CN109896823B - Hydrothermal preparation method of natural granite-like mineral solidified body - Google Patents
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Abstract
The invention discloses a hydrothermal preparation method of a natural granite-like mineral solidified body, which is characterized by comprising the following steps of: taking 100 parts by weight of metakaolin, 90-120 parts by weight of potash water glass, 0-105 parts by weight of silica micropowder and 150-300 parts by weight of quartz sand, adding 25-85 parts by weight of water, mixing and stirring to obtain slurry; injecting the slurry into a steel mould, standing, and placing in an autoclave at the temperature of 180-260 ℃ for 8-12 h; and after cooling, taking out the mold and demolding to obtain the natural granite-like mineral solidified body. The compressive strength of the natural granite-like mineral solidified body prepared by the invention is more than or equal to 80MPa, and the flexural strength is more than or equal to 12 MPa. The mineral solidified body has similar composition, structure and performance to natural granite, and is especially suitable for solidifying radioactive waste.
Description
Technical Field
The invention belongs to the preparation of artificial rock mineral materials and the solidification treatment of radioactive wastes, and relates to a hydrothermal preparation method of a natural granite-like mineral solidified body.
Background
Granite/granite is a natural rock composed of potassium feldspar, quartz, mica and other minerals, and the silicon dioxide content of the rock is more than 65%. Granite is hard, is difficult to be eroded by acid-base or weathering, and has stable geology. In addition, granite usually contains relatively more natural radionuclides, which exist in silicate minerals and aluminosilicate minerals, and uranium deposit 1/3 above is a granite type uranium ore, which also becomes the most important raw material source in the uranium ore metallurgy industry in China. Based on the above, it is known that granite itself is geologically stable, and even granite containing natural radionuclides can exist stably for over ten thousand years. Currently, most of the countries in the world take granite geology as the first choice for building radioactive waste deep geological repositories, and granite as the surrounding rock of high-level waste geological repositories.
However, granite is less common as a cured substrate for radionuclides. Firstly, the content of nuclide of granite is high, the radioactivity level is high, and the nuclide and the radioactivity level of a solidified body are further increased when the granite is used as a solidified base material; secondly, the granite is a natural rock material, and is taken as a curing base material, a certain binding agent needs to be added, the granite is subjected to high-pressure compression molding and then sintering, the process and the flow are complex, and radioactive waste leakage pollution is easily caused; finally, the granite is a mixture of a plurality of silicate minerals, nuclides in the radioactive waste at low temperature are difficult to enter a crystalline silicate mineral crystal structure, the granite needs to be reconstructed at high temperature, and then a solidified body is formed in the cooling process, but the original mineral composition of the granite is changed. The chemical and mineral composition of granite is referred to, the geological formation process of granite is simulated, the existing silicate and aluminosilicate raw materials which are easily obtained are used, and the low-temperature preparation of the natural granite-like mineral solidified body is expected to overcome the problems.
Disclosure of Invention
The invention aims to overcome the defects of the existing radioactive waste solidification treatment and solidification base material selection technology and provides a hydrothermal preparation method of a natural granite-like mineral solidified body. By adopting the invention, the slurry formed by injection molding is initially coagulated and hardened at room temperature, and then subjected to hydrothermal treatment, the zeolite-like gel is crystallized and converted into mineral structures like feldspar, potassium feldspar and the like, and the doped quartz sand is added, so that the hydrothermal preparation method of the natural granite-like mineral solidified body, which not only has excellent mechanical property and stable structure, but also contains a plurality of main minerals of natural granite, is provided.
The content of the invention is as follows: a hydrothermal preparation method of a natural granite-like mineral solidified body is characterized by comprising the following steps:
a. taking raw materials according to the weight ratio of 100 parts by weight of metakaolin, 90-120 parts by weight of potash water glass, 0-105 parts by weight of silica micropowder and 150-300 parts by weight of quartz sand, adding 25-85 parts by weight of water, mixing and stirring to obtain uniform slurry;
b. injecting the slurry into a steel mould, and standing for 1-3 h at room temperature;
c. then placing the steel mould filled with the slurry in an autoclave at the temperature of 180-260 ℃ for 8-12 h;
d. and (c) cooling the autoclave, taking out the mold with the sample (the sample is the reaction product of the slurry in the step (c) in the autoclave at the temperature of 180-260 ℃ for 8-12 hours), and demolding to obtain the natural granite-like mineral solidified body.
The invention comprises the following steps: the step a is preferably: taking the raw materials according to the weight ratio of 100 parts by weight of metakaolin, 90-120 parts by weight of potash water glass, 0.1-105 parts by weight of silica micropowder and 150-300 parts by weight of quartz sand, adding 25-85 parts by weight of water, mixing and stirring to obtain uniform slurry.
The invention comprises the following steps: the metakaolin in the step a mainly comprises the chemical components and the weight percentage of SiO2 50～55％、Al2O340-45% of other trace components (e.g. Fe)2O3、Na2O、K2O, CaO, etc.) 3% -5%, and the sum of all the components is 100%; the metakaolin is K1300 type metakaolin produced by inner Mongolia super-brand kaolin company Limited.
The invention comprises the following steps: the main chemical composition and weight percentage of the potash water glass in the step a are SiO2 22～28％、K2O 21～35％、H2O43-50%, and the sum of all the components is 100%.
The invention comprises the following steps: the silica micropowder in the step a can be superfine quartz powder, silica fume and diatomiteOne or a mixture of two or more of nano-silica and white carbon black, the particle diameter of which is less than 1 μm, and SiO in the fine silica powder2The weight percentage content is more than or equal to 95 percent.
The invention comprises the following steps: the quartz sand in step a is preferably graded particles with a particle size of 4.75mm or less.
The invention comprises the following steps: the steel moulds in step b are preferably triple steel moulds of dimensions 40mm in length by 40mm in width by 160mm in height.
The invention comprises the following steps: the compressive strength of the natural granite-like mineral solidified body prepared in the step d is more than or equal to 80MPa, and the flexural strength is more than or equal to 12 MPa.
The invention comprises the following steps: the natural granite-like mineral solidified body prepared in the step d is mainly used for solidifying various types of solid and liquid radioactive wastes.
Compared with the prior art, the invention has the following characteristics and beneficial effects:
(1) according to the invention, after metakaolin, potash water glass and silica micropowder are mixed with water, alkali-activated reaction is carried out, the reaction product is zeolite-like gel, the zeolite-like structure of the gel can adsorb and solidify various heavy metals and nuclide ions at room temperature, and the gel also has a binder effect;
(2) by adopting the invention, the slurry formed by injection molding is initially coagulated and hardened at room temperature, then after hydrothermal treatment, zeolite-like gel is crystallized and transformed into mineral structures like feldspar, potash feldspar and the like, and then the doped quartz sand is added, so that the formed mineral solidified body not only has excellent mechanical property, but also contains several main minerals of natural granite: such as quartz, potassium feldspar and feldspar-like silicate minerals. That is, the prepared mineral solidified body has a natural granite-like structure and properties; the compressive strength of the natural granite-like mineral solidified body prepared by the invention is more than or equal to 80MPa, and the flexural strength is more than or equal to 12 MPa.
(3) By adopting the invention, the composition, the structure and the performance of the mineral solidified body are similar to those of natural granite, and the mineral solidified body is particularly suitable for solidifying radioactive wastes; when the material is used as a base material to solidify radioactive waste, nuclide ions of the radioactive waste firstly enter the zeolite-like gel and then synchronously enter mineral crystal structures like feldspar, potassium feldspar and the like in a hydrothermal environment, so that the low-temperature lattice solidification of the nuclide ions is realized. The formed mineral solidified body has various advanced performances with natural granite and is a better multiple solidified body;
(4) by adopting the invention, the preparation temperature of the mineral solidified body is low, the condition is mild, the process is simple, various raw materials are easy to obtain, and the cost is low; the mineral solidified body has stable structure and high mechanical property, is easy to treat radioactive wastes in an industrial scale and has strong practicability.
Drawings
FIG. 1 is an X-ray diffraction pattern of a product of a mineral solidified body similar to natural granite obtained in example 4, and FIG. 1 shows that the product of example 4 is mainly composed of feldspar (potassium feldspar, analcite or leucite) and quartz, which is close to the mineral composition of natural granite;
FIG. 2 is a photograph showing the appearance of a mineral solidified body of natural granite obtained in example 4, and FIG. 2 shows that the product of example 4 has a white reddish appearance similar to that of natural granite.
Detailed Description
The following examples are intended to further illustrate the present invention and should not be construed as limiting the scope of the invention, which is intended to be covered by the claims appended hereto.
Example 1:
a hydrothermal preparation method of a natural granite-like mineral solidified body comprises the following steps: taking the raw materials according to the weight ratio of 100 parts by weight of metakaolin, 90 parts by weight of potash water glass, 25 parts by weight of silicon dioxide micropowder and 170 parts by weight of quartz sand, adding 25 parts by weight of water, mixing and stirring to prepare uniform slurry; injecting the slurry into a steel mould, and standing for 1-3 h at room temperature; then placing the steel mould filled with the slurry in an autoclave at the temperature of 200 ℃ for 10 hours; and (4) cooling the autoclave, taking out the mold with the sample, and demolding to obtain the natural granite-like mineral solidified body.
Example 2:
a hydrothermal preparation method of a natural granite-like mineral solidified body comprises the following steps: taking the raw materials according to the weight ratio of 100 parts by weight of metakaolin, 90 parts by weight of potash water glass, 53 parts by weight of silicon dioxide micropowder and 200 parts by weight of quartz sand, adding 55 parts by weight of water, mixing and stirring to prepare uniform slurry; injecting the slurry into a steel mould, and standing for 1-3 h at room temperature; then placing the steel mould filled with the slurry in an autoclave at the temperature of 200 ℃ for 10 hours; and (4) cooling the autoclave, taking out the mold with the sample, and demolding to obtain the natural granite-like mineral solidified body.
Example 3:
a hydrothermal preparation method of a natural granite-like mineral solidified body comprises the following steps: taking the raw materials according to the weight ratio of 100 parts by weight of metakaolin, 90 parts by weight of potash water glass, 80 parts by weight of silicon dioxide micropowder and 230 parts by weight of quartz sand, adding 70 parts by weight of water, mixing and stirring to prepare uniform slurry; injecting the slurry into a steel mould, and standing for 1-3 h at room temperature; then placing the steel mould filled with the slurry in an autoclave at the temperature of 200 ℃ for 10 hours; and (4) cooling the autoclave, taking out the mold with the sample, and demolding to obtain the natural granite-like mineral solidified body.
Example 4:
a hydrothermal preparation method of a natural granite-like mineral solidified body comprises the following steps: taking the raw materials according to the weight ratio of 100 parts by weight of metakaolin, 90 parts by weight of potash water glass, 105 parts by weight of silicon dioxide micropowder and 250 parts by weight of quartz sand, adding 85 parts by weight of water, mixing and stirring to prepare uniform slurry; injecting the slurry into a steel mould, and standing for 1-3 h at room temperature; then placing the steel mould filled with the slurry in an autoclave at the temperature of 200 ℃ for 10 hours; and (4) cooling the autoclave, taking out the mold with the sample, and demolding to obtain the natural granite-like mineral solidified body.
Example 5:
a hydrothermal preparation method of a natural granite-like mineral solidified body comprises the following steps: taking the raw materials according to the weight ratio of 100 parts by weight of metakaolin, 90 parts by weight of potash water glass, 0 part by weight of silicon dioxide micropowder and 300 parts by weight of quartz sand, adding 30 parts by weight of water, mixing and stirring to prepare uniform slurry; injecting the slurry into a steel mould, and standing for 1-3 h at room temperature; then placing the steel mould filled with the slurry in an autoclave at the temperature of 200 ℃ for 10 hours; and (4) cooling the autoclave, taking out the mold with the sample, and demolding to obtain the natural granite-like mineral solidified body.
Example 6:
a hydrothermal preparation method of a natural granite-like mineral solidified body comprises the following steps: taking the raw materials according to the weight ratio of 100 parts by weight of metakaolin, 100 parts by weight of potash water glass, 0 part by weight of silicon dioxide micropowder and 250 parts by weight of quartz sand, adding 30 parts by weight of water, mixing and stirring to prepare uniform slurry; injecting the slurry into a steel mould, and standing for 1-3 h at room temperature; then placing the steel mould filled with the slurry in an autoclave at the temperature of 200 ℃ for 10 hours; and (4) cooling the autoclave, taking out the mold with the sample, and demolding to obtain the natural granite-like mineral solidified body.
Example 7:
a hydrothermal preparation method of a natural granite-like mineral solidified body comprises the following steps: taking the raw materials according to the weight ratio of 100 parts by weight of metakaolin, 110 parts by weight of potash water glass, 0 part by weight of silicon dioxide micropowder and 200 parts by weight of quartz sand, adding 30 parts by weight of water, mixing and stirring to prepare uniform slurry; injecting the slurry into a steel mould, and standing for 1-3 h at room temperature; then placing the steel mould filled with the slurry in an autoclave at the temperature of 200 ℃ for 10 hours; and (4) cooling the autoclave, taking out the mold with the sample, and demolding to obtain the natural granite-like mineral solidified body.
Example 8:
a hydrothermal preparation method of a natural granite-like mineral solidified body comprises the following steps: taking the raw materials according to the weight ratio of 100 parts by weight of metakaolin, 120 parts by weight of potash water glass, 0 part by weight of silicon dioxide micropowder and 160 parts by weight of quartz sand, adding 25 parts by weight of water, mixing and stirring to prepare uniform slurry; injecting the slurry into a steel mould, and standing for 1-3 h at room temperature; then placing the steel mould filled with the slurry in an autoclave at the temperature of 200 ℃ for 10 hours; and (4) cooling the autoclave, taking out the mold with the sample, and demolding to obtain the natural granite-like mineral solidified body.
The mechanical properties of the natural granite-like mineral solidified body prepared in the embodiments 1 to 8 are as follows:
example 9 to example 12:
a hydrothermal preparation method of a natural granite-like mineral solidified body comprises the following steps: an experiment was carried out in the same manner as in example 4, except that the hydrothermal temperature was changed, and the reaction was carried out in a hydrothermal environment of 180 ℃, 220 ℃, 240 ℃ and 260 ℃.
Example 13 to example 15:
a hydrothermal preparation method of a natural granite-like mineral solidified body comprises the following steps: an experiment was carried out in the same manner as in example 4, except that the hydrothermal reaction time was changed and the reaction was carried out under hydrothermal conditions of 8 hours, 9 hours and 12 hours.
Example 16:
a hydrothermal preparation method of a natural granite-like mineral solidified body comprises the following steps:
a. taking raw materials according to the weight ratio of 100 parts by weight of metakaolin, 90 parts by weight of potash water glass and 150 parts by weight of quartz sand, adding 25 parts by weight of water, mixing and stirring to prepare uniform slurry;
b. injecting the slurry into a steel mould, and standing for 1h at room temperature;
c. then placing the steel mould filled with the slurry in an autoclave at the temperature of 180 ℃ for 12 hours;
d. and (c) cooling the autoclave, taking out the mold with the sample (the sample is the reaction product of the slurry in the step (c) after 12 hours in the autoclave at the temperature of 180 ℃), and demolding to prepare the natural granite-like mineral solidified body.
Example 17:
a hydrothermal preparation method of a natural granite-like mineral solidified body comprises the following steps:
a. taking the raw materials according to the weight ratio of 100 parts by weight of metakaolin, 120 parts by weight of potash water glass and 300 parts by weight of quartz sand, adding 85 parts by weight of water, mixing and stirring to prepare uniform slurry;
b. injecting the slurry into a steel mould, and standing for 3 hours at room temperature;
c. then placing the steel mould filled with the slurry in an autoclave at the temperature of 260 ℃ for 8 hours;
d. and (c) cooling the autoclave, taking out the mold with the sample (the sample is the reaction product of the slurry in the step (c) in the autoclave at the temperature of 260 ℃ for 8 hours), and demolding to obtain the natural granite mineral-like solidified body.
Example 18:
a hydrothermal preparation method of a natural granite-like mineral solidified body comprises the following steps:
a. taking raw materials according to the weight ratio of 100 parts by weight of metakaolin, 105 parts by weight of potash water glass and 225 parts by weight of quartz sand, adding 55 parts by weight of water, mixing and stirring to prepare uniform slurry;
b. injecting the slurry into a steel mould, and standing for 2 hours at room temperature;
c. then placing the steel mould filled with the slurry in an autoclave at the temperature of 220 ℃ for 10 hours;
d. and (c) cooling the autoclave, taking out the mold with the sample (the sample is the reaction product of the slurry in the step (c) in the autoclave at the temperature of 220 ℃ for 10 hours), and demolding to obtain the natural granite mineral-like solidified body.
Example 19:
a hydrothermal preparation method of a natural granite-like mineral solidified body comprises the following steps: taking the raw materials according to the weight ratio of 100 parts by weight of metakaolin, 90 parts by weight of potash water glass, 0.1 part by weight of silicon dioxide micropowder and 150 parts by weight of quartz sand, adding 25 parts by weight of water, mixing and stirring to prepare uniform slurry; the same as in any of examples 16 to 18, however, are omitted.
Example 20:
a hydrothermal preparation method of a natural granite-like mineral solidified body comprises the following steps: taking the raw materials according to the weight ratio of 100 parts by weight of metakaolin, 120 parts by weight of potash water glass, 105 parts by weight of silicon dioxide micropowder and 300 parts by weight of quartz sand, adding 85 parts by weight of water, mixing and stirring to prepare uniform slurry; the same as in any of examples 16 to 18, however, are omitted.
Example 21:
a hydrothermal preparation method of a natural granite-like mineral solidified body comprises the following steps: taking the raw materials according to the weight ratio of 100 parts by weight of metakaolin, 110 parts by weight of potash water glass, 53 parts by weight of silicon dioxide micropowder and 225 parts by weight of quartz sand, adding 55 parts by weight of water, mixing and stirring to prepare uniform slurry; the same as in any of examples 16 to 18, however, are omitted.
Example 22:
a hydrothermal preparation method of a natural granite-like mineral solidified body comprises the following steps: taking the raw materials according to the weight ratio of 100 parts by weight of metakaolin, 90-120 parts by weight of any potassium water glass, 0.1-105 parts by weight of any silicon dioxide micro powder and 150-300 parts by weight of any quartz sand, adding any water in 25-85 parts by weight, mixing and stirring to obtain uniform slurry; the same as in any of examples 16 to 18, however, are omitted.
In the above embodiment: the metakaolin in the step a mainly comprises the chemical components and the weight percentage of SiO2 50～55％、Al2O340-45% of other trace components (e.g. Fe)2O3、Na2O、K2O, CaO, etc.) 3% -5%, and the sum of all the components is 100%; the metakaolin is K1300 type metakaolin produced by inner Mongolia super-brand kaolin company Limited.
In the above embodiment: the main chemical composition and weight percentage of the potash water glass in the step a are SiO2 22～28％、K2O 21～35％、H2O43-50%, and the sum of all the components is 100%.
In the above embodiment: oxidation as described in step aThe silicon micropowder can be one or more of superfine quartz powder, silica fume, diatomaceous earth, nanometer silica and white carbon black, and has particle diameter of less than 1 μm and SiO in the silica micropowder2The weight percentage content is more than or equal to 95 percent.
In the above embodiment: the quartz sand in the step a is graded particles with the particle size of less than 4.75 mm.
In the above embodiment: the steel mould in step b is a triple steel mould with dimensions of 40mm length by 40mm width by 160mm height.
In the above embodiment: the compressive strength of the natural granite-like mineral solidified body prepared in the step d is more than or equal to 80MPa, and the flexural strength is more than or equal to 12 MPa.
In the above embodiment: the natural granite-like mineral solidified body prepared in the step d is mainly used for solidifying various types of solid and liquid radioactive wastes.
In the above embodiment: all the raw materials are commercially available products.
In the above embodiment: the percentages used, not specifically noted, are weight (mass) percentages or percentages known to those skilled in the art; the parts by weight (mass) may be both grams or kilograms.
In the above embodiment: the process parameters (temperature, time, etc.) and the numerical values of the components in each step are in the range, and any point can be applicable.
The present invention and the technical contents not specifically described in the above embodiments are the same as the prior art.
In the above embodiments, only different dosages of metakaolin, potash water glass, silica micropowder and quartz sand are selected to perform hydrothermal preparation of the natural granite-like mineral solidified body, and those skilled in the art can easily make different modifications on the basis of the embodiments, and apply the general principles described herein to other embodiments without creative work, so that the present invention is not limited to the above embodiments; those skilled in the art, having the benefit of this disclosure, will appreciate that many modifications and variations are possible in the light of the above teachings without departing from the scope of the invention, as defined in the appended claims.
Claims (8)
1. A hydrothermal preparation method of a natural granite-like mineral solidified body is characterized by comprising the following steps:
a. taking raw materials according to the weight ratio of 100 parts by weight of metakaolin, 90-120 parts by weight of potash water glass, 0.1-105 parts by weight of silica micropowder and 150-300 parts by weight of quartz sand, adding 25-85 parts by weight of water, mixing and stirring to prepare uniform slurry;
b. injecting the slurry into a steel mould, and standing for 1-3 h at room temperature;
c. then placing the steel mould filled with the slurry in an autoclave at the temperature of 180-260 ℃ for 8-12 h;
d. and cooling the autoclave, taking out the mold with the sample, and demolding to obtain the natural granite mineral-like solidified body.
2. The hydrothermal preparation method of the natural granite mineral-like solidified body as set forth in claim 1, characterized in that: the metakaolin in the step a mainly comprises the chemical components and the weight percentage of SiO2 50～55 %、Al2O340-45% and 3% -5% of other trace components.
3. The hydrothermal preparation method of the natural granite mineral-like solidified body as set forth in claim 1, characterized in that: the main chemical composition and weight percentage of the potash water glass in the step a are SiO2 22～28%、K2O 21～35%、H2O 43～50%。
4. The hydrothermal preparation method of the natural granite mineral-like solidified body as set forth in claim 1, characterized in that: the silicon dioxide micro powder in the step a is one or a mixture of more than two of superfine quartz powder, silica fume, diatomite, nano silicon dioxide and white carbon black.
5. The hydrothermal preparation method of the natural granite mineral-like solidified body as set forth in claim 1, characterized in that: the quartz sand in the step a is graded particles with the particle size of less than 4.75 mm.
6. The hydrothermal preparation method of the natural granite mineral-like solidified body as set forth in claim 1, characterized in that: the steel mould in step b is a triple steel mould with dimensions of 40mm length by 40mm width by 160mm height.
7. The hydrothermal preparation method of the natural granite mineral-like solidified body as set forth in claim 1, characterized in that: the compressive strength of the natural granite-like mineral solidified body prepared in the step d is more than or equal to 80MPa, and the flexural strength is more than or equal to 12 MPa.
8. The hydrothermal preparation method of the natural granite mineral-like solidified body as set forth in claim 1, characterized in that: the natural granite-like mineral solidified body prepared in the step d is mainly used for solidifying various types of solid and liquid radioactive wastes.
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