CN113698142B - Cold-sintered diatomite porous material and preparation method thereof - Google Patents
Cold-sintered diatomite porous material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to the field of porous materials, in particular to a cold-sintered diatomite porous material and a preparation method thereof. The preparation method of the cold-sintered diatomite porous material comprises the following steps: step 1, adding an alkaline solution into diatomite, and uniformly mixing the alkaline solution and the diatomite to prepare a paste; step 2, placing the paste into a mold, and keeping the mold for a set time under the conditions of preset pressure and preset temperature, wherein the preset temperature is room temperature-150 ℃; and 3, obtaining the block product in the mold, namely the cold-sintered diatomite porous material. The cold-sintered diatomite porous material is prepared by the method, and the bending strength of the porous material is more than 40 MPa. The cold-sintered diatomite porous material has higher specific surface area, adsorbability and carrier property.
Description
Technical Field
The invention relates to the field of porous materials, in particular to a cold-sintered diatomite porous material and a preparation method thereof.
Background
The diatomite is a porous natural mineral and is mainly formed by piling up dead porous shells of diatoms, and the single-particle diatom shell has a unique macroporous structure and high-efficiency adsorbability and is a natural adsorbing material and a carrier. However, when the diatom, the diatom is used as a powder material adsorbent, the problem that the efficiency of diffusion mass transfer is low, the recovery is not easy and the like exists often, and therefore the diatom is prepared into a bulk material, such as porous ceramic and the like, and the diatom is used for adsorbing water, atmospheric pollutants and the like.
It must be pointed out, however, that conventional sintering processes generally require the calcination of the diatomaceous earth at relatively high temperatures (. gtoreq.800 ℃) in order to ensure the structural stability and the compressive capacity of the blocks formed. At such high temperatures, the macropores of the single diatomite particles are obviously collapsed, the macroporous structure gradually disappears, and more disadvantageously, at temperatures higher than 1000 ℃, the diatomite undergoes phase change to form a cristobalite phase, so that the porosity disappears, the specific surface is reduced, and the adsorptivity and carrier performance are reduced.
Disclosure of Invention
In view of the above, the present invention aims to provide a method for preparing a cold-sintered porous diatomite material by sintering diatomite at a low temperature, so as to solve the problems of collapse of macropores and gradual disappearance of a macroporous structure of single diatomite particles caused by high-temperature sintering.
In order to achieve the above purpose, the present invention mainly provides the following technical solutions:
a preparation method of a cold-sintered diatomite porous material comprises the following steps:
step 1, adding an alkaline solution into diatomite, and uniformly mixing the alkaline solution and the diatomite to prepare a paste;
step 2, placing the paste into a mold, and keeping the mold for a set time under the conditions of preset pressure and preset temperature, wherein the preset temperature is room temperature-150 ℃;
and 3, obtaining the block product in the mold, namely the cold-sintered diatomite porous material.
In the preparation method of the cold-sintered diatomite porous material, the alkaline solution is a sodium hydroxide solution with a concentration of 0.1-3M.
In the preparation method of the cold-sintered diatomite porous material, the alkaline solution is a potassium hydroxide solution with a concentration of 0.1-3M.
In the preparation method of the cold-sintered diatomite porous material, SiO in the diatomite 2 The mass percentage of the component (A) is more than or equal to 70 percent.
In the preparation method of the cold-sintered diatomite porous material, the preset pressure is 100-300 MPa.
In the preparation method of the cold-sintered diatomite porous material, the set time is 1-5 min.
In the above preparation method of the cold-sintered diatomite porous material, the preset pressure is a pressure applied to the mold by using a mechanical strength tester.
A cold-sintered diatomite porous material prepared by the preparation method of any one of claims 1-7, wherein the bending strength of the porous material is more than 40 MPa.
In the cold-sintered diatomite porous material, the specific surface area of the porous material is 29-41 m 2 /g。
In the cold-sintered diatomite porous material, the density of the porous material is 1.45-1.88 g/cm 3 。
By the technical scheme, the cold-sintered diatomite porous material and the preparation method provided by the invention at least have the following advantages:
according to the preparation method provided by the embodiment of the invention, energy can be saved through low-temperature sintering, the original pore structure of the obtained diatomite porous material can not be changed, and the cold-sintered diatomite porous material keeps higher adsorbability and carrier property.
The foregoing description is only an overview of the technical solutions of the present invention, and in order to make the technical solutions of the present invention more clearly understood and to implement them in accordance with the contents of the description, the following detailed description is given with reference to the preferred embodiments of the present invention and the accompanying drawings.
Drawings
FIG. 1 is a scanning electron microscope image of a cold-sintered diatomite porous material provided in example 1 of the present invention.
Detailed Description
To further illustrate the technical means and effects of the present invention adopted to achieve the predetermined objects, the following detailed description will be given to the specific embodiments, structures, characteristics and effects of the cold-sintered diatomite porous material and the preparation method thereof according to the present invention with reference to the accompanying drawings and preferred embodiments. In the following description, different "one embodiment" or "an embodiment" refers to not necessarily the same embodiment. Furthermore, the particular features, structures, or characteristics may be combined in any suitable manner in one or more embodiments.
Example 1
The embodiment discloses a preparation method of a cold-sintered diatomite porous material, which comprises the following steps: step 1, adding 3mol/L alkaline solution of sodium hydroxide solution into diatomite, and uniformly mixing the sodium hydroxide solution and the alkaline solution to prepare paste; step 2, placing the paste into a mold, and keeping the mold for 1 minute at the temperature of 150 ℃ and the pressure of 100 MPa; and 3, cold sintering the paste in the mold into a blocky product, namely cold sintering the diatomite porous material.
In this example, SiO in the diatomaceous earth 2 The mass percentage of the component (A) is more than or equal to 70 percent.
In the embodiment, the diatomite can be sintered at a lower temperature (less than or equal to 150 ℃), so that on one hand, energy is saved, on the other hand, the original pore structure of the diatomite is not changed, and the cold-sintered diatomite porous material keeps higher adsorbability and carrier property.
The reaction equation of the preparation method of the cold-sintered diatomite porous material is as follows:
-Si-O-Si-OH+OH-Si-O-Si-→-Si-O-Si-O-Si-O-Si-+H 2 O
in this example, a scanning electron microscope image of the obtained cold-sintered diatomite porous material is shown in fig. 1, in which we can clearly see the morphology of the cold-sintered diatomite porous material, and the cold-sintered diatomite porous material has no pore loss.
Further, it was determined that: the bending strength of the porous material is more than 40 MPa; the specific surface area of the porous material is 39.3m 2 The density of the porous material is 1.70 +/-0.01 g/cm 3 。
Example 2
The embodiment discloses a preparation method of a cold-sintered diatomite porous material, which is different from the embodiment 1 in that: in step 2, the mold was held at a temperature of 150 ℃ and a pressure of 100MPa for 2 minutes. The specific surface area of the resulting porous material was 35.8m 2 Per g, density of 1.75 + -0.01 g/cm 3 。
Example 3
The embodiment discloses a preparation method of a cold-sintered diatomite porous material, which is different from the embodiment 1 in that: in step 2, the mold was held at a temperature of 150 ℃ and a pressure of 100MPa for 3 minutes. The specific surface area of the resulting porous material was 33.4m 2 (ii) a density of 1.77. + -. 0.02g/cm 3.
Example 4
The embodiment discloses a preparation method of a cold-sintered diatomite porous material, which is different from the embodiment 1 in that: in step 2, the mold was held at a temperature of 150 ℃ and a pressure of 200MPa for 1 minute. The specific surface area of the resulting porous material was 35.9m 2 Per g, density of 1.85 + -0.01 g/cm 3 。
Example 5
The embodiment discloses a preparation method of a cold-sintered diatomite porous material, which is different from the embodiment 1 in that: in step 2, the mold was held at a temperature of 150 ℃ and a pressure of 200MPa for 2 minutes. The specific surface area of the resulting porous material was 34.3m 2 (ii) a density of 1.90. + -. 0.01g/cm 3 。
Example 6
The embodiment discloses a preparation method of a cold-sintered diatomite porous material, which is different from the embodiment 1 in that: in step 2, the mold was held at a temperature of 150 ℃ and a pressure of 200MPa for 3 minutes. The specific surface area of the obtained porous material was 30.3m 2 (ii)/g, density 1.93 + -0.02 g/cm 3 。
Example 7
The embodiment discloses a cold sinteringThe preparation method of the kieselguhr porous material is different from the preparation method of the kieselguhr porous material in that: in step 2, the mold was held at a temperature of 150 ℃ and a pressure of 300MPa for 1 minute. The specific surface area of the obtained porous material was 37.2m 2 (ii)/g, density is 1.94 +/-0.01 g/cm 3 。
Example 8
The embodiment discloses a preparation method of a cold-sintered diatomite porous material, which is different from the embodiment 1 in that: in step 2, the mold was held at a temperature of 150 ℃ and a pressure of 300MPa for 2 minutes. The specific surface area of the obtained porous material was 30.4m 2 (ii)/g, density of 2.04 + -0.01 g/cm 3 。
Example 9
The embodiment discloses a preparation method of a cold-sintered diatomite porous material, which is different from the embodiment 1 in that: in step 2, the mold was held at a temperature of 150 ℃ and a pressure of 300MPa for 3 minutes. The specific surface area of the resulting porous material was 29.8m 2 (ii)/g, density of 2.05 + -0.01 g/cm 3 。
Example 10
The embodiment discloses a preparation method of a cold-sintered diatomite porous material, which is different from the embodiment 1 in that: in step 2, the mold was held at room temperature under a pressure of 100MPa for 1 minute. The specific surface area of the obtained porous material was 40.2m 2 (ii)/g, density 1.43 + -0.02 g/cm 3 。
Example 11
The embodiment discloses a preparation method of a cold-sintered diatomite porous material, which is different from the preparation method of the embodiment 1 in that: in step 2, the mold was held at room temperature under a pressure of 100MPa for 2 minutes. The specific surface area of the resulting porous material was 37.7m 2 (ii)/g, density 1.45 + -0.02 g/cm 3 。
Example 12
The embodiment discloses a preparation method of a cold-sintered diatomite porous material, which is different from the embodiment 1 in that: in step 2, the mold was held at room temperature under a pressure of 100MPa for 3 minutes. Proportion of the obtained porous MaterialThe area is 33.6m 2 (ii)/g, density 1.46 + -0.01 g/cm 3 。
Example 13
The embodiment discloses a preparation method of a cold-sintered diatomite porous material, which is different from the embodiment 1 in that: in step 2, the mold was held at room temperature under a pressure of 200MPa for 1 minute. The specific surface area of the obtained porous material was 38.4m 2 (ii)/g, density 1.48 + -0.02 g/cm 3 。
Example 14
The embodiment discloses a preparation method of a cold-sintered diatomite porous material, which is different from the embodiment 1 in that: in step 2, the mold was held at room temperature under a pressure of 200MPa for 2 minutes. The specific surface area of the obtained porous material was 37.8m 2 (ii)/g, density 1.49 + -0.01 g/cm 3 。
Example 15
The embodiment discloses a preparation method of a cold-sintered diatomite porous material, which is different from the embodiment 1 in that: in step 2, the mold was held at room temperature under a pressure of 200MPa for 3 minutes. The specific surface area of the resulting porous material was 33.6m 2 (ii)/g, density 1.49 + -0.02 g/cm 3 。
Example 16
The embodiment discloses a preparation method of a cold-sintered diatomite porous material, which is different from the embodiment 1 in that: in step 2, the mold was held at room temperature under a pressure of 300MPa for 1 minute. The specific surface area of the resulting porous material was 35.3m 2 (ii)/g, density 1.52 + -0.01 g/cm 3 。
Example 17
The embodiment discloses a preparation method of a cold-sintered diatomite porous material, which is different from the embodiment 1 in that: in step 2, the mold was held at room temperature under a pressure of 300MPa for 2 minutes. The specific surface area of the obtained porous material was 30.0m 2 (ii)/g, density 1.52 + -0.02 g/cm 3 。
Example 18
The embodiment discloses a cold-sintered diatomite porous materialThe difference from example 1 is that: in step 2, the mold was held at room temperature under a pressure of 300MPa for 3 minutes. The specific surface area of the obtained porous material was 30.4m 2 (ii)/g, density 1.52 + -0.02 g/cm 3 。
Example 19
The embodiment discloses a preparation method of a cold-sintered diatomite porous material, which is different from the embodiment 1 in that: in step 1, the concentration of sodium hydroxide was 0.1M, and the mold was kept at a temperature of 150 ℃ and a pressure of 100MPa for 2 minutes. The density of the obtained porous material is 1.52 +/-0.01 g/cm 3 。
Example 20
The embodiment discloses a preparation method of a cold-sintered diatomite porous material, which is different from the embodiment 1 in that: in step 1, the concentration of sodium hydroxide was 0.5M, and the mold was kept at a temperature of 150 ℃ and a pressure of 100MPa for 3 minutes. The density of the obtained porous material is 1.55 +/-0.01 g/cm 3 。
Example 21
The embodiment discloses a preparation method of a cold-sintered diatomite porous material, which is different from the embodiment 1 in that: in step 1, the concentration of sodium hydroxide was 1M, and the mold was kept at a temperature of 150 ℃ and a pressure of 100MPa for 3 minutes. The density of the obtained porous material is 1.65 +/-0.01 g/cm 3 。
Example 22
The embodiment discloses a preparation method of a cold-sintered diatomite porous material, which is different from the embodiment 1 in that: in step 1, the concentration of sodium hydroxide was 0.1M, and the mold was kept at a temperature of 150 ℃ and a pressure of 200MPa for 2 minutes. The density of the obtained porous material is 1.64 +/-0.01 g/cm 3 。
Example 23
The embodiment discloses a preparation method of a cold-sintered diatomite porous material, which is different from the embodiment 1 in that: in step 1, the concentration of sodium hydroxide was 0.5M, and the mold was kept at a temperature of 150 ℃ and a pressure of 200MPa for 3 minutes. Density of the resulting porous materialIs 1.70 +/-0.01 g/cm 3 。
Example 24
The embodiment discloses a preparation method of a cold-sintered diatomite porous material, which is different from the embodiment 1 in that: in step 1, the concentration of sodium hydroxide was 1M, and the mold was kept at a temperature of 150 ℃ and a pressure of 200MPa for 3 minutes. The density of the obtained porous material is 1.77 +/-0.01 g/cm 3 。
Example 25
The embodiment discloses a preparation method of a cold-sintered diatomite porous material, which is different from the embodiment 1 in that: in step 1, the concentration of sodium hydroxide was 0.1M, and the mold was kept at a temperature of 150 ℃ and a pressure of 300MPa for 2 minutes. The density of the obtained porous material is 1.75 +/-0.02 g/cm 3 。
Example 26
The embodiment discloses a preparation method of a cold-sintered diatomite porous material, which is different from the embodiment 1 in that: in step 1, the concentration of sodium hydroxide was 0.5M, and the mold was kept at a temperature of 150 ℃ and a pressure of 300MPa for 3 minutes. The density of the obtained porous material is 1.78 +/-0.02 g/cm 3 。
Example 27
The embodiment discloses a preparation method of a cold-sintered diatomite porous material, which is different from the embodiment 1 in that: in step 1, the concentration of sodium hydroxide was 1M, and the mold was kept at a temperature of 150 ℃ and a pressure of 300MPa for 3 minutes. The density of the obtained porous material is 1.86 +/-0.02 g/cm 3 。
Example 28
The embodiment discloses a preparation method of a cold-sintered diatomite porous material, which is different from the embodiment 1 in that: in step 1, the concentration of sodium hydroxide was 0.1M, and the mold was kept at room temperature under a pressure of 100MPa for 1 minute. The density of the obtained porous material is 1.47 +/-0.02 g/cm 3 。
Example 29
This example discloses a method for preparing cold-sintered diatomite porous material, which is similar to example 1The differences are as follows: in step 1, the concentration of sodium hydroxide was 0.1M, and the mold was kept at room temperature under a pressure of 200MPa for 1 minute. The density of the obtained porous material is 1.50 +/-0.02 g/cm 3 。
Example 30
The embodiment discloses a preparation method of a cold-sintered diatomite porous material, which is different from the embodiment 1 in that: in step 1, the concentration of sodium hydroxide was 1M, and the mold was kept at room temperature under a pressure of 300MPa for 1 minute. The density of the obtained porous material is 1.53 +/-0.02 g/cm 3 。
Comparative example
The applicant has made relevant comparative examples for specific embodiments of high temperature sintered diatomaceous earth, and the specific experimental results refer to the following table:
| comparative example | Sintering temperature | Sintering pressure | Density (g cm) -3 ) | Specific surface area (m) 2 /g) |
| Comparative example 1 | 800℃ | Atmospheric pressure | 1.17±0.02 | 8.7 |
| Comparative example 2 | 900℃ | Atmospheric pressure | 1.18±0.02 | 8.2 |
| Comparative example 3 | 1000℃ | Atmospheric pressure | 1.22±0.02 | 6.5 |
| Comparative example 4 | 1100℃ | Atmospheric pressure | 1.60±0.02 | 5.9 |
| Comparative example 5 | 1200℃ | Atmospheric pressure | 1.91±0.02 | 5.2 |
The preparation method of the low-temperature sintering diatomite porous material disclosed by the application can ensure that the original pore structure of the diatomite does not change, the specific surface area is far higher than a high-temperature sintering product, and the higher specific surface area can also ensure that the low-temperature sintering diatomite porous material has higher adsorbability and carrier property.
The above description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and any simple modification, equivalent change and modification made to the above embodiment according to the technical spirit of the present invention are still within the scope of the technical solution of the present invention.
Claims (9)
1. The preparation method of the cold-sintered diatomite porous material is characterized by comprising the following steps:
step 1, adding an alkaline solution into diatomite, and uniformly mixing the alkaline solution and the diatomite to prepare a paste;
step 2, placing the paste into a mold, and keeping the mold for a set time under the conditions of a preset pressure and a preset temperature, wherein the preset pressure is 100-300 MPa, and the preset temperature is room temperature-150 ℃;
and 3, obtaining the block product in the mold, namely the cold-sintered diatomite porous material.
2. The method for preparing a cold-sintered diatomite porous material according to claim 1,
the alkaline solution is a sodium hydroxide solution with the concentration of 0.1-3M.
3. The method for preparing a cold-sintered diatomite porous material according to claim 1,
the alkaline solution is potassium hydroxide solution with the concentration of 0.1-3M.
4. The method for preparing a cold-sintered diatomite porous material according to claim 1,
SiO in the diatomaceous earth 2 The mass percentage of the component (A) is more than or equal to 70 percent.
5. The method for preparing a cold-sintered diatomite porous material according to claim 1,
the set time is 1-5 min.
6. The method for preparing a cold-sintered diatomite porous material according to claim 1,
the preset pressure is a pressure applied to the mold by using a mechanical strength tester.
7. A cold-sintered diatomite porous material prepared by the preparation method of any one of claims 1-6, wherein the flexural strength of the porous material is more than 40 MPa.
8. The cold-sintered diatomite porous material of claim 7,
the specific surface area of the porous material is 29-41 m 2 /g。
9. The cold-sintered diatomite porous material of claim 7,
the density of the porous material is 1.45-1.88 g/cm 3 。
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