CN114292024A - Nitrate-free environment-friendly steel plate enamel high-temperature titanium dioxide overglaze and preparation method thereof - Google Patents
Nitrate-free environment-friendly steel plate enamel high-temperature titanium dioxide overglaze and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a nitrate-free environment-friendly high-temperature titanium dioxide overglaze for steel plate enamel and a preparation method thereof. The enamel belongs to the technical field of enamel, and the formula comprises the following components in parts by mass: 25-27 parts of quartz, 26-28 parts of borax anhydrous, 0.1-0.14 part of antimony oxide, 9-11 parts of potassium feldspar, 12-14 parts of titanium dioxide, 2-4 parts of magnesium carbonate, 6-8 parts of sodium tripolyphosphate and 5-7 parts of sodium fluosilicate. The raw materials are evenly mixed according to the proportion and melted under the condition of 1290 +/-10 ℃ and pure oxygen, and the firing temperature of the finished product is 850-. The formula of the invention does not contain nitrate, thereby fundamentally solving the problem that the prior high-temperature titanium white overglaze for steel plate enamel generates Nitrogen Oxide (NO) in the production processx) The gas emission pollutes the environment.
Description
Technical Field
The invention belongs to the technical field of enamel, and particularly relates to a nitrate-free environment-friendly high-temperature titanium dioxide overglaze for steel plate enamel and a preparation method thereof.
Background
The enamel glaze is mainly prepared from fire-resistant raw materials such as feldspar and quartz, fusible chemical raw materials such as borax, sodium nitrate, potassium nitrate and soda ash, characteristic raw materials such as non-ferrous metal oxides and the like according to a certain proportion, and is prepared by high-temperature melting and rapid cooling to form granular or flaky borosilicate glass.
The introduction of nitrate (sodium nitrate, potassium nitrate, etc.) as an oxidant and a fluxing agent into the enamel glaze is a common consensus among people in the industry and is an essential enamel glaze raw material in the traditional enamel theory. So far, no safe, colorless, reasonably priced, oxidizing and fluxing raw material is available to replace nitrate. Production practices have long proved that nitrates, in particular alkali metal nitrates, are indeed essential raw materials in enamel.
In the process of melting the enamel glaze at high temperature, a series of complex physical and chemical reactions are carried out among the raw materials. Nitrate has good effect in enamel glaze, but can be decomposed at high temperature to generate a large amount of nitrogen oxides, thereby polluting the atmospheric environment. The nitrogen oxide exceeds the national emission standard by more than 40 times, and if the converter is adopted for production, the instantaneous release concentration of the nitrogen oxide exceeds the national standard by hundreds of thousands of times. As is well known, nitrogen oxides are the main factors of acid rain in the air, and with the increasing awareness of environmental protection, the harm of nitrogen oxides released by nitrates in the production of enamel glaze to the environment is more and more concerned by all parties.
Therefore, the emission of nitrogen oxides reaching the standard and the improvement of the environment are inevitable trends of social responsibility and social economic development of enterprises, and are inevitable choices for the survival of the enterprises. The applicant starts to research the use amount of nitrate in the enamel glaze from 2018, and ensures that the waste gas in the production process of the enamel glaze reaches the emission standard by adding other measures and using no or less nitrate as far as possible on the premise of not influencing the product performance.
The main three technical routes for reducing the emission of nitrogen oxides in the production process of the enamel glaze are as follows: firstly, the use of nitrate is removed or reduced from the source, secondly, nitrogen oxide generated by air in a high-temperature state in the melting process is eliminated, thirdly, the emission of the nitrogen oxide is reduced from the treatment facility, and therefore the national emission standard is achieved.
Prior to this, there have also been technical studies of the single nitrate-removal in enamel formulations, but if nitrate is removed purely for nitrate-removal, the direct consequence is that the quality of the product needs to be sacrificed to some extent, since the fluxing and oxidizing properties of the corresponding nitrate are not supplemented correspondingly, i.e.: on one hand, the fluxing agent in the formula of the porcelain glaze is reduced, and the smoothness, the leveling property and the expansion coefficient of the porcelain glaze product are directly influenced; on the other hand, since nitrate is oxidizing, removal of nitrate during the glaze melting process results in reduction of some of the metal oxides in the glaze formulation, and the glaze color development and adhesion properties are affected.
From the perspective of the fluxing agent, the compound salt is used for replacing nitrate to serve as a raw material formula of the porcelain glaze, the traditional melting process is used for melting, and the fluxing effect is hopeful to be replaced. However, the use of nitrate removal results in a reduction of the oxidizing atmosphere during the enamel melting process, with the consequent partial reduction of the corresponding metal oxides, which has an effect both on the colour and on the adherence of the enamel product. Therefore, after the nitrate is removed, the supplement of the fluxing effect and the oxidation effect must be considered simultaneously to maintain the original performance of the enamel product.
The specific application of the nitrate in the enamel is mainly sodium nitrate and potassium nitrate, and the nitrate has good oxidation effect under the high-temperature condition, so that oxides can be prevented from being reduced into simple substances in the melting process, and meanwhile, the common products Na of the nitrate sodium nitrate and potassium nitrate after being decomposed at high temperature2O and K2O has good fluxing action.
Taking sodium nitrate commonly used in the enamel glaze of the traditional steel plate containing nitrate as an example, the chemical reaction of nitrate in the enamel glaze production is as follows:
the nitrate is decomposed during heating to generate nitrite and release oxygen, thereby preventing the metal oxide from generating reduction reaction during melting, converting the metal oxide to a low valence state, and even reducing the metal oxide to elemental metal, thereby changing the components, the physical and chemical properties and the process performance of the enamel glaze.
At present, partial nitrate removal research is explored. The Chinese invention CN201810677390.4 provides a preparation technology of phosphosilicate enamel, and the Chinese invention CN201010608133.9 discloses a high-toughness enamel glaze which is represented by the above materials, and various oxides are directly mixed and melted to obtain an enamel product, so that the use of nitrate is avoided. This may be feasible for theoretical studies. However, under the conditions of the prior art, Na2O and K2O has no industrialized product, and has extremely active activity, poor stability and difficult stable storage. Therefore, the method directly uses oxides such as sodium oxide and potassium oxide as raw materials, and cannot realize industrial production at present, so that the method has no practicability. The invention CN201310166353.4 of China discloses a high and low temperature resistant porcelain glaze for enamel, the use of nitrate is not involved in the formula, but the invention introduces the use of heavy metal lead for improving the product quality and reducing the sintering point, which completely violates the safety requirement of daily application and is prohibited by the industry, and simultaneously, the invention also relates to the use of a large amount of sulfate, even if the content is very low, the existence of the sulfate is likely to cause explosion in the quenching link, thereby violating the basic requirement of safe production. In addition, the borate content in the formula is low, and the basic requirement of the enamel industry cannot be met. That is, the invention is claimed to be able to be used for enamels, the conditions of which are practically not reached even without taking into account the aforementioned drawbacks. The Chinese invention CN201711361365.7 discloses a matt sand-grain enamel glaze core glaze and a production method thereof, wherein the core glaze seems not to relate to the use of nitrate, but is a flatting agent in essence, and needs to be combined with a real glaze to achieve the flatting purpose of the glaze, and is not an independent glaze and can not be used independently. Furthermore, in "preliminary practice of nitrate-free enamels" (New Schedule, New City, New Jinnau cattle practice Co., Ltd., glass and enamel. 2007.35 (1)), in order to intensify the oxidation, the document uses a method of increasing the air flow, although the use of nitrate is not involved, but its starting point is not at allThis is achieved not by reducing the nitrogen oxides but by solving the problem of sufficient oxidation of the Ti-containing overglaze by means of increasing the air flow. However, the increase of the air flow rate can have an obvious cooling effect on the melting furnace, in order to enable the temperature of the melting furnace to meet the requirement, the energy consumption needs to be increased to increase the reaction temperature of the melting furnace, and the air contains a large amount of nitrogen, and under the effect of high temperature, the introduction of a large amount of air can cause the generation of more nitrogen oxides. Research practice shows that the empty burning smelting furnace can cause the content of nitrogen oxides to exceed the national emission standard by more than 2 times. If air is introduced at a high flow rate, the result is more conceivable. Thus, although the use of nitrates is avoided, the production of nitrogen oxides is ultimately exacerbated, contrary to the goal of reducing or eliminating nitrogen oxides.
In conclusion, in the enamel research, the nitrate is removed, the environmental benefit is improved, and simultaneously the excellent quality of the enamel product can be maintained, so that the method is significant and has a difficult task.
Disclosure of Invention
One of the purposes of the invention is to provide a nitrate-free environment-friendly high-temperature titanium dioxide overglaze for steel plate enamel on the premise of not reducing various performance indexes of products aiming at the environmental protection problem existing in the prior traditional nitrate-containing steel plate enamel.
The invention relates to a nitrate-free environment-friendly steel plate enamel high-temperature titanium dioxide overglaze, which comprises the following components in percentage by weight: quartz, borax anhydrous, antimony oxide, potassium feldspar, titanium dioxide, magnesium carbonate, sodium tripolyphosphate and sodium fluosilicate; wherein the mass parts of the components are respectively as follows: 25-27 parts of quartz, 26-28 parts of borax anhydrous, 0.1-0.14 part of antimony oxide, 9-11 parts of potassium feldspar, 12-14 parts of titanium dioxide, 2-4 parts of magnesium carbonate, 6-8 parts of sodium tripolyphosphate and 5-7 parts of sodium fluosilicate.
Preferably, the mass parts of the components are respectively as follows: 26.5 parts of quartz, 27 parts of borax anhydrous, 0.12 part of antimony oxide, 10.5 parts of potassium feldspar, 13 parts of titanium dioxide, 3.4 parts of magnesium carbonate, 7.5 parts of sodium tripolyphosphate and 7 parts of sodium fluosilicate.
In particular, among the said quartz, Sio2、Fe2O3Mass ofThe percentage content is as follows: sio2≥99％、Fe2O3≤0.05％。
Specifically, in the potassium feldspar, K is2The mass percentage of O is as follows: k2O≥11％。
Specifically, in the titanium dioxide, Tio2The mass percentage of the components is as follows: tio2≥99％。
The second purpose of the invention is to provide a preparation method of the nitrate-free environment-friendly steel plate enamel high-temperature titanium dioxide overglaze.
The invention relates to a preparation method of nitrate-free environment-friendly high-temperature titanium dioxide overglaze for steel plate enamel, which comprises the following steps:
(1) weighing the following raw materials in parts by mass;
25-27 parts of quartz, 26-28 parts of borax anhydrous, 0.1-0.14 part of antimony oxide, 9-11 parts of potassium feldspar, 12-14 parts of titanium dioxide, 2-4 parts of magnesium carbonate, 6-8 parts of sodium tripolyphosphate and 5-7 parts of sodium fluosilicate;
(2) stirring and uniformly mixing the raw materials in the step (1);
(3) adding the uniformly mixed materials into a melting furnace, melting under the condition of pure oxygen, and controlling the melting temperature to be 1290 +/-10 ℃;
(4) and (3) obtaining a borosilicate glass body after the materials in the step (3) are completely melted, drilling the melted borosilicate glass body, and rapidly drawing 1.2-1.5 m glass fibers for detection, wherein the detection requirements are as follows: the glass fiber is melted within 1 m;
(5) and (3) quenching the molten borosilicate glass body to obtain the product.
Specifically, the quenching in the step (5) is a water quenching or tabletting process.
The third purpose of the invention is to provide the application of the nitrate-free environment-friendly steel plate enamel high-temperature titanium dioxide overglaze, namely the application of the nitrate-free environment-friendly steel plate enamel high-temperature titanium dioxide overglaze on a blank taking a steel plate as a substrate, wherein the firing temperature of a finished product is 850-880 ℃.
The invention has the beneficial effects that:
at high temperature or at discharge, nitrogen and oxygen can be combined into NOx. With respect to NOxThe mechanism of formation of (A) is N in air at high temperature2The oxidation generates NO, and the generation rate thereof has a large relationship with the gas concentration and the combustion temperature. Practice shows that when the temperature reaches over 1000 ℃, the air-fired melting furnace can also cause the generation of high-content nitrogen oxides. Therefore, the invention adopts pure oxygen to replace air, on one hand, the oxidizing atmosphere in the melting process can be increased, and on the other hand, the zero emission of nitrogen oxides generated in the combustion process is realized.
In addition, the components and the dosage of the non-nitrate fluxing agent are adjusted in the formula, so that the melting can be completed as required even if no nitrate fluxing agent is used in the enamel glaze. The key technical innovation point of the invention is that after nitrate is removed, the fluxing property in the enamel glaze can still be ensured.
The nitrate-free environment-friendly steel plate enamel high-temperature titanium dioxide overglaze and the preparation method thereof can remove nitrate from the enamel glaze, realize industrialization, solve the problem that the environment is polluted by nitrogen oxide discharged in the production process of the enamel glaze, and ensure that the original physical and chemical properties of the enamel glaze are kept unchanged. Experimental practice proves that 80% of the series products of enamel glaze manufacturers of the applicant of the invention do not contain nitrate, and the use amount of nitrate can be reduced by more than 50% even though the nitrate cannot be completely removed from the rest 20% of the series products. The usage amount of the nitrate is reduced to about 100 tons from the original annual usage amount of 1000 tons, and the reduction rate is close to 85 percent. Nitrate removal alone directly reduces the nitrogen oxide emissions by 500 tons per year, and does not include the conversion of nitrogen in the air to nitrogen oxides. In addition, the performance (porcelain surface, luster, sintering temperature) and other aspects of the product after nitrate removal are not changed, and the quality detection requirements of the national enamel products are met. Therefore, the implementation and popularization of the invention are beneficial to driving the industrial upgrading, protecting the ecological environment and having extremely important environmental benefit, social benefit and popularization and application significance.
Drawings
FIG. 1 is a photograph of a steel plate enamel high-temperature titanium dioxide overglaze applied to a steel plate enamel product prepared in example 1 of the present invention.
FIGS. 2, 3 and 4 are the first, second and third pages of the test report of the high temperature titanium dioxide overglaze application of steel plate enamel prepared in example 2 of the present invention.
Detailed Description
The present invention will be described in further detail with reference to specific experimental examples.
The equipment used in the embodiment of the invention is as follows:
preparing materials: adopts a full-automatic batching and mixing system. The system is fully-automatic computer control, and has the characteristics of accurate weighing, uniform mixing and high batching efficiency.
Melting: an automatic feeding system, a pure oxygen combustion system and an automatic discharging system are adopted. Because the effect of the oxidant is removed after the nitrate is removed, the combustion condition of the smelting furnace is improved, pure oxygen combustion is changed, and the effect of the oxidant can also meet the requirement after the nitrate is removed. This is also the key point in the present invention to remove nitrate, but the performance of the oxidizer is not changed.
Packaging: an automatic packaging system is used.
Among the raw materials used in the examples of the present invention, Sio in quartz2、Fe2O3The mass percentage of the components is as follows: sio2≥99％、Fe2O3Less than or equal to 0.05 percent; k in potassium feldspar2The mass percentage of O is as follows: k2O is more than or equal to 11 percent; tio in titanium dioxide2The mass percentage of the components is as follows: tio2Not less than 99 percent. The purity of other raw materials meets the requirement of industrial grade.
Example 1:
(1) weighing the following raw materials in parts by mass:
26.5KG quartz, 26KG anhydrous borax, 0.12KG antimony oxide, 11KG potassium feldspar, 13KG titanium dioxide, 3.4KG magnesium carbonate, 7.5KG sodium tripolyphosphate and 8KG sodium fluosilicate.
(2) The raw materials are stirred and mixed evenly.
(3) And adding the uniformly mixed materials into a melting furnace, melting under the condition of pure oxygen, and controlling the melting temperature to 1290 +/-10 ℃ for melting.
(4) Obtaining a borosilicate glass body after the above materials are completely melted, drilling the melted borosilicate glass body, and rapidly drawing 1.2-1.5 m glass fiber to detect, wherein the detection requirement is as follows: the glass fiber is melted within 1 m.
(5) And (3) rapidly cooling (water quenching) the molten borosilicate glass body to obtain the product.
Example 2:
this example is prepared substantially identically to example 1, except that:
the mass parts of the components in the step (1) are as follows: 26.5KG quartz, 27KG anhydrous borax, 0.12KG antimony oxide, 10.5KG potassium feldspar, 13KG titanium dioxide, 3.4KG magnesium carbonate, 7.5KG sodium tripolyphosphate and 7KG sodium fluosilicate.
In the step (5), the rapid cooling of the molten borosilicate glass body adopts a tabletting process.
Example 3:
this example is prepared substantially identically to example 1, except that:
the mass parts of the components in the step (1) are as follows: 26.5KG of quartz, 28KG of anhydrous borax, 0.12KG of antimony oxide, 10KG of potassium feldspar, 13KG of titanium dioxide, 3.4KG of magnesium carbonate, 7.5KG of sodium tripolyphosphate and 6KG of sodium fluosilicate.
Example 4:
this example is prepared substantially identically to example 1, except that:
the mass parts of the components in the step (1) are as follows: quartz 25KG, anhydrous borax 26KG, antimony oxide 0.1KG, potassium feldspar 9KG, titanium white powder 12KG, magnesium carbonate 2KG, sodium tripolyphosphate 6KG, sodium fluorosilicate 5 KG.
Example 5:
this example is prepared substantially identically to example 1, except that:
the mass parts of the components in the step (1) are as follows: 27KG quartz, 27.5KG anhydrous borax, 0.14KG antimony oxide, 10.8KG potassium feldspar, 14KG titanium dioxide, 4KG magnesium carbonate, 8KG sodium tripolyphosphate, 6.8KG sodium fluosilicate.
The product prepared by the invention is applied to a blank taking a steel plate as a substrate, and the firing temperature of the finished product is 850-.
Taking the product obtained in the embodiment of the invention as an example, the performance evaluation is as follows:
referring to fig. 1, the high-temperature titanium white overglaze for steel plate enamel prepared in the embodiment 1 of the invention has a smooth and fine surface, uniform and beautiful color, and the hue completely meets the requirements of users.
Referring to fig. 2, a report of the test of the application of the high-temperature titanium white overglaze for steel plate enamel prepared in example 2 of the present invention is shown. The detection unit is the national glasses and glass detection center.
Experiments and detection results prove that the nitrate-free environment-friendly high-temperature titanium dioxide overglaze for steel plate enamel, which is produced by the method, does not generate nitrogen oxides in the preparation process, and various properties (porcelain surface, luster, whiteness, hue, sintering temperature) and the like of the obtained product meet the requirements of the high-temperature titanium dioxide overglaze for steel plate enamel, thereby realizing the aim of removing the nitrate from the environment-friendly high-temperature titanium dioxide overglaze for steel plate enamel, and fundamentally solving the problem that the Nitrogen Oxides (NO) are generated in the production and processing processes of the traditional high-temperature titanium dioxide overglaze for steel plate enamelx) The gas emission pollutes the environment.
Claims (8)
1. The nitrate-free environment-friendly steel plate enamel high-temperature titanium dioxide overglaze is characterized by comprising the following components in percentage by weight: quartz, borax anhydrous, antimony oxide, potassium feldspar, titanium dioxide, magnesium carbonate, sodium tripolyphosphate and sodium fluosilicate; wherein the mass parts of the components are respectively as follows: 25-27 parts of quartz, 26-28 parts of borax anhydrous, 0.1-0.14 part of antimony oxide, 9-11 parts of potassium feldspar, 12-14 parts of titanium dioxide, 2-4 parts of magnesium carbonate, 6-8 parts of sodium tripolyphosphate and 5-7 parts of sodium fluosilicate.
2. The nitrate-free, environmentally friendly, steel plate enamel high temperature titanium dioxide overglaze according to claim 1, wherein: the weight portions of the components are respectively as follows: 26.5 parts of quartz, 27 parts of borax anhydrous, 0.12 part of antimony oxide, 10.5 parts of potassium feldspar, 13 parts of titanium dioxide, 3.4 parts of magnesium carbonate, 7.5 parts of sodium tripolyphosphate and 7 parts of sodium fluosilicate.
3. The nitrate-free, environmentally friendly, steel plate enamel high temperature titanium dioxide overglaze according to claim 1, wherein: among the quartz, Sio2、Fe2O3The mass percentage of the components is as follows: sio2≥99％、Fe2O3≤0.05％。
4. The nitrate-free, environmentally friendly high temperature steel sheet enamel titanium dioxide overglaze according to claim 1, wherein: in the potassium feldspar, K2The mass percentage of O is as follows: k2O≥11％。
5. The nitrate-free, environmentally friendly, steel plate enamel high temperature titanium dioxide overglaze according to claim 1, wherein: in the titanium dioxide, Tio2The mass percentage of the components is as follows: tio2≥99％。
6. The method for preparing the nitrate-free environment-friendly steel plate enamel high-temperature titanium dioxide overglaze according to claim 1, which is characterized by comprising the following steps:
(1) weighing the following raw materials in parts by mass;
25-27 parts of quartz, 26-28 parts of borax anhydrous, 0.1-0.14 part of antimony oxide, 9-11 parts of potassium feldspar, 12-14 parts of titanium dioxide, 2-4 parts of magnesium carbonate, 6-8 parts of sodium tripolyphosphate and 5-7 parts of sodium fluosilicate;
(2) stirring and uniformly mixing the raw materials in the step (1);
(3) adding the uniformly mixed materials into a melting furnace, melting under the condition of pure oxygen, and controlling the melting temperature to be 1290 +/-10 ℃;
(4) and (3) obtaining a borosilicate glass body after the materials in the step (3) are completely melted, drilling the melted borosilicate glass body, and rapidly drawing 1.2-1.5 m glass fibers for detection, wherein the detection requirements are as follows: the glass fiber is melted within 1 m;
(5) and (3) quenching the molten borosilicate glass body to obtain the product.
7. The method for preparing the nitrate-free environment-friendly steel plate enamel high-temperature titanium dioxide overglaze according to claim 6, wherein the method comprises the following steps: and (5) quenching by adopting a water quenching or tabletting process.
8. The use of the nitrate-free environment-friendly steel plate enamel high-temperature titanium dioxide overglaze according to claim 1, wherein: the method is applied to a blank taking a steel plate as a substrate, and the firing temperature of the finished product is 850-880 ℃.
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