and in addition, the natural color sand has the problems of smaller hardness, fragility and the like, and is only suitable for wall bodies, roofs and ground decoration materials with small pressure bearing capacity. The artificial colored sand is mainly obtained by artificially coloring white or light-colored quartz sand, is applied to asphalt tiles of villas in western countries on a large scale, is embedded with a layer of inorganic basalt colored sand particles on the upper surface of the asphalt tiles to achieve the aesthetic effect, and also plays a role in enhancing the weather resistance of roof asphalt tiles.
The first method is to mix organic pigment and quartz sand and dry the mixture; secondly, curing the organic pigment toner on the surface of quartz sand by using resin at the temperature of about 200 ℃; the third method is a high-temperature sintering method, wherein inorganic pigments are sintered on the surface of quartz sand at the high temperature of 1000 ℃, and the pigments and the surface layer of quartz stone undergo chemical solid-phase reaction to generate stable substances such as metal silicate; in the three methods, the color of the first quartz stone is not aging resistant, nor rain wash resistant, and the color is extremely unstable; thirdly, the cost is too high, the energy consumption is too large, and the method is obviously not suitable for being adopted in large quantities; the second one is popular at present, but has the problems of bad color fastness, easy fading under illumination, bad acid and alkali resistance, etc.; particularly, for the colorful sand with bright color, such as the red, yellow or green colorful sand, the preparation is mostly carried out by adopting a high-temperature sintering method, the energy consumption in the preparation process is large, and the prepared color has the problems of large color difference, easy fading under friction and the like.
The patent with the application number of CN201910874835.2 discloses 'high-wear-resistance low-temperature sintered artificial colored sand and a preparation method thereof', and particularly discloses that the artificial colored sand is composed of quartz sand, inorganic pigment and an inner and outer double-layer coating agent, wherein the inner coating agent is a self-made waterborne silicon-based modifier, the outer coating agent is a self-made waterborne aluminum-based modifier, and the artificial colored sand is prepared by coating twice.
Disclosure of Invention
Aiming at the preparation of bright red, yellow or green artificial colored sand, the finally prepared artificial colored sand is bright in color, small in color difference, wear-resistant and not easy to fade under the impact action.
The technical scheme of the invention is as follows:
the invention discloses a preparation method of low-temperature sintering colored sand, which takes white or light-colored quartz sand as a base material, and carries out primary sintering on the surface of the base material to form a smooth silica gel primer, wherein the silica gel primer contains a high-temperature color developing agent and can develop color under the high-temperature sintering condition, then the surface of the silica gel primer is sprayed with gelatinous coloring slurry and then sintered again, and finally, the color is fixed through a steam method, so that the wear-resistant colored sand with bright color is prepared.
Further, the silica gel primer comprises the following raw materials in parts by weight: 40-60 parts of fluorocarbon resin, 10-20 parts of silane coupling agent, 10-20 parts of polyvinylidene fluoride micro powder, 10-15 parts of high-temperature color developing agent, 5-8 parts of titanium dioxide and alumina powder, 1-3 parts of fluorine-containing leveling agent and 1-3 parts of defoaming agent.
Further, the main component of the high-temperature color developing agent is red polyurethane, green polyurethane or yellow polyurethane.
Further, sodium carboxymethyl cellulose and a dispersing agent are also added into the high-temperature color developing agent; the mass ratio of the red polyurethane, the green polyurethane or the yellow polyurethane to the sodium carboxymethyl cellulose is 6 (1-3).
Further, the gelatinous coloring slurry comprises the following raw materials in parts by weight: 24-40 parts of hydrolysable silicide (KH 560), 12-18 parts of inorganic pigment, 5-8 parts of glycol and 5-8 parts of sodium polyacrylate.
Further, the preparation method of the low-temperature sintered colored sand specifically comprises the following steps:
(1) Selecting and screening quartz sand, cleaning with absolute ethyl alcohol, and drying for later use;
(2) Adding fluorocarbon resin into a high-speed stirrer, sequentially adding a silane coupling agent, polyvinylidene fluoride micro powder, a high-temperature color developing agent, titanium dioxide and aluminum oxide powder, a fluorine-containing leveling agent and a defoaming agent, and mixing and stirring for 15-25min at 1200-1500 r/min to prepare a mixed solution A for later use;
(3) Putting the quartz sand processed in the step (1) and the mixed solution A prepared in the step (2) in a rotary roller furnace according to the weight ratio, mixing, drying, sintering at 50-80 ℃ for 30-40min, forming a silica gel primer on the surface of the quartz sand, and forming a primary sintered sample with a ground color because the color developing agent begins to develop the ground color at 50-80 ℃;
(4) Preparation of a gelatinous coloring paste: after hydrolysis reaction is carried out on hydrolyzable silicide (KH 560) to form sol, the sol is subjected to condensation reaction to form a sol-gel system; adding an inorganic colorant, ethylene glycol and sodium polyacrylate to a sol-gel system to form a colored sol-gel composition (gel-like colored paste) for standby;
(5) Spraying, coloring and sintering: adding the colored sol-gel composition prepared in the step (4) into a feeding box of a guniting device, spraying a primary sintered sample with a ground color through the guniting device, calcining the primary sintered sample after the surface of the primary sintered sample forms a uniform coating under the condition of guniting while stirring, and naturally cooling after calcining;
(6) And (3) placing the sample obtained after coloring and sintering in a steam room at the temperature of 45-60 ℃, and performing color fixing treatment through high-temperature steam to obtain a color sand sample.
Further, the weight ratio of the mixed solution A to the quartz sand in the step (3) is 1 (5~8).
Further, the calcination treatment in the step (5) includes four stages of low-temperature heating, medium-temperature heating, high-temperature heating and natural cooling, and the specific steps are as follows:
a1, when the temperature in a soaking furnace is not more than 50 ℃, loading a sample, gradually heating to the temperature of 120-150 ℃, and heating for 10-15min at a low temperature;
a2, heating the sample at a low temperature, heating to 150 to 200 ℃ at a heating speed of not more than 5 ℃/min, and keeping the temperature at the temperature of 150 to 200 ℃ for 10 to 15min;
a3, heating the sample in a medium-temperature period, heating to 200-300 ℃ at a heating speed of not more than 8 ℃/min, and calcining for 30-40min at the temperature;
and A4, after the calcination is finished, gradually reducing the temperature, controlling the temperature of the soaking furnace below 100 ℃, and then naturally cooling to the room temperature.
Further, the interval time of each steam treatment in the high-temperature steam treatment in the step (6) is 30 to 45min, and three fixation processes are realized.
Compared with the prior art, the invention has the following beneficial effects:
1. the invention is used for preparing artificial colored sand with bright colors such as red, yellow or green and the like under the condition of low-temperature sintering, overcomes the problem of higher energy consumption of preparing the colored sand by adopting a high-temperature sintering method at the temperature of more than 500 ℃ in the prior art, and the colored sand with bright colors prepared by low-temperature sintering is difficult to decolor, is wear-resistant and has uniform color.
2. The sintering and coloring process of the colored sand adopts secondary sintering and coloring, the surface of quartz sand is primarily sintered to form a silica gel primer, fluorocarbon resin, silane coupling agent and high-temperature color developing agent are added into the silica gel primer, during sintering, the fluorocarbon resin forms a film on the surface of the quartz sand substrate, the fluorocarbon resin has extremely small atomic radius and stronger electronegativity because the main chain of the fluorocarbon resin is a high-energy C-F bond, the bond energy is as high as 485 kJ/mol, only a small part of the sunlight ultraviolet region can dissociate the C-F bond, and only a small part of the short-wave ultraviolet light of the part can reach the surface of the earth after passing through the atmospheric layer, so the coloring layer added with the fluorocarbon resin mainly plays a role in ultraviolet resistance and can achieve the purpose of aging resistance; the addition of the silane coupling agent can enhance the bonding between the silica gel primer and the base material on one hand, and can enhance the bonding strength between the color paste and the silica gel primer in the subsequent secondary sintering on the other hand, the high-temperature color developing agent can promote the color development to be formed on the base material under the condition of 50 to 80 ℃ in the primary sintering, so that the color tone is established, the color difference and the omission generated in the direct sintering coloring can be reduced by performing the color development on the silica gel primer layer firstly, and the existence of the primer layer can not generate large color difference even if the subsequent color sand surface generates the decoloration; the gel-like coloring slurry is adopted during the second sintering, a coloring layer is formed on the surface of the quartz sand which is sintered to form the silica gel primer layer in a slurry spraying mode, the coloring sol-gel composition is used for coloring, the bonding effect of the gel can be fully exerted, the inorganic pigment can be better adhered to the surface of the quartz sand, the particle falling caused by temperature change in the subsequent sintering process is reduced, and meanwhile, the gel material can form a film in the sintering process of 200-300 ℃ to form secondary coating.
3. According to the invention, different sintering processes are matched with different temperature control methods, the temperature is controlled within 50-80 ℃ during the first sintering, a proper fluorocarbon resin is selected to form a film body on the surface of the quartz sand base layer, the effective and uniform coloring at the later stage can be mainly ensured, the second sintering temperature is controlled within 200-300 ℃, and different heating modes of low temperature, medium temperature and high temperature sections are matched, so that the color fixing effect can be achieved, and the color sand coloring unevenness and particle adhesion caused by rapid temperature change in the sintering process can be avoided.
4. The invention adopts high-temperature steam treatment at the final stage of high-temperature calcination of the colored sand, fixes the color in three steps, assists the coloring layer to form a layer protective film on the surface of the quartz sand, isolates the quartz sand from the air, and prevents the problems of decolorization, color layer cracking and the like again.
Drawings
FIG. 1 is a pictorial view of the colored sand prepared by the present invention.
Detailed Description
The invention is further described in connection with the preferred embodiments, and the endpoints of the ranges disclosed herein and any values are not limited to the precise range or value, and such ranges or values should be understood to encompass values close to those ranges or values; for numerical ranges, each range between its endpoints and individual point values, and each individual point value can be combined with each other to give one or more new numerical ranges, and such numerical ranges should be construed as specifically disclosed herein.
Materials, reagents and the like used in the following examples are commercially available unless otherwise specified;
the experimental procedures in the following examples are conventional unless otherwise specified.
Example 1
A preparation method of low-temperature sintered colored sand takes white quartz sand as a base material, primary sintering is carried out on the surface of the base material to form a smooth silica gel primer, the silica gel primer contains a high-temperature color developing agent, color development can be carried out under the high-temperature sintering condition, then, the surface of the silica gel primer is sprayed with gel-like coloring slurry and then sintered again, and finally, color fixation is carried out through a steam method, so that the wear-resistant colored sand with bright color is prepared.
The preparation method of the low-temperature sintered colored sand comprises the following steps:
(1) Selecting and screening quartz sand, cleaning with absolute ethyl alcohol, and drying for later use;
(2) Preparing a silica gel primer: adding 40 parts of fluorocarbon resin into a high-speed stirrer, sequentially adding 10 parts of silane coupling agent, 10 parts of polyvinylidene fluoride micro powder, 10 parts of high-temperature color developing agent, 5 parts of titanium dioxide and alumina powder, 1 part of fluorine-containing leveling agent and 1 part of defoaming agent, and mixing and stirring at 1200r/min for 25min to prepare a mixed solution A for later use (the raw materials are calculated according to parts by weight); wherein, the main color development component of the high-temperature color developing agent is red polyurethane, green polyurethane or yellow polyurethane; sodium carboxymethyl cellulose and a dispersing agent are also added into the high-temperature color developing agent to be matched with the main color developing components; the mass ratio of the red polyurethane, the green polyurethane or the yellow polyurethane to the sodium carboxymethyl cellulose is 2:1;
(3) Putting the quartz sand obtained by the treatment in the step (1) and the mixed solution A prepared in the step (2) into a rotary roller furnace according to a weight ratio for mixing, wherein the weight ratio of the mixed solution A to the quartz sand is 1:5, sintering at 60 ℃ for 35min after drying, forming a silica gel primer on the surface of the quartz sand, and enabling a color developing agent to show a ground color to form a primary sintered sample with the ground color;
(4) Preparation of a gelatinous coloring paste: after 24 parts of hydrolysable silicide (KH 560) is subjected to hydrolysis reaction to form sol, the sol is subjected to condensation reaction to form a sol-gel system; adding 12 parts of inorganic pigment, 5 parts of ethylene glycol and 8 parts of sodium polyacrylate into a sol-gel system to form a colored sol-gel composition for later use (the raw materials are calculated according to parts by weight);
(5) Spraying, coloring and sintering: adding the colored sol-gel composition prepared in the step (4) into a feeding box of a guniting device, spraying a primary sintered sample with a ground color through the guniting device, calcining the primary sintered sample after the surface of the primary sintered sample forms a uniform coating under the condition of guniting while stirring, and naturally cooling after calcining;
(6) And (3) placing the sample obtained after coloring and sintering in a steam room at the temperature of 45 ℃, wherein the interval time of each steam treatment in high-temperature steam treatment is 45min, realizing three-step color fixation, and finally obtaining the colored sand sample.
Further, the calcination treatment in the step (5) includes four stages of low-temperature heating, medium-temperature heating, high-temperature heating and natural cooling, and the specific steps are as follows:
a1, when the temperature in a soaking furnace is not more than 50 ℃, loading a sample, gradually heating to 120 ℃ and heating for 12min at a low temperature section;
a2, heating the sample at a low-temperature section, heating to 150 ℃ at a heating rate of 5 ℃/min, and keeping the temperature at the temperature of 150 ℃ for 15min;
a3, heating the sample to 200 ℃ at a heating rate of 7 ℃/min after heating in a medium-temperature section, and calcining for 35min at the temperature;
and A4, after the calcination is finished, gradually reducing the temperature, controlling the temperature of the soaking furnace to be below 100 ℃, naturally cooling to room temperature, and taking out the sample prepared after the calcination.
Example 2
White quartz sand is used as a base material, primary sintering is carried out on the surface of the base material to form a smooth silica gel primer, the silica gel primer contains a high-temperature color developing agent, color development can be carried out under the high-temperature sintering condition, then, the surface of the silica gel primer is sprayed with gelatinous coloring slurry and then sintered again, and finally, color fixation is carried out through a steam method, so that the wear-resistant colored sand with bright color is prepared.
The preparation method of the low-temperature sintered colored sand specifically comprises the following steps:
(1) Selecting and screening quartz sand, cleaning by using absolute ethyl alcohol, and drying for later use;
(2) Preparing a silica gel primer: adding 60 parts of fluorocarbon resin into a high-speed stirrer, sequentially adding 20 parts of silane coupling agent, 20 parts of polyvinylidene fluoride micro powder, 15 parts of high-temperature color developing agent, 6 parts of titanium dioxide and alumina powder, 2 parts of fluorine-containing leveling agent and 2 parts of defoaming agent, and mixing and stirring at 1500r/min for 15min to prepare a mixed solution A for later use (the raw materials are calculated according to parts by weight); wherein, the main color development component of the high-temperature color developing agent is red polyurethane, green polyurethane or yellow polyurethane; sodium carboxymethyl cellulose and a dispersant are also added into the high-temperature color developing agent to be matched with the main color developing components; the mass ratio of the red polyurethane, the green polyurethane or the yellow polyurethane to the sodium carboxymethyl cellulose is 6:1;
(3) Putting the quartz sand obtained by the treatment in the step (1) and the mixed solution A prepared in the step (2) into a rotary roller furnace according to a weight ratio for mixing, wherein the weight ratio of the mixed solution A to the quartz sand is 1:8, sintering for 30min at 80 ℃ after drying, forming a silica gel primer on the surface of the quartz sand, and developing a color developing agent to show a background color to form a primary sintered sample with the background color;
(4) Preparation of a gelatinous coloring paste: after 40 parts of hydrolysable silicide (KH 560) is subjected to hydrolysis reaction to form sol, the sol is subjected to condensation reaction to form a sol-gel system; adding 18 parts of inorganic pigment, 8 parts of ethylene glycol and 8 parts of sodium polyacrylate into a sol-gel system to form a colored sol-gel composition for later use (the raw materials are calculated according to parts by weight);
(5) Spraying slurry, coloring and sintering: adding the colored sol-gel composition prepared in the step (4) into a feeding box of a guniting device, spraying a primary sintered sample with a ground color through the guniting device, calcining the primary sintered sample after a uniform coating is formed on the surface of the primary sintered sample under the condition of guniting while stirring, and naturally cooling the calcined sample;
(6) And (3) placing the sample obtained after coloring and sintering in a steam room at the temperature of 60 ℃, wherein the interval time of each steam treatment in high-temperature steam treatment is 30min, realizing three-step color fixation, and finally obtaining the colored sand sample.
Further, the calcination treatment in the step (5) includes four stages of low-temperature heating, medium-temperature heating, high-temperature heating and natural cooling, and the specific steps are as follows:
a1, loading a sample when the temperature in a soaking furnace is not more than 50 ℃, gradually heating to 120 ℃ and heating for 15min in a low-temperature section;
a2, heating the sample to 150 ℃ at a heating rate of 5 ℃/min after heating in a low-temperature section, and preserving heat for 10min in a temperature section of 150 ℃;
a3, heating the sample to 200 ℃ at a heating rate of 7 ℃/min after heating in a medium-temperature section, and calcining for 40min at the temperature;
and A4, after the calcination is finished, gradually reducing the temperature, controlling the temperature of the soaking furnace to be below 100 ℃, naturally cooling to room temperature, and taking out the sample prepared after the calcination.
Example 3
A preparation method of low-temperature sintered colored sand takes white quartz sand as a base material, primary sintering is carried out on the surface of the base material to form a smooth silica gel primer, the silica gel primer contains a high-temperature color developing agent, color development can be carried out under the high-temperature sintering condition, then, the surface of the silica gel primer is sprayed with gel-like coloring slurry and then sintered again, and finally, color fixation is carried out through a steam method, so that the wear-resistant colored sand with bright color is prepared.
The preparation method of the low-temperature sintered colored sand specifically comprises the following steps:
(1) Selecting and screening quartz sand, cleaning with absolute ethyl alcohol, and drying for later use;
(2) Preparing a silica gel primer: adding 50 parts of fluorocarbon resin into a high-speed stirrer, sequentially adding 15 parts of silane coupling agent, 15 parts of polyvinylidene fluoride micro powder, 13 parts of high-temperature color developing agent, 8 parts of titanium dioxide and aluminum oxide powder, 3 parts of fluorine-containing flatting agent and 3 parts of defoaming agent, and mixing and stirring at 1300r/min for 20min to prepare a mixed solution A for later use (the raw materials are calculated according to parts by weight); wherein, the main color development component of the high-temperature color developing agent is red polyurethane, green polyurethane or yellow polyurethane; sodium carboxymethyl cellulose and a dispersing agent are also added into the high-temperature color developing agent to be matched with the main color developing components; the mass ratio of the red polyurethane, the green polyurethane or the yellow polyurethane to the sodium carboxymethyl cellulose is 3:1;
(3) Putting the quartz sand obtained by the treatment in the step (1) and the mixed solution A prepared in the step (2) into a rotary roller furnace according to a weight ratio for mixing, wherein the weight ratio of the mixed solution A to the quartz sand is 1:6, sintering for 40min at 50 ℃ after drying, forming a silica gel primer on the surface of the quartz sand, and enabling a color developing agent to show a ground color to form a primary sintered sample with the ground color;
(4) Preparation of a gelatinous coloring paste: 35 parts of hydrolysable silicide (KH 560) are subjected to hydrolysis reaction to form sol, and then the sol is subjected to condensation reaction to form a sol-gel system; adding 16 parts of inorganic pigment, 6 parts of ethylene glycol and 6 parts of sodium polyacrylate into a sol-gel system to form a colored sol-gel composition for later use (the raw materials are calculated according to parts by weight);
(5) Spraying slurry, coloring and sintering: adding the colored sol-gel composition prepared in the step (4) into a feeding box of a guniting device, spraying a primary sintered sample with a ground color through the guniting device, calcining the primary sintered sample after the surface of the primary sintered sample forms a uniform coating under the condition of guniting while stirring, and naturally cooling after calcining;
(6) And (3) placing the sample obtained after coloring and sintering in a steam room at the temperature of 55 ℃, wherein the interval time of each steam treatment in high-temperature steam treatment is 40min, realizing three-step color fixation, and finally obtaining the colored sand sample.
Further, the calcination treatment in the step (5) includes four stages of low-temperature heating, medium-temperature heating, high-temperature heating and natural cooling, and the specific steps are as follows:
a1, when the temperature in a soaking furnace is not more than 50 ℃, loading a sample, gradually heating to 120 ℃ and heating for 10min at a low temperature section;
a2, heating the sample to 150 ℃ at a heating rate of 5 ℃/min after heating in a low-temperature section, and preserving heat for 14min in a temperature section of 150 ℃;
a3, heating the sample to 200 ℃ at a heating rate of 7 ℃/min after heating in a medium-temperature section, and calcining for 30min at the temperature;
and A4, after the calcination is finished, gradually reducing the temperature, controlling the temperature of the soaking furnace to be below 300 ℃, naturally cooling to room temperature, and taking out the sample prepared after the calcination.
TABLE 1 color sand stability test
The above description is only an embodiment of the present invention, and not intended to limit the scope of the present invention, and all modifications of equivalent structures and equivalent processes, which are made by the present specification, or directly or indirectly applied to other related technical fields, are included in the scope of the present invention.
Claims (5)
1. The preparation method of the low-temperature sintered colored sand is characterized by comprising the following steps:
(1) Selecting and screening quartz sand, cleaning with absolute ethyl alcohol, and drying for later use;
(2) Adding fluorocarbon resin into a high-speed stirrer, sequentially adding a silane coupling agent, polyvinylidene fluoride micro powder, a high-temperature color developing agent, titanium dioxide and aluminum oxide powder, a fluorine-containing leveling agent and an antifoaming agent, and mixing and stirring at 1200-1500r/min for 15-25min to prepare a mixed solution A for later use;
(3) Putting the quartz sand processed in the step (1) and the mixed solution A prepared in the step (2) in a rotary roller furnace according to the weight ratio, mixing, drying, sintering at 50-80 ℃ for 30-40min, forming a silica gel primer on the surface of the quartz sand, and forming a primary sintered sample with a ground color because the color developing agent begins to develop the ground color at 50-80 ℃;
(4) Preparation of a gelatinous coloring paste: after the hydrolysable silicide is subjected to hydrolysis reaction to form sol, the sol is subjected to condensation reaction to form a sol-gel system; adding inorganic pigment, glycol and sodium polyacrylate into the sol-gel system to form gel-like coloring slurry for later use;
(5) Spraying, coloring and sintering: adding the gel-like coloring slurry prepared in the step (4) into a feeding box of a slurry spraying device, spraying a primary sintering sample with a ground color through the slurry spraying device, calcining the primary sintering sample after a uniform coating is formed on the surface of the primary sintering sample under the condition of spraying slurry while stirring, and naturally cooling the calcined primary sintering sample;
(6) Placing the sample obtained after coloring and sintering in a steam room at the temperature of 45-60 ℃, and performing color fixing treatment through high-temperature steam to obtain a color sand sample;
the calcination in the step (5) comprises four stages of low-temperature heating, medium-temperature heating, high-temperature heating and natural cooling, and the method comprises the following specific steps:
a1, when the temperature in a soaking furnace is not more than 50 ℃, loading a sample, gradually heating to the temperature of 120-150 ℃, and heating for 10-15min at a low temperature;
a2, heating the sample at a low temperature section, heating to 150-200 ℃ at a heating speed of not more than 5 ℃/min, and preserving heat for 10-15min at a temperature section of 150-200 ℃;
a3, heating the sample in a medium-temperature period, heating to 200-300 ℃ at a heating speed of not more than 8 ℃/min, and calcining for 30-40min at the temperature;
a4, after the calcination is finished, gradually reducing the temperature, controlling the temperature of the soaking furnace below 100 ℃, and then naturally cooling to room temperature;
in the step (6), the interval time of each steam treatment in the high-temperature steam treatment is 30 to 45min, and three fixation processes are realized;
the main component of the high-temperature color developing agent is red polyurethane, green polyurethane or yellow polyurethane.
2. The method for preparing low-temperature sintered colored sand according to claim 1, wherein the method comprises the following steps: the silica gel primer comprises the following raw materials in parts by weight: 40-60 parts of fluorocarbon resin, 10-20 parts of silane coupling agent, 10-20 parts of polyvinylidene fluoride micro powder, 10-15 parts of high-temperature color developing agent, 5-8 parts of titanium dioxide and alumina powder, 1-3 parts of fluorine-containing leveling agent and 1-3 parts of defoaming agent.
3. The method for preparing low-temperature sintered colored sand according to claim 1, wherein the method comprises the following steps: sodium carboxymethyl cellulose and a dispersing agent are also added into the high-temperature color developing agent; the mass ratio of the red polyurethane, the green polyurethane or the yellow polyurethane to the sodium carboxymethyl cellulose is 6 (1-3).
4. The method for preparing low-temperature sintered colored sand according to claim 1, wherein the method comprises the following steps: the gel-like coloring slurry comprises the following raw materials in parts by weight: 24-40 parts of hydrolysable silicide, 12-18 parts of inorganic pigment, 5-8 parts of glycol and 5-8 parts of sodium polyacrylate.
5. The method for preparing low-temperature sintered colored sand according to claim 1, wherein the method comprises the following steps: the weight ratio of the mixed solution A to the quartz sand in the step (3) is 1 (5~8).
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