CN114367268A - Diatomite and modification method and application thereof - Google Patents

Diatomite and modification method and application thereof Download PDF

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Publication number
CN114367268A
CN114367268A CN202210038621.3A CN202210038621A CN114367268A CN 114367268 A CN114367268 A CN 114367268A CN 202210038621 A CN202210038621 A CN 202210038621A CN 114367268 A CN114367268 A CN 114367268A
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diatomite
mixture
diatomaceous earth
modification method
modification
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任子杰
郭争争
高惠
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Wuhan University of Technology WUT
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
    • B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
    • B01J20/14—Diatomaceous earth
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D37/00—Processes of filtration
    • B01D37/02—Precoating the filter medium; Addition of filter aids to the liquid being filtered
    • B01D37/025—Precoating the filter medium; Addition of filter aids to the liquid being filtered additives incorporated in the filter
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
    • B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
    • B01J20/28054—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their surface properties or porosity
    • B01J20/28057—Surface area, e.g. B.E.T specific surface area
    • B01J20/28059—Surface area, e.g. B.E.T specific surface area being less than 100 m2/g
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J29/00—Catalysts comprising molecular sieves
    • B01J29/04—Catalysts comprising molecular sieves having base-exchange properties, e.g. crystalline zeolites
    • B01J29/06—Crystalline aluminosilicate zeolites; Isomorphous compounds thereof
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
    • B01J35/39—Photocatalytic properties

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  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
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  • Crystallography & Structural Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Inorganic Chemistry (AREA)
  • Solid-Sorbent Or Filter-Aiding Compositions (AREA)

Abstract

The invention provides diatomite and a modification method and application thereof, wherein the modification method of the diatomite comprises the following steps: mixing diatomite and sodium hydroxide to obtain a mixture; adding water into the mixture to obtain a mixture; placing the mixture in a still kettle, and reacting to obtain a reaction product; and washing the reaction product to be neutral, and drying to finish the modification of the diatomite. According to the modification method, sodium hydroxide is used as a modifier, hydrothermal reaction is carried out in an autoclave, the modified calcined diatomite has a high specific surface area, and zeolite newly generated on the surface of the diatomite has high adsorption performance on dye, so that the modified calcined diatomite has the high specific surface area and a good dye removal effect; the diatomite modification method is simple in operation and flow, low in raw material price, large in specific surface area of modified roasted diatomite and good in adsorption effect, can be used as a filter aid, an adsorbent, a photocatalytic carrier and the like, and application of the roasted diatomite is expanded.

Description

Diatomite and modification method and application thereof
Technical Field
The invention relates to the technical field of deep processing of nonmetallic mineral materials, in particular to diatomite and a modification method and application thereof.
Background
Diatomite is a biogenic siliceous sedimentary rock, the main chemical component of which is SiO2And also a small amount of Al2O3、Fe2O3And CaO, and the like, and in addition, the diatomite ore often contains part of organic matters. China diatomaceous earth is rich in mineral resources and is located in the 2 nd place of the world. The method is mainly distributed in Jilin province in China, and accounts for 54.8 percent of the total reserves in China, and is inferior to Yunnan province, Fujian province and the like. Due to the special structure of the diatomite, the diatomite has a plurality of excellent physical properties and chemical properties such as light weight, fire resistance, acid resistance, large specific surface area, high adsorbability, stable chemical properties and the like. Therefore, the diatom can be used as a filter aid, an adsorbent, a catalytic carrier and the like, and is widely applied to various fields of food, environmental protection, medicine, construction, agriculture and the like
Diatomite often needs to be purified because the diatomite contains more impurities. These impurities generally adhere to the outer shell of the diatomaceous earth or are present in the framework of the diatomaceous earth, severely blocking the micropores of the diatomaceous earth. Therefore, the natural diatomite needs to be modified or purified to increase the specific surface area. The roasting method is widely applied to the purification process. However, during the calcination process, since the calcination temperature is high, the original pore structure of the diatomite is reduced in a molten state or molten diatomite fragments are adhered to the diatomite shell, so that the specific surface area of the diatomite is reduced. In addition, the roasting enables silicon hydroxyl groups rich on the surface of the diatomite to disappear, the adsorption performance of the diatomite to be greatly reduced, the application range of the diatomite is limited in the field of filter aids, and the application of the roasted diatomite is severely limited.
In order to overcome the defects existing in the prior diatomite modification, the improvement is needed.
Disclosure of Invention
In view of the above, the present invention provides a diatomite, a modification method thereof and an application thereof, so as to solve or partially solve the problems in the prior art.
In a first aspect, the present invention provides a method for modifying diatomaceous earth, comprising the steps of:
mixing diatomite and sodium hydroxide to obtain a mixture;
adding water into the mixture, and stirring to obtain a mixture;
placing the mixture in an autoclave, and reacting at 120-180 ℃ for 6-18 h to obtain a reaction product;
and washing the reaction product to be neutral, and drying to finish the modification of the diatomite.
Preferably, in the method for modifying diatomaceous earth, the diatomaceous earth is calcined diatomaceous earth.
Preferably, in the method for modifying diatomite, the mass of the sodium hydroxide is 1-10% of the mass of the diatomite.
Preferably, in the diatomite modification method, water is added into the mixture so that the solid-to-liquid ratio of the mixture is 1 (3-8).
Preferably, the diatomite modification method comprises the steps of washing a reaction product to be neutral, and drying to complete modification of the diatomite, wherein the drying temperature is 80-120 ℃.
In a second aspect, the invention also provides diatomite modified by the modification method.
In a third aspect, the invention also provides an application of the diatomite as a filter aid, an adsorbent and a photocatalytic carrier.
Compared with the prior art, the diatomite and the modification method and the application thereof have the following beneficial effects:
according to the method for modifying the diatomite, the roasted diatomite is used as a raw material, the sodium hydroxide is used as a modifier, and hydrothermal reaction is carried out in an autoclave to prepare the modified diatomite with a high specific surface area. After the diatomite is roasted at high temperature, Si-OH on the surface of the diatomite is changed into-Si-O-Si-bond, and a sodium-containing fluxing agent is added in the roasting process, so that a small amount of CaO and Na are contained on the surface of the roasted diatomite2O, etc. on the surface of the diatomite in a high-temperature closed environment2And Al2O3Can be mixed with CaO and Na2O, etc. to form coral-like zeolite phase crystals. The newly generated zeolite phase mineral has more pores, so that the specific surface area of the modified calcined diatomite is increased, and the original pores of the calcined diatomite cannot be blocked, therefore, the modified calcined diatomite has high specific surface area and better adsorption effect on the dye, and the zeolite has very high adsorption performance on the dye, so that the modified calcined diatomite has high specific surface area and better removal effect on the dye; the diatomite modification method is simple in operation and flow, low in raw material price, large in specific surface area of modified roasted diatomite and good in adsorption effect, can be used as a filter aid, an adsorbent, a photocatalytic carrier and the like, and application of the roasted diatomite is expanded.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below. It is obvious that the drawings in the following description are only some embodiments of the invention, and that for a person skilled in the art, other drawings can be derived from them without inventive effort.
FIG. 1 is an XRD pattern of a modified calcined diatomaceous earth used in example 1 of the present invention;
FIG. 2 is an XRD spectrum of the calcined diatomaceous earth of example 1 without modification;
FIGS. 3 to 4 are SEM images of the surface morphology of the modified calcined diatomaceous earth in example 1 of the present invention;
FIGS. 5 to 6 are SEM images of the surface morphology of the calcined diatomaceous earth in example 1 of the present invention.
Detailed Description
In the following, the technical solutions in the embodiments of the present invention will be clearly and completely described in conjunction with the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
The embodiment of the application provides a diatomite modification method, which comprises the following steps:
s1, mixing diatomite and sodium hydroxide to obtain a mixture;
s2, adding water into the mixture, and stirring to obtain a mixture;
s3, placing the mixture in an autoclave, and reacting at 120-180 ℃ for 6-18 h to obtain a reaction product;
and S4, washing the reaction product to be neutral, and drying to finish the modification of the diatomite.
In some embodiments, the diatomaceous earth is calcined diatomaceous earth. The roasted diatomite is the roasted diatomite.
In some embodiments, the sodium hydroxide is 1-10% by mass of the diatomaceous earth.
In some embodiments, water is added to the mixture so that the solid-to-liquid ratio of the mixture is 1 (3-8).
Specifically, the solid-liquid ratio is the mass ratio of the solid phase to the liquid phase in the mixture, i.e., the ratio of the mass sum of the diatomite and the sodium hydroxide to the mass of the water.
In some embodiments, the drying is performed to complete the modification of the diatomite, wherein the drying temperature is 80-120 ℃.
In some embodiments, step S3 is specifically: placing the mixture in a container, sealing, and then placing the container in an autoclave for hydrothermal reaction at 120-180 ℃ for 6-18 h to obtain a reaction product; the container is a ceramic crucible, the mixture is placed in the ceramic crucible, and then a cover is covered on the ceramic crucible, so that the entry of water vapor in the autoclave during hydrothermal reaction is avoided; meanwhile, before hydrothermal reaction, a certain amount of water needs to be added into the autoclave to be kept flush with the bottom plate of the sample holder, so that the ceramic crucible is prevented from being knocked down by boiling water due to excessive water in the autoclave.
The modification method of the diatomite takes the roasted diatomite as a raw material and takes sodium hydroxide as a raw materialThe modified diatomite with high specific surface area is prepared by performing hydrothermal reaction in an autoclave as a modifier. After the diatomite is roasted at high temperature, Si-OH on the surface of the diatomite is changed into-Si-O-Si-bond, and a sodium-containing fluxing agent is added in the roasting process, so that a small amount of CaO and Na are contained on the surface of the roasted diatomite2O, etc. on the surface of the diatomite in a high-temperature closed environment2And Al2O3Can be mixed with CaO and Na2O, etc. to form coral-like zeolite phase crystals. The newly generated zeolite phase mineral has more pores, so that the specific surface area of the modified calcined diatomite is increased, and the original pores of the calcined diatomite cannot be blocked, therefore, the modified calcined diatomite has high specific surface area and better adsorption effect on the dye, and the zeolite has very high adsorption performance on the dye, so that the modified calcined diatomite has high specific surface area and better removal effect on the dye; the diatomite modification method is simple in operation and flow, low in raw material price, large in specific surface area of modified roasted diatomite and good in adsorption effect, can be used as a filter aid, an adsorbent, a photocatalytic carrier and the like, and application of the roasted diatomite is expanded.
Based on the same inventive concept, the embodiment of the application also provides an application of the diatomite prepared by the modification method as a filter aid, an adsorbent and a photocatalytic carrier.
The modification method and application of diatomaceous earth of the present application are further described in the following examples, which are conventional methods unless otherwise specified. The experimental materials used in the present example were all purchased from the market unless otherwise specified; the calcined diatomaceous earth in the following examples is from Jilin Linjiang (SiO)287.02% by mass); NaOH was analytically pure.
Example 1
The embodiment of the application provides a diatomite modification method, which comprises the following steps:
s1, baking 10g of diatomite (SiO)287.02 percent of mass content) and sodium hydroxide are mixed to obtain a mixture; wherein the mass of the sodium hydroxide is 6 percent of that of the calcined diatomite;
s2, adding water into the mixed material according to the solid-liquid ratio of 1:3, and uniformly stirring to obtain a mixed material;
s3, placing the mixture in a crucible, covering the crucible with a crucible cover, placing the crucible in an autoclave, and carrying out hydrothermal reaction for 12 hours at 160 ℃ to obtain a reaction product;
and S4, washing the reaction product with water to be neutral, and drying and dehydrating at 100 ℃ to complete the modification of the diatomite and obtain the hydrothermal modified calcined diatomite.
Example 2
The method for modifying diatomaceous earth provided in the present application example is the same as example 1, except that the mass of sodium hydroxide in step S1 is 4% of the mass of calcined diatomaceous earth, and the rest of the processes are the same as example 1.
Example 3
The method for modifying diatomaceous earth provided in the present application example is the same as example 1, except that the mass of sodium hydroxide in step S1 is 4% of the mass of calcined diatomaceous earth, the solid-to-liquid ratio in step S2 is 1:5, and the rest of the processes are the same as example 1.
Example 4
The method for modifying diatomite provided in the embodiment of the application is the same as the embodiment 1, except that the mass of the sodium hydroxide in the step S1 is 4% of the mass of the roasted diatomite, the solid-to-liquid ratio in the step S2 is 1:5, the hydrothermal reaction is carried out for 12h at 140 ℃ in the step S3, and the rest processes are the same as the embodiment 1.
Example 5
The method for modifying diatomite provided in the embodiment of the application is the same as the embodiment 1, except that the mass of the sodium hydroxide in the step S1 is 4% of the mass of the roasted diatomite, the solid-to-liquid ratio in the step S2 is 1:5, the hydrothermal reaction is carried out for 10h at 140 ℃ in the step S3, and the rest processes are the same as the embodiment 1.
Performance testing
The XRD pattern of the modified calcined diatomaceous earth of example 1 was measured, and the result is shown in fig. 1. The XRD pattern of the unmodified calcined diatomaceous earth (i.e., the original calcined diatomaceous earth) of example 1 is shown in FIG. 2.
As can be seen from fig. 1-2, the calcined diatomaceous earth modified with sodium hydroxide in example 1 has new absorption peaks at 2 θ of 12.50 °, 17.74 °, 28.12 °, and 33.46 °, and the diffraction peaks of the spectrum are sharp, indicating that the crystals are strong. Comparing it with standard card and searching, the material is NaP zeolite molecular sieve.
The surface morphology of the modified calcined diatomaceous earth in example 1 was tested, and the results are shown in fig. 3-4. FIGS. 3-4 show the surface topography of the calcined diatomaceous earth in various locations. The surface morphology of the calcined diatomaceous earth in example 1, which was not modified, is shown in FIGS. 5 to 6. FIGS. 5 to 6 show the surface topography of the calcined diatomaceous earth under different times.
As is clear from fig. 3 to 6, in the calcined diatomaceous earth modified with sodium hydroxide in example 1, coral-like crystals were grown on the surface of diatoms, and these crystals were in the form of a zeolite phase, resulting in an increase in the specific surface area.
The modified calcined diatomaceous earth and unmodified calcined diatomaceous earth (i.e., original calcined diatomaceous earth) in examples 1 to 5 were tested for the adsorption amount of methylene blue and the specific surface area thereof (the specific surface area was measured by the BET method), and the results are shown in table 1 below.
Specifically, methylene blue adsorption was tested as follows:
40mg of sample (i.e. the modified calcined diatomite or unmodified calcined diatomite) is respectively weighed and placed into a 100mL conical flask, 50mL of 10mg/L methylene blue solution is added, and the mixture is placed into a thermostatic water bath box at 25 ℃ and shaken for 25 min. The supernatant from the flask was centrifuged in a centrifuge and the absorbance of methylene blue was measured using a spectrophotometer. The methylene blue concentration and the absorbance have a good linear relation, the methylene blue concentration is calculated according to the absorbance, and the adsorption quantity can be obtained by substituting a fixed formula according to the concentration difference of the methylene blue before and after adsorption.
TABLE 1-adsorption amount of modified calcined diatomaceous earth in examples 1 to 5
Figure BDA0003469303770000071
As can be seen from Table 1, the calcined diatomaceous earth prepared by modification in examples 1 to 5 has a large specific surface area of 27.78m2(ii)/g, 44 times that of the original calcined diatomaceous earth; the adsorption effect on methylene blue is better and is 14.48 times of that of original baked diatomite. This shows that the specific surface area of the calcined diatomite can be effectively increased, the adsorption performance of the calcined diatomite can be improved, and the application range of the calcined diatomite can be expanded by adopting the modification method.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.

Claims (7)

1. A diatomite modification method is characterized by comprising the following steps:
mixing diatomite and sodium hydroxide to obtain a mixture;
adding water into the mixture, and stirring to obtain a mixture;
placing the mixture in an autoclave, and reacting at 120-180 ℃ for 6-18 h to obtain a reaction product;
and washing the reaction product to be neutral, and drying to finish the modification of the diatomite.
2. The method of modifying diatomaceous earth of claim 1, wherein the diatomaceous earth is calcined diatomaceous earth.
3. The method for modifying diatomaceous earth according to claim 1, wherein the sodium hydroxide is present in an amount of 1 to 10% by mass based on the total mass of diatomaceous earth.
4. The method for modifying diatomite as claimed in claim 1, wherein water is added to the mixture so that the solid-to-liquid ratio of the mixture is 1 (3-8).
5. The method for modifying diatomaceous earth according to claim 1, wherein the reaction product is washed to neutrality and dried to complete modification of diatomaceous earth, wherein the drying temperature is 80-120 ℃.
6. Diatomite modified by the modification method according to any one of claims 1 to 5.
7. Use of the diatomaceous earth of claim 6 as a filter aid, adsorbent, photocatalytic support.
CN202210038621.3A 2022-01-13 2022-01-13 Diatomite and modification method and application thereof Pending CN114367268A (en)

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CN109012575A (en) * 2018-08-30 2018-12-18 武汉理工大学 A method of improving roasting specific surface area of diatomite and adsorption capacity
CN111774045A (en) * 2020-06-03 2020-10-16 武汉理工大学 Regeneration method of diatomite adsorbent
RU2740995C1 (en) * 2020-05-22 2021-01-22 Федеральное государственное бюджетное образовательное учреждение высшего образования «Национальный исследовательский Мордовский государственный университет им. Н.П. Огарёва» Method of producing microsilica from natural diatomite by precipitation of nitric acid solution
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CN109012575A (en) * 2018-08-30 2018-12-18 武汉理工大学 A method of improving roasting specific surface area of diatomite and adsorption capacity
RU2740995C1 (en) * 2020-05-22 2021-01-22 Федеральное государственное бюджетное образовательное учреждение высшего образования «Национальный исследовательский Мордовский государственный университет им. Н.П. Огарёва» Method of producing microsilica from natural diatomite by precipitation of nitric acid solution
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