CN110156316B - Low-temperature coloring agent for glass decoration - Google Patents
Low-temperature coloring agent for glass decoration Download PDFInfo
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- CN110156316B CN110156316B CN201910448989.5A CN201910448989A CN110156316B CN 110156316 B CN110156316 B CN 110156316B CN 201910448989 A CN201910448989 A CN 201910448989A CN 110156316 B CN110156316 B CN 110156316B
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- C—CHEMISTRY; METALLURGY
- C03—GLASS; MINERAL OR SLAG WOOL
- C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
- C03C1/00—Ingredients generally applicable to manufacture of glasses, glazes, or vitreous enamels
- C03C1/04—Opacifiers, e.g. fluorides or phosphates; Pigments
Abstract
The invention discloses a low-temperature coloring agent for glass decoration, which comprises the following components in parts by weight: 8-12 parts of silicon dioxide, 13-14 parts of zinc oxide, 26-28 parts of borax, 15-18 parts of sodium carbonate, 0.81-0.83 part of talcum powder, 1.3-1.6 parts of aluminum oxide and 15-20 parts of load ferrochrome pigment. According to the invention, chromium ions are directly loaded on the silicon dioxide base material, and a layer of ferric oxide is coated on the surface of the chromium ions, so that the prepared colorant can realize a dark reddish brown coloring effect, and the loading base material and the ferric oxide directly fix the chromium ions, so that the problem that heavy metal ions in glass are slowly dissolved out after the glass is corroded can be effectively prevented, and particularly, when a glass product is used for preparing tableware, the glass product is extremely harmful to a human body.
Description
Technical Field
The invention belongs to the field of colored glass preparation, and relates to a low-temperature coloring agent for glass decoration.
Background
The color glass can absorb, reflect and transmit light with different wavelengths to present different colors, is used for various glass ornaments, has the characteristics of attractive appearance and luxuriance, is popular among people, and is generally added with a colorant in the glass preparation process in the prior art, so that the prepared glass has the color of the colorant through the melting and mixing of the colorant and glass raw materials, and further has different colors.
The invention patent with application number CN201710886824.7 discloses a black colorant for low-temperature color glass, a preparation method and a use method thereof, the low-temperature colorant is prepared by compounding quartz powder, borax, sodium carbonate, a coloring additive and other auxiliary raw materials, the coloring additive uses one or more of cobalt oxide, nickel oxide, chromium oxide and iron oxide, but hexavalent chromium is carcinogenic and toxic and easily causes skin diseases, respiratory system diseases and immune system diseases, the prepared glass directly uses the chromium oxide, so that the chromium is directly distributed in the glass and on the surface of the glass, heavy metal ions in the glass are slowly dissolved out after the glass is corroded with long-term use, and particularly when a glass product is used for preparing tableware, the damage to a human body is very large.
Disclosure of Invention
The invention aims to provide a low-temperature coloring agent for glass decoration, which can realize a dark reddish brown coloring effect by directly loading chromium ions on a silicon dioxide base material and coating a layer of ferric oxide on the surfaces of the chromium ions, and can effectively prevent heavy metal ions in glass from being slowly dissolved out after the glass is corroded, and particularly solve the problem of great harm to human bodies when glass products are used for preparing tableware.
The purpose of the invention can be realized by the following technical scheme:
the low-temperature coloring agent for glass decoration comprises the following components in parts by weight:
8-12 parts of silicon dioxide, 13-14 parts of zinc oxide, 26-28 parts of borax, 15-18 parts of sodium carbonate, 0.81-0.83 part of talcum powder, 1.3-1.6 parts of aluminum oxide and 15-20 parts of load ferrochrome pigment;
the specific preparation process of the supported ferrochrome pigment is as follows:
step 1: adding a certain amount of ammonia water and absolute ethyl alcohol into water, adding TEOS after uniformly mixing, then stirring and reacting for 2-3h, then centrifuging through a centrifuge to collect a precipitate, drying the collected precipitate to obtain nano-silica, then adding the obtained nano-silica into the water, simultaneously adding sodium hydroxide, stirring and reacting for 20-22h, then centrifuging to obtain a precipitate, washing the precipitate with distilled water and absolute ethyl alcohol in sequence, and drying to obtain silicon dioxide carrier powder; wherein the mass ratio of ammonia water, absolute ethyl alcohol, water and TEOS is 1.6-1.7: 2.3-2.4: 1: 0.15-0.16, 0.21-0.22g of sodium hydroxide is added into each gram of nano silicon dioxide;
step 2: adding the silicon dioxide carrier powder prepared in the step 1 and absolute ethyl alcohol into a reaction container, continuously filling nitrogen into the reaction container for 30min, dropwise adding 3-aminopropyltriethoxysilane into the reaction container, stirring at constant temperature for reaction for 3-4h after complete dropwise addition, performing centrifugal precipitation, washing and drying to obtain aminated silicon dioxide carrier powder; wherein 0.68-0.71g of 3-aminopropyltriethoxysilane is added into each gram of silicon dioxide carrier powder; because the surface of the prepared silicon dioxide carrier powder contains a large number of pore channels, and the pore channels and the surface of the silicon dioxide contain a large number of silicon hydroxyl groups, the silicon dioxide can react with silicon oxygen bonds in 3-aminopropyltriethoxysilane, so that the 3-aminopropyltriethoxysilane is grafted on the surface and the pore channels of the silicon dioxide, the surface of the prepared aminated silicon dioxide carrier powder contains abundant amino groups, the amino functional groups can be complexed with hexavalent chromium ions, and because the surface of the silicon dioxide contains a large number of pore diameters, the amino functional group content introduced into the prepared aminated silicon dioxide carrier powder is greatly increased after the silicon dioxide is reacted with the 3-aminopropyltriethoxysilane;
and step 3: preparing 50mL of potassium dichromate solution with chromium ion concentration of 500mg/L, adding the aminated silicon dioxide carrier powder prepared in the step 2 into the aminated silicon dioxide carrier powder, performing static oscillation reaction for 3-4h at normal temperature, filtering and drying, adding the dried solid powder into the newly prepared potassium dichromate solution with chromium ion concentration of 500mg/L again, performing static oscillation reaction for 3-4h at normal temperature, filtering and drying again, adsorbing the dried powder again, filtering and drying after 5 times of repeated adsorption, and obtaining chromium-loaded silicon dioxide; carrying out a complex reaction between amino groups in the aminated silicon dioxide carrier powder and chromium ions in potassium dichromate so as to enable the chromium ions to be adsorbed on the surface of the silicon dioxide, and enabling the aminated silicon dioxide carrier powder to reach adsorption saturation on the chromium ions through 5 times of repeated adsorption;
and 4, step 4: adding the chromium-loaded silicon dioxide prepared in the step 3 into water, simultaneously adding sodium hydroxide into the water, then preparing a ferric chloride solution with the concentration of 1mol/L, dropwise adding the ferric chloride solution into a reaction container, violently stirring while dropwise adding, reacting for 5-6h under constant-temperature stirring after completely dropwise adding, and then filtering and drying to obtain dark brownish red powder; wherein 20mL of water is added into each gram of chromium-loaded silicon dioxide, 1g of sodium hydroxide is added, and 24mL of 1mol/L ferric chloride solution is added, after the chromium-loaded silicon dioxide is added into the water, ferric chloride and the sodium hydroxide are added into a reaction container, ferric hydroxide precipitate is generated on the surface of the chromium-loaded silicon dioxide, the silicon dioxide loaded with chromium ions is gray-green, and after a layer of reddish-brown ferric hydroxide precipitate is loaded on the surface of the silicon dioxide, the prepared product is dark brownish red;
and 5: roasting the black powder prepared in the step 4 in a muffle furnace at the temperature of 450-500 ℃ for 3-4h to obtain a loaded ferrochrome pigment, decomposing ferric hydroxide on the surface of the powder at high temperature after high-temperature calcination to generate ferric oxide, and simultaneously changing hexavalent chromium particles into trivalent chromium ions to coat the interior of the ferric oxide layer, wherein the ferric oxide is reddish brown, and the doped trivalent chromium ions in the ferric oxide layer are green, so that the prepared loaded ferrochrome pigment is dark brownish red;
the specific preparation process of the low-temperature coloring agent for glass decoration comprises the following steps: the raw materials are uniformly mixed according to a certain mass, then the mixture is added into a smelting furnace to be heated to 950 ℃ and 1000 ℃ for smelting for 3-4h, the smelted melt is added into water for water quenching, and then the obtained granular product is dried and crushed to obtain the colorant.
The invention has the beneficial effects that:
1. according to the invention, chromium ions are directly loaded on the silicon dioxide base material, and a layer of ferric oxide is coated on the surface of the chromium ions, so that the prepared colorant can realize a dark reddish brown coloring effect, and the loading base material and the ferric oxide directly fix the chromium ions, so that the problem that heavy metal ions in glass are slowly dissolved out after the glass is corroded can be effectively prevented, and particularly, when a glass product is used for preparing tableware, the glass product is extremely harmful to a human body.
2. According to the invention, the matrix material is prepared into the porous structure in the preparation process of the supported ferrochrome pigment, so that the action site on the surface of the matrix material can be improved, the adsorption capacity of the matrix material on chromium ions is improved, the required color can be achieved, the matrix material is directly used for adsorbing the chromium ions to prepare the pigment, the matrix material can be used for adsorbing the chromium ions in the chromium-polluted water, the polluted water can be treated, the environment is protected, the chromium ions can be reasonably utilized, and the cost is saved.
Detailed Description
Example 1:
the specific preparation process of the supported ferrochrome pigment is as follows:
step 1: adding 160mL of ammonia water and 230mL of absolute ethyl alcohol into 100mL of water, uniformly mixing, adding 15mL of TEOS, stirring for reacting for 2-3h, centrifuging by a centrifuge to collect a precipitate, drying the collected precipitate to obtain nano-silica, adding 100g of the obtained nano-silica into 1000g of water, simultaneously adding 210g of sodium hydroxide, stirring for reacting for 20-22h, centrifuging to obtain a precipitate, washing the precipitate with distilled water and absolute ethyl alcohol in sequence, and drying to obtain silicon dioxide carrier powder;
step 2: adding 100g of the silicon dioxide carrier powder prepared in the step 1 and 2Lg of absolute ethyl alcohol into a reaction container, continuously filling nitrogen into the reaction container for 30min, dropwise adding 680g of 3-aminopropyltriethoxysilane into the reaction container, stirring at constant temperature for reacting for 3-4h after completely adding, performing centrifugal precipitation, washing and drying to obtain aminated silicon dioxide carrier powder;
and step 3: preparing 50mL of potassium dichromate solution with chromium ion concentration of 500mg/L, adding the aminated silicon dioxide carrier powder prepared in the step 2 into the aminated silicon dioxide carrier powder, performing static oscillation reaction for 3-4h at normal temperature, filtering and drying, adding the dried solid powder into the newly prepared potassium dichromate solution with chromium ion concentration of 500mg/L again, performing static oscillation reaction for 3-4h at normal temperature, filtering and drying again, adsorbing the dried powder again, filtering and drying after 5 times of repeated adsorption, and obtaining chromium-loaded silicon dioxide;
and 4, step 4: adding 100g of the chromium-loaded silicon dioxide prepared in the step 3 into 2L of water, simultaneously adding 100g of sodium hydroxide, then preparing a ferric chloride solution with the concentration of 1mol/L, dropwise adding 24mL of the ferric chloride solution into a reaction container while violently stirring, after complete dropwise addition, stirring at constant temperature for reaction for 5-6h, then filtering and drying to obtain dark brownish red powder, after the chromium-loaded silicon dioxide is added into the water, adding ferric chloride and sodium hydroxide into the reaction container, generating ferric hydroxide precipitate on the surface of the chromium-loaded silicon dioxide, wherein the silicon dioxide loaded with chromium ions is grayish green, and after a layer of reddish brown ferric hydroxide precipitate is loaded on the surface of the silicon dioxide, the prepared product is dark brownish red;
and 5: roasting the black powder prepared in the step 4 in a muffle furnace at the temperature of 450-500 ℃ for 3-4h to obtain a loaded ferrochrome pigment, decomposing ferric hydroxide on the surface of the powder at high temperature after high-temperature calcination to generate ferric oxide, and simultaneously changing hexavalent chromium particles into trivalent chromium ions to coat the interior of the ferric oxide layer, wherein the ferric oxide is reddish brown, and the doped trivalent chromium ions in the ferric oxide layer are green, so that the prepared loaded ferrochrome pigment is dark brownish red.
Example 2:
the specific preparation process of the supported ferrochrome pigment is as follows:
step 1: adding 100g of nano silicon dioxide powder and 2Lg of absolute ethyl alcohol into a reaction container, continuously introducing nitrogen into the reaction container for 30min, dropwise adding 680g of 3-aminopropyltriethoxysilane into the reaction container, stirring at constant temperature for reacting for 3-4h after completely adding, performing centrifugal precipitation, washing and drying to obtain aminated silicon dioxide carrier powder;
step 2: preparing 50mL of potassium dichromate solution with chromium ion concentration of 500mg/L, adding the aminated silicon dioxide carrier powder prepared in the step 1 into the aminated silicon dioxide carrier powder, performing static oscillation reaction for 3-4h at normal temperature, filtering and drying, adding the dried solid powder into the newly prepared potassium dichromate solution with chromium ion concentration of 500mg/L again, performing static oscillation reaction for 3-4h at normal temperature, filtering and drying again, adsorbing the dried powder again, filtering and drying after 5 times of repeated adsorption, and obtaining chromium-loaded silicon dioxide;
and step 3: adding 100g of the chromium-loaded silicon dioxide prepared in the step 4 into 2L of water, simultaneously adding 100g of sodium hydroxide, then preparing a ferric chloride solution with the concentration of 1mol/L, dropwise adding 24mL of the ferric chloride solution into a reaction container while violently stirring, after complete dropwise addition, stirring at constant temperature for reaction for 5-6h, then filtering and drying to obtain dark brownish red powder, after the chromium-loaded silicon dioxide is added into the water, adding ferric chloride and sodium hydroxide into the reaction container, generating ferric hydroxide precipitate on the surface of the chromium-loaded silicon dioxide, wherein the silicon dioxide loaded with chromium ions is grayish green, and after a layer of reddish brown ferric hydroxide precipitate is loaded on the surface of the silicon dioxide, the prepared product is dark brownish red;
and 4, step 4: roasting the black powder prepared in the step 3 in a muffle furnace at the temperature of 450-500 ℃ for 3-4h to obtain a loaded ferrochrome pigment, decomposing ferric hydroxide on the surface of the powder at high temperature after high-temperature calcination to generate ferric oxide, and simultaneously changing hexavalent chromium particles into trivalent chromium ions to coat the interior of the ferric oxide layer, wherein the ferric oxide is reddish brown, and the doped trivalent chromium ions in the ferric oxide layer are green, so that the prepared loaded ferrochrome pigment is dark brownish red.
Example 3:
the specific preparation process of the supported ferrochrome pigment is as follows:
step 1: preparing 50mL of potassium dichromate solution with chromium ion concentration of 500mg/L, adding the silicon dioxide carrier powder prepared in the step 1 into the solution, performing static oscillation reaction for 3-4h at normal temperature, filtering and drying, adding the dried solid powder into the newly prepared potassium dichromate solution with chromium ion concentration of 500mg/L again, performing static oscillation reaction for 3-4h at normal temperature, filtering and drying again, adsorbing the dried powder again, filtering and drying after 5 times of repeated adsorption, and obtaining chromium-loaded silicon dioxide;
step 2: adding 100g of the chromium-loaded silicon dioxide prepared in the step 1 into 2L of water, simultaneously adding 100g of sodium hydroxide, then preparing a ferric chloride solution with the concentration of 1mol/L, dropwise adding 24mL of the ferric chloride solution into a reaction container while violently stirring, after complete dropwise addition, stirring at constant temperature for reaction for 5-6h, then filtering and drying to obtain dark brownish red powder, after the chromium-loaded silicon dioxide is added into the water, adding ferric chloride and sodium hydroxide into the reaction container, generating ferric hydroxide precipitate on the surface of the chromium-loaded silicon dioxide, wherein the silicon dioxide loaded with chromium ions is grayish green, and after a layer of reddish brown ferric hydroxide precipitate is loaded on the surface of the silicon dioxide, the prepared product is dark brownish red;
and step 3: roasting the black powder prepared in the step 2 in a muffle furnace at the temperature of 450-500 ℃ for 3-4h to obtain a loaded ferrochrome pigment, decomposing ferric hydroxide on the surface of the powder at high temperature after high-temperature calcination to generate ferric oxide, and simultaneously changing hexavalent chromium particles into trivalent chromium ions to coat the interior of the ferric oxide layer, wherein the ferric oxide is reddish brown, and the doped trivalent chromium ions in the ferric oxide layer are green, so that the prepared loaded ferrochrome pigment is dark brownish red.
Example 4:
the concentrations of chromium ions in the potassium dichromate solutions before and after the static adsorption of the aminated silica support powder in the third step of example 1 and the aminated silica support powder in the second step of example 2 and the silica support powder in example 3 were measured, and the results of the measurements were C1、C1 θ、C2、C2 θ、C3、C3 θ、C4、C4 θ、C5、C5 θWherein the adsorption amounts of the aminated silica support powder in example 1 and example 2 and the silica support powder in example 3 to chromium ions are = (C)1-C1 θ)+(C2-C2 θ)+(C3-C3 θ)+(C4-C4 θ)+（C5-C5 θ) As can be seen from the calculation, the amount of adsorption of chromium ions by the aminated silica carrier powder in example 1 was 73.62mg.g-1The amount of adsorption of chromium ions by the aminated silica carrier powder prepared in example 2 was 29.35mg.g-1The adsorption amount of chromium ions by the silica carrier powder prepared in example 3 was 8.21mg.g-1(ii) a It is known that the surface area of the porous silica prepared by modification is increased, and the number of action sites contained in the surface is increased, and the amino group content of the surface complex is increased by amination modification, and the adsorption amount of chromium ions is increased, therebyThe surface of the silicon dioxide which is not subjected to amination modification does not have the chemical adsorption effect of amino and chromium ions, but only has the physical adsorption effect, so that the content of the chromium ions adsorbed by the prepared carrier powder is reduced, and the later-stage coloring effect is influenced.
Example 5:
the specific preparation process of the low-temperature coloring agent for glass decoration comprises the following steps: 80g of silicon dioxide, 130g of zinc oxide, 260g of borax, 150g of sodium carbonate, 8.1g of talcum powder, 13g of aluminum oxide and 150g of the supported ferrochrome pigment prepared in the embodiment 1 are uniformly mixed, then the mixture is added into a smelting furnace, the temperature is raised to 950 ℃ and 1000 ℃ for smelting for 3-4h, the smelted melt is added into water for water quenching, and then the obtained particle product is dried and crushed to obtain the dark brownish red colorant.
The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise embodiments disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.
Claims (1)
1. The low-temperature coloring agent for glass decoration is characterized by comprising the following components in parts by weight:
8-12 parts of silicon dioxide, 13-14 parts of zinc oxide, 26-28 parts of borax, 15-18 parts of sodium carbonate, 0.81-0.83 part of talcum powder, 1.3-1.6 parts of aluminum oxide and 15-20 parts of load ferrochrome pigment;
the specific preparation process of the supported ferrochrome pigment is as follows:
step 1: adding a certain amount of ammonia water and absolute ethyl alcohol into water, adding TEOS after uniformly mixing, then stirring and reacting for 2-3h, then centrifuging through a centrifuge to collect a precipitate, drying the collected precipitate to obtain nano-silica, then adding the obtained nano-silica into the water, simultaneously adding sodium hydroxide, stirring and reacting for 20-22h, then centrifuging to obtain a precipitate, washing the precipitate with distilled water and absolute ethyl alcohol in sequence, and drying to obtain silicon dioxide carrier powder;
step 2: adding the silicon dioxide carrier powder prepared in the step 1 and absolute ethyl alcohol into a reaction container, continuously introducing nitrogen into the reaction container for 30min, dropwise adding 3-aminopropyltriethoxysilane into the reaction container, stirring at constant temperature for reacting for 3-4h after completely adding, performing centrifugal precipitation, washing and drying to obtain aminated silicon dioxide carrier powder;
and step 3: preparing 50mL of potassium dichromate solution with chromium ion concentration of 500mg/L, adding the aminated silicon dioxide carrier powder prepared in the step 2 into the aminated silicon dioxide carrier powder, performing static oscillation reaction for 3-4h at normal temperature, filtering and drying, adding the dried solid powder into the newly prepared potassium dichromate solution with chromium ion concentration of 500mg/L again, performing static oscillation reaction for 3-4h at normal temperature, filtering and drying again, adsorbing the dried powder again, filtering and drying after 5 times of repeated adsorption, and obtaining chromium-loaded silicon dioxide; carrying out a complex reaction between amino groups in the aminated silicon dioxide carrier powder and chromium ions in potassium dichromate so as to enable the chromium ions to be adsorbed on the surface of the silicon dioxide, and enabling the aminated silicon dioxide carrier powder to reach adsorption saturation on the chromium ions through 5 times of repeated adsorption;
and 4, step 4: adding the chromium-loaded silicon dioxide prepared in the step 3 into water, simultaneously adding sodium hydroxide into the water, then preparing a ferric chloride solution with the concentration of 1mol/L, dropwise adding the ferric chloride solution into a reaction container, violently stirring while dropwise adding, reacting for 5-6h under constant-temperature stirring after completely dropwise adding, and then filtering and drying to obtain dark brownish red powder;
and 5: roasting the dark brown red powder prepared in the step 4 in a muffle furnace at the temperature of 450-500 ℃ for 3-4h to obtain a loaded ferrochrome pigment;
in the step 1, the mass ratio of ammonia water, absolute ethyl alcohol, water and TEOS is 1.6-1.7: 2.3-2.4: 1: 0.15-0.16, 0.21-0.22g of sodium hydroxide is added into each gram of nano silicon dioxide;
in the step 2, 0.68-0.71g of 3-aminopropyltriethoxysilane is added into each gram of silicon dioxide carrier powder;
in the step 4, 20mL of water, 1g of sodium hydroxide and 24mL of 1mol/L ferric chloride solution are added into each gram of chromium-loaded silicon dioxide;
the specific preparation process of the low-temperature colorant is as follows: the raw materials are uniformly mixed according to a certain mass, then the mixture is added into a smelting furnace, the temperature is raised to 950 ℃ and 1000 ℃ for smelting for 3-4h, the smelted melt is added into water for water quenching, and then the obtained particle product is dried and crushed to obtain the colorant.
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Address after: Ding Shu Zhen Xi Wang Cun, Yixing City, Wuxi City, Jiangsu Province Applicant after: Jiangsu Beifu Technology Co.,Ltd. Address before: Ding Shu Zhen Xi Wang Cun, Yixing City, Wuxi City, Jiangsu Province Applicant before: JIANGSU BAIFU TECHNOLOGY Co.,Ltd. |
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| GR01 | Patent grant | ||
| GR01 | Patent grant |