CN109824265B - Preparation method of environment-friendly lead-free cadmium red glass and product prepared by preparation method - Google Patents
Preparation method of environment-friendly lead-free cadmium red glass and product prepared by preparation method Download PDFInfo
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Abstract
The invention discloses a preparation method of environment-friendly lead-free cadmium red glass, which takes basic components and stable coloring agents as raw materials; firstly, uniformly mixing a stable colorant with sodium silicate water glass, carrying out low-temperature pretreatment, and then uniformly mixing with a basic component to obtain a mixed raw material; after the mixed raw materials are heated and melted to form a melt, cooling, forming and naturally cooling to room temperature to obtain base glass; and carrying out secondary color development treatment on the base glass through calcination to obtain the environment-friendly lead-free cadmium-free red glass. In addition, the product prepared by the preparation method of the environment-friendly lead-free cadmium red glass is also disclosed. The preparation method is simple and easy to implement, the process is stable and reliable, the problems of complex melting process and unstable color generation in the prior art are effectively solved, and the obtained product has good visible light transmittance and can be widely applied to a plurality of fields such as building materials, artistic decoration, optical application and the like.
Description
Technical Field
The invention relates to the technical field of glass materials, in particular to a preparation method of environment-friendly lead-free cadmium red glass suitable for the fields of building materials, artistic decoration, optical application and the like and a product prepared by the method.
Background
Red is the color of festive celebration, and the red glass is not only commonly used for building materials and optical application, but also used in the fields of art decoration, jewelry necklace products, ruby imitation and the like at present, and has very wide application prospect and market potential. However, as people pay more attention to environmental protection, the materials, components and production processes of the traditional red glass are more and more concerned. It is known that in order to obtain bright red glass, it is necessary to add colorants to the components of the glass to achieve a stable coloration of the glass. Common red glass on the market at present comprises selenium red glass, gold red glass, copper red glass, lead red glass and antimony red glass. The production technology of the selenium red glass is quite mature and is most widely applied, the used colorant is cadmium sulfoselenide, cadmium is a heavy metal element, the environment is easily polluted in the glass preparation process, and meanwhile, partial ions are dissolved out in the use process of the cadmium red glass to cause the human bodyPotential hazards. The existing research shows that cadmium poisoning can cause nausea, salivation, vomiting, abdominal pain and diarrhea, and further cause central nervous poisoning symptoms, so that the cadmium poisoning is an excellent cause of 'pain diseases' which cannot be cured, severe people can die due to collapse, the American poisonous substance and disease registration administration lists cadmium as a 7 th substance harmful to human health, and cadmium is one of key monitoring indexes for implementing total emission control in China. Gold red glass is also a common type of large red glass, however, it requires the use of lead to dissolve gold to color the glass and the introduction of SnO when using soda-lime glass to dissolve gold2The required additives, namely lead and tin, are heavy metal elements, and the production cost is high due to the introduction of noble metals in the composition of the gold red glass, so that the method is limited in practical production. The production process conditions of the copper red glass are very strict, the reduction atmosphere is needed to ensure that the valence state of copper ions is not changed, and simultaneously, the glass is difficult to clarify due to higher acid composition and high viscosity of glass melt in the component. Lead red glass is relatively easy to prepare because lead can increase the refractive index of the glass and reduce the melting temperature, but the pollution problem of heavy metal elements cannot be avoided all the time. Antimony oxide is used as a coloring agent of the antimony red glass, although antimony is also one of heavy metal elements and has certain toxicity, the toxicity is much lower than that of heavy metal ions such as cadmium and lead, and related regulations do not exist at present to limit the use of antimony, so that the antimony oxide is used as the coloring agent to prepare the bright red glass material, and the bright red glass material has a very wide prospect.
In China, the research on antimony red glass is less, and CN101381202A discloses a preparation process of antimony red glass, because sulfur and carbon are added in the composition, in order to prevent oxidation loss, feeding is needed at a high temperature of more than 1400 ℃, so that molten glass is quickly formed on the surface of mixed materials in a crucible so as to seal the sulfur and the carbon under the molten glass, the method is not only unfavorable for operation, but also dust loss is easily caused by feeding at a high temperature, so that the color development effect of glass of samples prepared in different batches is greatly different. In addition, Guomeowei and the like take sulfur powder and metal antimony powder as coloring agents, carbon powder as reducing agents and sodium chloride and sodium fluosilicate as clarifying agents to prepare antimony red glass; the Sunwachi and the like take a mixture of antimony oxide, sulfur powder and carbon powder as a coloring agent, and obtain red glass through high-temperature melting and low-temperature color development treatment; wang Riyao and the like prepare red glass by using antimony oxide, sulfur, a carbon colorant and copper oxide as a stabilizer. However, the method adopted by the above prior art is not only complicated in melting process, but also difficult to ensure color stability due to no effective anti-oxidation measures taken for the colorant, and thus difficult to reasonably evaluate the color, therefore, no data on the chromaticity value of the color itself is given for the prepared glass product, and the evaluation description is only limited to the visible light transmittance.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a preparation method of environment-friendly lead-free cadmium red glass, which effectively solves the problems of complex melting process and unstable color generation of antimony red glass in the prior art by carrying out low-temperature pretreatment on a colorant. The invention also aims to provide a product prepared by the preparation method of the environment-friendly lead-free cadmium red glass.
The purpose of the invention is realized by the following technical scheme:
the invention provides a preparation method of environment-friendly lead-free cadmium red glass, which comprises the following steps:
(1) pretreatment of stabilized colorants
The composition of the stable colorant according to the mass part is Sb2O3 1-3 parts of S, 0.1-2.0 parts of C and 0.01-0.27 part of CuO; uniformly mixing the stable colorant with sodium silicate water glass to form a semi-solid mixture, drying at the temperature of 80-150 ℃, crushing, and sieving to obtain a pretreated stable colorant;
(2) preparation of Mixed raw materials
The basic components are SiO according to the mass portion2 41-53 parts of Na2CO3 19 to 27 parts of K2CO3 7 to 13 parts of CaCO3 7 to 13 parts by weight of H3BO3 1-5 parts; uniformly mixing the basic component and the pretreated stable colorant, sieving,obtaining a mixed raw material;
(3) preparation of base glass
Melting the mixed raw materials by heating to form a melt, then removing bubbles in the melt by cooling, and obtaining transparent and light yellow basic glass by molding and naturally cooling to room temperature;
(4) preparation of Red glass
And (3) calcining the base glass for secondary color development treatment to obtain the environment-friendly lead-free cadmium-free red glass.
Further, in the step (1), the mass ratio of the stable colorant to the sodium silicate water glass is 1: 7-13.
Further, in the step (3), the mixed raw materials are melted at the temperature of 1420-1550 ℃ and are subjected to heat preservation for 1-2 hours; cooling the melt to 1350-1450 ℃, and preserving heat for 0.5-1 h to remove bubbles in the melt; and pouring the melt after the bubbles are removed into a mold at 500-620 ℃, and preserving heat for 2-4 h for molding.
Further, in the preparation method, in the step (4), the calcination is carried out at the temperature of 600-750 ℃, and the heat preservation is carried out for 0.5-1.5 h.
The product prepared by the preparation method of the environment-friendly lead-free cadmium red glass has the chromatic value L of 24.03-39.02, a of 1.65-17.01, b of 0.37-15.40, and the cut-off wavelength in the ultraviolet visible light interval of 550-650 nm.
The invention has the following beneficial effects:
(1) the invention mixes the key raw materials which play a color role on the glass with the liquid sodium silicate water glass under the condition of room temperature through the pretreatment of the colorant, and realizes the full wrapping of the amorphous sodium silicate to the raw materials of the colorant after the water in the water glass is removed in the low-temperature drying process. The sodium silicate can isolate the contact between the colorant and oxygen in the air, so that the colorant is prevented from being oxidized at high temperature, the content of the colorant in the glass composition is stable, and a key guarantee is provided for the stable coloring of the lead-free and cadmium-free bright red glass.
(2) Due to the coloring of the antimony red glassThe principle is that antimony oxide and sulfur form Sb at high temperature2S3The color is formed by colloid particles, so that the stable color formation of the glass is realized by firstly ensuring Sb in a glass network structure3+And S2-The ions can be bound by diffusion under high temperature conditions. In the invention, because the colorant is separately and uniformly mixed in advance and is added into the glass basic component after being pretreated, compared with the prior art that the antimony oxide and the sulfur powder in the colorant are directly mixed with the glass basic component, the Sb in the invention3+And S2-The ions all have shorter diffusion distances, so that Sb is more favored2S3The colloidal particles are generated efficiently, so that the color generation of the glass is remarkably promoted, and the product has bright red characteristics.
(3) The preparation method is simple and easy to implement, the process is stable and reliable, the problems of complex melting process and unstable color generation of the antimony red glass in the prior art are effectively solved, and the obtained product has good visible light transmittance and can be widely applied to a plurality of fields such as building materials, artistic decoration, optical application and the like.
The present invention will be described in further detail with reference to examples.
Detailed Description
The first embodiment is as follows:
the preparation method of the environment-friendly lead-free cadmium red glass comprises the following steps:
(1) pretreatment of stabilized colorants
The composition of the stable colorant according to the mass part is Sb2O3 1.50 parts of S2.63 parts of C0.38 part of CuO 0.011 part; after the stable colorant is uniformly mixed, the stable colorant and sodium silicate water glass are uniformly mixed to form a semi-solid mixture according to the mass ratio of 1: 9; then placing the mixture in a low-temperature oven at 90 ℃ for drying until the weight is constant, and sieving the crushed mixture through a standard sieve of 200 meshes to obtain a pretreated stable colorant;
(2) preparation of Mixed raw materials
The basic components are SiO according to the mass portion2 48.81 parts、Na2CO3 22.72 parts of K2CO3 11.08 parts of CaCO3 10.84 parts of H3BO32.02 parts; mixing the basic components, uniformly mixing the basic components with the pretreated stable colorant, and sieving the mixture through a 80-mesh standard sieve to obtain a mixed raw material;
(3) preparation of base glass
Melting the mixed raw materials at 1430 ℃ to form a melt, preserving heat for 2h to promote melt homogenization, then cooling to 1370 ℃ and preserving heat for 1h to remove bubbles in the melt, pouring into a mold at 530 ℃ for molding, preserving heat for 3h to release thermal stress in the melt, and then naturally cooling to room temperature to obtain transparent light yellow base glass;
(4) preparation of Red glass
Calcining the basic glass at the temperature of 630 ℃ and preserving heat for 1h for secondary color development treatment to form Sb in situ in the glass2S3Colloid particles, so that the glass is changed from light yellow to bright red, and the environment-friendly lead-free cadmium red glass is obtained.
The environment-friendly lead-free cadmium-free red glass prepared by the embodiment has bright red characteristics, and the colorimetric values L are 27.61, a are 6.57 and b are 3.39; the cut-off wavelength in the UV-visible region is 610 nm.
Example two:
the preparation method of the environment-friendly lead-free cadmium red glass comprises the following steps:
(1) pretreatment of stabilized colorants
The composition of the stable colorant according to the mass part is Sb2O3 2.51 parts of S2.27 parts of C0.46 part of CuO 0.015 part; after the stable colorant is uniformly mixed, the stable colorant and sodium silicate water glass are uniformly mixed to form a semi-solid mixture according to the mass ratio of 1: 11; then placing the mixture in a low-temperature oven at 130 ℃ for drying until the weight is constant, and sieving the crushed mixture through a standard sieve of 200 meshes to obtain a pretreated stable colorant;
(2) preparation of Mixed raw materials
The basic components are SiO according to the mass portion2 46.45 parts of Na2CO3 20.61 parts of K2CO3 12.07 parts of CaCO3 12.56 parts by weight, H3BO33.05 parts of a mixture; mixing the basic components, uniformly mixing the basic components with the pretreated stable colorant, and sieving the mixture through a 80-mesh standard sieve to obtain a mixed raw material;
(3) preparation of base glass
Melting the mixed raw materials at 1450 ℃ to form a melt, preserving heat for 1h to promote melt homogenization, then cooling to 1390 ℃ and preserving heat for 0.5h to remove bubbles in the melt, pouring the melt into a 550 ℃ mold for molding, preserving heat for 2.5h to release thermal stress in the melt, and naturally cooling to room temperature to obtain transparent yellowish base glass;
(4) preparation of Red glass
Calcining the basic glass at the temperature of 650 ℃ and preserving heat for 1.5h for secondary color development treatment to form Sb in situ in the glass2S3Colloid particles, so that the glass is changed from light yellow to bright red, and the environment-friendly lead-free cadmium red glass is obtained.
The environment-friendly lead-free cadmium-free red glass prepared by the embodiment has bright red characteristics, and the colorimetric values L are 22.71, a are 7.93 and b are 1.65; the cut-off wavelength in the UV-visible region is 560 nm.
Example three:
the preparation method of the environment-friendly lead-free cadmium red glass comprises the following steps:
(1) pretreatment of stabilized colorants
The composition of the stable colorant according to the mass part is Sb2O3 1.77 parts of S, 1.95 parts of C, 1.07 parts of CuO and 0.015 part of CuO; after the stable colorant is uniformly mixed, the stable colorant and sodium silicate water glass are uniformly mixed to form a semi-solid mixture according to the mass ratio of 1: 13; then placing the mixture in a low-temperature oven at 150 ℃ for drying until the weight is constant, and sieving the crushed mixture through a standard sieve of 200 meshes to obtain a pretreated stable colorant;
(2) preparation of Mixed raw materials
The basic components are SiO according to the mass portion2 49.22 parts of Na2CO3 24.71 parts of K2CO3 9.67 parts of CaCO3 8.93 parts of H3BO32.67 parts; mixing the basic components, uniformly mixing the basic components with the pretreated stable colorant, and sieving the mixture through a 80-mesh standard sieve to obtain a mixed raw material;
(3) preparation of base glass
Melting the mixed raw materials at 1490 ℃ to form a melt, preserving heat for 1.5h to promote melt homogenization, then cooling to 1420 ℃, preserving heat for 1h to remove bubbles in the melt, pouring into a 570 ℃ mold for molding, preserving heat for 2h to release thermal stress in the melt, and naturally cooling to room temperature to obtain transparent yellowish base glass;
(4) preparation of Red glass
Calcining the basic glass at the temperature of 690 ℃, and preserving heat for 1h for secondary color development treatment to form Sb in situ in the glass2S3Colloid particles, so that the glass is changed from light yellow to bright red, and the environment-friendly lead-free cadmium red glass is obtained.
The environment-friendly lead-free cadmium-free red glass prepared by the embodiment has bright red characteristics, and the colorimetric values L are 27.36, a are 5.71 and b are 3.67; the cut-off wavelength in the UV-visible region is 620 nm.
Example four:
the preparation method of the environment-friendly lead-free cadmium red glass comprises the following steps:
(1) pretreatment of stabilized colorants
The composition of the stable colorant according to the mass part is Sb2O3 2.17 parts of S2.06 parts of C1.33 parts of CuO 0.012 part; after the stable colorant is uniformly mixed, the stable colorant and sodium silicate water glass are uniformly mixed to form a semi-solid mixture according to the mass ratio of 1: 7.5; then placing the mixture in a low-temperature oven at 100 ℃ for drying until the weight is constant, and crushing the mixtureA 200-mesh standard sieve is used for obtaining the pretreated stable colorant;
(2) preparation of Mixed raw materials
The basic components are SiO according to the mass portion2 50.33 parts of Na2CO3 19.42 parts of K2CO3 10.66 parts of CaCO3 9.97 parts of hydrogen and H3BO34.05 parts of a mixture; mixing the basic components, uniformly mixing the basic components with the pretreated stable colorant, and sieving the mixture through a 80-mesh standard sieve to obtain a mixed raw material;
(3) preparation of base glass
Melting the mixed raw materials at 1520 ℃ to form a melt, preserving heat for 1h to promote melt homogenization, then cooling to 1450 ℃, preserving heat for 0.5h to remove bubbles in the melt, pouring into a mold at 590 ℃ for molding, preserving heat for 2h to release thermal stress in the melt, and naturally cooling to room temperature to obtain transparent yellowish base glass;
(4) preparation of Red glass
Calcining the basic glass at the temperature of 710 ℃ and preserving heat for 1.5h for secondary color development treatment to form Sb in situ in the glass2S3Colloid particles, so that the glass is changed from light yellow to bright red, and the environment-friendly lead-free cadmium red glass is obtained.
The environment-friendly lead-free cadmium-free red glass prepared by the embodiment has bright red characteristics, wherein the colorimetric values L are 36.71, a are 15.93 and b are 0.61; the cut-off wavelength in the UV-visible region is 580 nm.
Example five:
the preparation method of the environment-friendly lead-free cadmium red glass comprises the following steps:
(1) pretreatment of stabilized colorants
The composition of the stable colorant according to the mass part is Sb2O3 2.19 parts of S, 1.97 parts of C2.0 parts of CuO 0.01 part; mixing the above stable colorant uniformly, mixing with sodium silicate water glass at mass ratio of 1: 12 to form semi-solid mixtureA body; then placing the mixture in a low-temperature oven at 130 ℃ for drying until the weight is constant, and sieving the crushed mixture through a standard sieve of 200 meshes to obtain a pretreated stable colorant;
(2) preparation of Mixed raw materials
The basic components are SiO according to the mass portion2 47.27 parts of Na2CO3 20.02 parts of K2CO3 12.63 parts of CaCO3 10.21 parts of, H3BO33.67 parts; mixing the basic components, uniformly mixing the basic components with the pretreated stable colorant, and sieving the mixture through a 80-mesh standard sieve to obtain a mixed raw material;
(3) preparation of base glass
Melting the mixed raw materials at 1460 ℃ to form a melt, preserving heat for 2h to promote melt homogenization, then cooling to 1400 ℃, preserving heat for 1h to remove bubbles in the melt, pouring into a 550 ℃ mold for molding, preserving heat for 2h to release thermal stress in the melt, and naturally cooling to room temperature to obtain transparent yellowish base glass;
(4) preparation of Red glass
Calcining the basic glass at 660 ℃ and preserving heat for 1h for secondary color development treatment to form Sb in situ in the glass2S3Colloid particles, so that the glass is changed from light yellow to bright red, and the environment-friendly lead-free cadmium red glass is obtained.
The environment-friendly lead-free cadmium-free red glass prepared by the embodiment has bright red characteristics, wherein the colorimetric values L are 29.67, a are 8.69 and b are 7.35; the cut-off wavelength in the UV-visible region is 610 nm.
Claims (8)
1. The preparation method of the environment-friendly lead-free cadmium red glass is characterized by comprising the following steps:
(1) pretreatment of stabilized colorants
The composition of the stable colorant according to the mass part is Sb2O31-3 parts of S, 0.1-2.0 parts of C and 0.01-0.27 part of CuO; uniformly mixing the stable colorant and sodium silicate water glass to form semi-solid mixtureCombining, drying at the temperature of 80-150 ℃, crushing and sieving to obtain a pretreated stable colorant;
(2) preparation of Mixed raw materials
The basic components are SiO according to the mass portion241-53 parts of Na2CO319 to 27 parts of K2CO37 to 13 parts of CaCO37 to 13 parts by weight of H3BO31-5 parts; uniformly mixing the basic component and the pretreated stable colorant, and sieving to obtain a mixed raw material;
(3) preparation of base glass
Melting the mixed raw materials by heating to form a melt, then removing bubbles in the melt by cooling, and obtaining transparent and light yellow basic glass by molding and naturally cooling to room temperature;
(4) preparation of Red glass
And (3) calcining the base glass for secondary color development treatment to obtain the environment-friendly lead-free cadmium-free red glass.
2. The method for preparing the environment-friendly lead-free cadmium red glass according to claim 1, which is characterized in that: and (2) stabilizing the colorant and sodium silicate water glass according to the mass ratio of 1: 7-13 in the step (1).
3. The method for preparing the environment-friendly lead-free cadmium red glass according to claim 1, which is characterized in that: and (4) melting the mixed raw materials in the step (3) at the temperature of 1420-1550 ℃, and preserving heat for 1-2 hours.
4. The method for preparing the environment-friendly lead-free cadmium red glass according to claim 1 or 3, which is characterized in that: and (4) cooling the melt in the step (3) to 1350-1450 ℃, and preserving heat for 0.5-1 h to remove bubbles in the melt.
5. The method for preparing the environment-friendly lead-free cadmium red glass according to claim 1, which is characterized in that: and (4) pouring the melt with the bubbles removed in the step (3) into a mold at 500-620 ℃, and preserving heat for 2-4 h for molding.
6. The method for preparing the environment-friendly lead-free cadmium red glass according to claim 1, which is characterized in that: calcining at the temperature of 600-750 ℃ in the step (4), and preserving heat for 0.5-1.5 h.
7. A product obtained by the method for preparing the environment-friendly lead-free cadmium red glass as claimed in any one of claims 1 to 6.
8. The product prepared by the method for preparing the environment-friendly lead-free cadmium red glass according to claim 7 is characterized in that: the lead-free cadmium-free antimony red glass product has a chromatic value L of 24.03-39.02, a of 1.65-17.01, b of 0.37-15.40, and a cut-off wavelength of 550-650 nm in an ultraviolet-visible light interval.
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