CN112159202B - Iron-stable selenium-rich ceramic material and preparation method thereof - Google Patents
Iron-stable selenium-rich ceramic material and preparation method thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of ceramic materials, and particularly discloses an iron-stable selenium-rich ceramic material and a preparation method thereof, wherein the iron-stable selenium-rich ceramic material mainly comprises kaolin, a selenium source and an iron source, the uniformly mixed selenium-rich pottery clay material is molded by a conventional pottery preparation process, dried, and sintered at the temperature of 800-1200 ℃ for 1-6h in a reducing atmosphere or other inert atmospheres to prepare a selenium-rich pottery sample, and the selenium content and the selenium dissolution amount after the selenium-rich pottery clay material is soaked in water are detected to obtain the iron-stable selenium-rich ceramic material; wherein the iron content is 1 wt% -15 wt%, and the selenium content is 10-200 ppm. The preparation method of the invention is beneficial to the selenium-rich ceramic to be sintered at high temperature and to ensure that selenium stably exists in the ceramic, and the selenium-rich ceramic can dissolve out a proper amount of selenium when being soaked in water or water containing food during use. The invention is characterized in that the sintering temperature of the selenium-rich ceramic can be improved and the selenium content in the selenium-rich ceramic can be stabilized by adding the iron source, and the release amount of selenium can be controlled, thereby achieving the effect of safely, stably and releasing selenium for a long time.
Description
Technical Field
The invention belongs to the technical field of ceramic materials, and particularly relates to an iron-stable selenium-rich ceramic material and a preparation method thereof.
Background
Selenium is an essential trace element for human body and plays a role in improving human health, but the selenium content in food and drinking water of most people is very low, and cannot reach the selenium content level required by normal physiology, so that daily supplement and intake of selenium become especially important. At present, the daily selenium supplement method is divided into organic selenium and inorganic selenium, wherein the supplement of the inorganic selenium is usually realized by additionally adding a selenium source in daily necessities, such as daily necessities made of selenium-rich ceramics, such as cups, bowls, dishes and the like, the preparation of the selenium-rich ceramics needs a sintering process, the higher the sintering temperature is, the higher the strength and hardness of the prepared selenium-rich ceramics are, but the loss amount of the selenium is obviously increased, and meanwhile, the energy consumption is increased.
The selenium-enriched pottery reported in the patent does not mention the loss of selenium in the sintering process, and does not find the detection of the selenium content and the selenium release performance. For example, Chinese patent CN106336196A discloses a selenium-supplementing ceramic and a preparation process thereof, wherein the mass ratio of kaolin to selenium powder is 10:1, the sintering temperature is as high as 1240 ℃, but the selenium content after sintering into ceramic and the characterization of the selenium release performance when the ceramic is soaked in water are not reported; chinese patent CN105541406A discloses a preparation method of a selenium-rich ceramic body, wherein the sintering temperature of the ceramic is 1000-1400 ℃, the heat preservation time is 12-24 h, and the characteristics of the selenium content after sintering into ceramic and the selenium release performance when the ceramic is soaked in water are not reported. It can be seen that most of the selenium-enriched ceramics at present have high sintering temperature, but the loss of selenium in the selenium-enriched ceramics at high temperature is not considered, which causes the high production cost of the selenium-enriched ceramics and the unobvious effect of releasing selenium.
Disclosure of Invention
In order to solve the problems, the invention provides a preparation method of an iron-stable selenium-rich ceramic material, which comprises the following steps:
s1: weighing a certain amount of kaolin, adding a certain amount of selenium source and iron source, and mixing to obtain a selenium-rich pottery clay material;
s2: mixing, ball-milling and drying the selenium-rich argil material according to a conventional pottery preparation process to prepare a selenium-rich mud blank;
s3: protecting and firing the selenium-rich mud blank in a reducing atmosphere or an inert atmosphere to obtain a selenium-rich ceramic sample;
s4: detecting the selenium content in the selenium-enriched ceramic sample and the selenium elution amount of the selenium-enriched ceramic sample after being soaked in water, and determining the selenium enrichment level and the selenium release capacity of the selenium-enriched ceramic sample to obtain the iron-stable selenium-enriched ceramic material.
As a further illustration of the scheme, in the step S1, the content of iron in the selenium-rich pottery clay material is 1-15 wt%, and the content of selenium is 10-200 ppm.
As a further illustration of the scheme, in step S2, the selenium-rich pottery clay material is sintered to prepare a selenium-rich mud blank after being subjected to heat preservation at 800-.
As a further illustration of the above scheme, in step S1, the iron source is an iron compound or an iron simple substance; the iron compound is any one of ferrous sulfate, ferric nitrate and ferric oxide, and the iron simple substance is reducing iron powder.
As a further explanation of the above scheme, in step S1, the selenium source is elemental selenium or any one of selenious acid and sodium selenite, or selenium-rich soil is used to substitute for kaolin without adding a selenium source.
The invention also provides an iron-stable selenium-rich ceramic material, which comprises kaolin, a selenium source and an iron source in preparation raw materials, wherein the iron content is 1-15 wt%, and the selenium content is 10-200 ppm.
The invention has the beneficial effects that: the method is characterized in that in the process of preparing the selenium-rich ceramic, the iron element is added into the raw materials to improve the sintering temperature of the selenium-rich ceramic and stabilize the content of selenium, and the release amount of the selenium can be controlled simultaneously, so that the effects of safe, stable and long-term selenium supplement are achieved.
Drawings
FIG. 1 is a graph showing the relationship between the amount of released selenium and the soaking time of selenium-enriched ceramic samples prepared by adding different iron compounds after soaking in water at 90 ℃;
FIG. 2 is an SEM photograph of selenium enriched ceramic samples prepared by adding different iron compounds;
FIG. 3 is a graph showing the relationship between the amount of released selenium of selenium-enriched ceramic samples prepared at different firing temperatures when immersed in water at 90 ℃ and the immersion time;
FIG. 4 is a graph showing the relationship between the selenium release amount and the soaking time of selenium-enriched ceramic samples prepared by different iron oxide adding amounts after soaking in water at 90 ℃.
Detailed Description
In order to make the solution of the present invention clearer, the present invention will be further explained with reference to the drawings and embodiments.
Example 1:
in this example, a sodium selenite solution (selenium source) of 200ppm was added to a certain amount of kaolin, and the mixture was divided into six portions, wherein a certain amount of ferrous sulfate, ferric nitrate, ferric oxide and reducing iron powder (iron source) was added to each of the five portions, respectively, so that the iron content in the soil was 1-5 wt%, and a control sample was prepared without adding an iron source to the other portion; the selenium-rich pottery clay samples are prepared by respectively using uniform selenium-rich pottery clay materials prepared from ferrous sulfate, ferric nitrate, ferric oxide and reducing iron powder as iron sources and preserving heat at 900 ℃ for 2 hours, and are sequentially marked as #1, #2, #3, #4, #5 and # 6.
The preparation process comprises the following steps:
firstly, adding 200ppm of sodium selenite solution into kaolin, dividing into six parts, wherein a certain amount of ferrous sulfate, ferric nitrate, ferric oxide and reducing iron powder are respectively added into five parts to ensure that the iron content in soil is 5 wt%, respectively preparing 10g of uniform selenium-rich pottery clay materials by ball milling and mixing, and meanwhile, preparing a control sample without adding an iron source into the other part; mixing and ball-milling the selenium-rich argil material according to a conventional pottery preparation process, drying and preparing a selenium-rich mud blank; firing the selenium-rich mud blank in a nitrogen atmosphere, preserving heat at 900 ℃ for 2h, and sintering to obtain a selenium-rich ceramic sample; finally, in order to detect the selenium content in the selenium-enriched pottery sample and the selenium elution amount of the selenium-enriched pottery sample after being soaked in water at 90 ℃, a hydride atomic fluorescence spectrometer is used for detecting the selenium content, the detection results of the selenium content in the selenium-enriched pottery and the unsintered soil powder are shown in tables 1 and 2, and the selenium elution amount result of the selenium-enriched pottery sample after being soaked in water at 90 ℃ is shown in figure 1.
TABLE 1 selenium content and percentage selenium loss for prepared selenium-enriched ceramic samples and unsintered soil powders prepared by adding different iron compounds
TABLE 2 relationship table of selenium release (ppm) and time in selenium-enriched pottery sample water prepared by adding different iron compounds
As can be seen from table 1, table 2 and fig. 1, in this example, by adding an iron-containing compound to the soil, the loss of selenium during the sintering of the selenium pottery can be significantly reduced; the loss amount of selenium of a sample added with ferric oxide is minimum and is only 24.8%, and the loss rate of selenium of a selenium ceramic sample prepared without adding an iron source can reach 73.3%. In addition, the loss of selenium is about 10% during the preparation of the pottery clay of selenium-enriched ceramic on one hand, and the loss of selenium is severe during the sintering process, for example, the loss of selenium content of the sample # 6 is as high as 73.3%.
As can be seen from fig. 2, the selenium-rich pottery prepared by adding the compound of iron has a large number of pore structures on the surface, which is beneficial to the release of selenium, while the selenium-rich pottery added with reducing iron and the blank sample without adding the iron source have much smaller number of pores on the surface and smaller pore diameter than other samples; the obtained selenium-rich ceramic samples are soaked in water at 90 ℃, the content of released selenium of the No. 1 and No. 2 samples is increased and then reduced along with the increase of time, and the content of released selenium of other samples is increased along with the increase of the soaking time; the content of released selenium can be controlled between 0.00040 ppm and 0.018 ppm.
Therefore, the loss of selenium in the sintering process of the selenium pottery can be obviously reduced by adding the iron-containing compound into the soil, and the release amount of the selenium can be controlled.
Example 2:
in this example, 200ppm sodium selenite solution (selenium source) and a certain amount of iron oxide (iron source) were added to kaolin to make the iron content in the soil 5 wt%; the prepared uniform selenium-rich pottery clay materials are respectively subjected to heat preservation at 900 ℃, 1000 and 1100 ℃ for 2h to prepare selenium-rich pottery samples which are respectively marked as #7, #8 and # 9.
The preparation process comprises the following steps:
firstly, adding 200ppm of sodium selenite solution and a certain amount of ferric oxide into kaolin to ensure that the iron content in soil is 5 wt%, and performing ball milling and mixing to respectively prepare a selenium-rich pottery clay material with the uniform selenium content of 10-200ppm and 10 g; then, mixing and ball-milling the mixed soil sample according to a conventional pottery preparation process, drying the mixed soil sample, and preparing a selenium-rich mud blank; then firing the selenium-rich mud blank in nitrogen atmosphere, respectively preserving heat for 2h at 900, 1000 and 1100 ℃, and then sintering to obtain a selenium-rich ceramic sample; finally, the selenium content in the selenium-enriched ceramic sample and the selenium elution amount after the selenium-enriched ceramic sample is soaked in water at 90 ℃ can be detected by a hydride atomic fluorescence spectrometer, the detection results of the selenium content in the selenium-enriched ceramic sample and the unsintered soil powder are shown in tables 3 and 4, and the selenium elution amount result after the selenium-enriched ceramic sample is soaked in water at 90 ℃ is shown in fig. 3.
As can be seen from tables 3 and 4 and fig. 3, in this embodiment, under the condition of a certain iron addition amount and other conditions, the higher the sintering temperature of the selenium-rich pottery sample is, the higher the selenium loss rate is, and when the sintering temperature is increased to 1100 ℃, the selenium loss rate of the selenium-rich pottery is increased to 54.6%; soaking the obtained selenium-rich ceramic samples in water at 90 ℃, wherein the content of released selenium of all samples is increased along with the prolonging of the soaking time; the content of released selenium can be controlled between 0.0028 ppm and 0.015 ppm.
Therefore, the selenium content in the selenium-enriched pottery and the release concentration of selenium in the selenium-enriched pottery can be controlled by the firing temperature.
TABLE 3 preparation of selenium-enriched pottery sample and unsintered soil powder with different sintering temperatures
TABLE 4 relationship table of selenium release amount (ppm) and time in selenium-enriched pottery sample water prepared at different sintering temperatures
Example 3:
in this example, 200ppm sodium selenite solution and a certain amount of iron oxide were added to kaolin, and the mixture was divided into four portions, so that the iron content in the soil was 1 wt%, 5 wt%, 10 wt% and 15 wt%, respectively, and the obtained uniform selenium-rich pottery clay material was heat-preserved at 900 ℃ for 2 hours to obtain selenium-rich pottery samples, which were designated as #10, #11, #12 and # 13.
The preparation process comprises the following steps:
firstly, adding 200ppm of sodium selenite solution and a certain amount of ferric oxide into kaolin, dividing into four parts to ensure that the iron content in each part of soil is respectively 1 wt%, 5 wt%, 10 wt% and 15 wt%, and ball-milling and mixing to respectively prepare 12g of uniform selenium-rich kaolin materials; then, mixing and ball-milling the mixed soil sample according to a conventional pottery preparation process, drying the mixed soil sample, and preparing a selenium-rich mud blank; then firing the selenium-rich mud blank in a nitrogen atmosphere, preserving heat for 2 hours at 900 ℃, and sintering to obtain a selenium-rich ceramic sample; finally, the selenium content in the selenium-enriched pottery sample and the selenium elution amount after the selenium-enriched pottery sample is soaked in water at 90 ℃ can be detected by a hydride atomic fluorescence spectrometer, the detection results of the selenium content in the selenium-enriched pottery and the unsintered soil powder are shown in tables 5 and 6, and the selenium elution amount result after the selenium-enriched pottery sample is soaked in water at 90 ℃ is shown in figure 4.
TABLE 5 preparation of selenium-enriched ceramic samples and unsintered soil powders with different amounts of iron oxide added and percent selenium loss
TABLE 6 relationship table of selenium release (ppm) and time for selenium-enriched pottery sample water prepared by adding different iron oxide
As can be seen from tables 5 and 6 and fig. 4, in this embodiment, under the condition that other conditions are not changed, the larger the iron addition amount is, the smaller the selenium loss rate of the selenium-rich pottery sample is, and when the iron addition amount reaches 5 wt%, the selenium loss rate of the selenium-rich pottery tends to be stable; soaking the obtained selenium-rich ceramic samples in water at 90 ℃, wherein the content of released selenium of all samples is increased along with the prolonging of the soaking time; the content of released selenium can be controlled between 0.0013 ppm and 0.016 ppm.
Therefore, the selenium content in the selenium-enriched pottery and the release concentration of selenium in the selenium-enriched pottery can be controlled by adjusting the addition amount of iron.
In conclusion, in the preparation method, the loss of selenium in the selenium-rich ceramic sample in the high-temperature sintering process is effectively reduced by adding the iron compound, and under the condition that other conditions are not changed, different iron compounds and different adding amounts have different influences on the stability of the selenium in the selenium-rich ceramic sample. Soaking in 90 deg.C water to release selenium content of 0.00040-0.018 ppm. Therefore, the loss of selenium in the sintering process can be reduced by adding the iron compound, the release amount of selenium in water is kept at a proper level, and the service life of the selenium ceramic can be prolonged.
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 using the contents of the present specification and the accompanying drawings, 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 iron-stable selenium-rich ceramic material is characterized by comprising the following steps of:
s1: weighing a certain amount of kaolin, adding a selenium source and an iron source, and mixing to obtain a selenium-rich pottery clay material, wherein the iron content in the selenium-rich pottery clay material is 1-15 wt%, and the selenium content is 10-200 ppm;
s2: mixing, ball-milling and drying the selenium-rich argil material according to a conventional pottery preparation process to prepare a selenium-rich mud blank;
s3: protecting and firing the selenium-rich mud blank in a reducing atmosphere or an inert atmosphere to obtain a selenium-rich ceramic sample;
s4: detecting the selenium content in the selenium-enriched ceramic sample and the selenium elution amount after the selenium-enriched ceramic sample is soaked in water, and determining the selenium enrichment level and the selenium release capacity of the selenium-enriched ceramic sample to obtain the iron-stable selenium-enriched ceramic material.
2. The method for preparing the Fe-stable selenium-rich ceramic material as claimed in claim 1, wherein in step S2, the selenium-rich pottery clay material is sintered to prepare the selenium-rich mud blank after heat preservation at 800-1200 ℃ for 1-6 h.
3. The method for preparing the iron-stable selenium-rich ceramic material as claimed in claim 1, wherein in step S1, the iron source is an iron compound or an iron simple substance; the iron compound is any one of ferrous sulfate, ferric nitrate and ferric oxide, and the iron simple substance is reducing iron powder.
4. The method for preparing the iron-stable selenium-rich ceramic material as claimed in claim 1, wherein in step S1, the selenium source is selenium or one of selenious acid and sodium selenite, or the kaolin is replaced by selenium-rich soil without adding the selenium source.
5. An iron-stable selenium-enriched ceramic material, characterized by being prepared by the preparation method of any one of claims 1 to 4.
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