CN112742342A - Preparation method of magnetic diatom shell material and magnetic diatom shell material - Google Patents
Preparation method of magnetic diatom shell material and magnetic diatom shell material Download PDFInfo
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- CN112742342A CN112742342A CN202011473195.3A CN202011473195A CN112742342A CN 112742342 A CN112742342 A CN 112742342A CN 202011473195 A CN202011473195 A CN 202011473195A CN 112742342 A CN112742342 A CN 112742342A
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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
- B01J20/103—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate comprising silica
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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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28002—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 physical properties
- B01J20/28009—Magnetic properties
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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
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4812—Sorbents characterised by the starting material used for their preparation the starting material being of organic character
- B01J2220/4843—Algae, aquatic plants or sea vegetals, e.g. seeweeds, eelgrass
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Abstract
The invention provides a preparation method of a magnetic diatom shell material, which comprises the following steps: 1) washing diatom with water to remove water-soluble salts; 2) then carrying out acid washing to remove magnesium hydroxide; 3) then washing with an organic solvent to remove chlorophyll and lutein; 4) washing with water again to remove acid remained in the acid washing and organic solvent remained in the alcohol washing; 5) after drying, heat treatment is carried out, the heat treatment temperature is 300-800 ℃, and the heat treatment time is 0.5-2 h. The preparation method is simple, other materials do not need to be introduced, and the diatom serving as a preparation raw material is easy to obtain, so that the large-scale production is facilitated.
Description
Technical Field
The invention relates to the field of frustules, in particular to a preparation method of a magnetic frustule material and the magnetic frustule material.
Background
The diatom cell walls are covered with many regular mesh openings ranging from tens of nanometers to several micrometers in size for exchanging nutrients and gases. The residual crystal obtained by the diatom through a chemical roasting method is a diatom shell which is composed of silicon dioxide with extremely complex and precise structure, has good thermal stability and hydrothermal stability, high biocompatibility, low toxicity and the like, has wide application prospects in aspects of macromolecular catalysis, biological processes, selective adsorption, functional materials and the like, but is difficult to recycle.
The diatomite is a biochemical sedimentary rock formed by depositing diatoms for millions of years, and the composite material prepared by combining or loading diatomite micron-sized particles and a magnetic material is a diatomite-based magnetic composite material which has large specific surface area and good corrosion resistance, can directionally move under an applied electric field, is easy to separate, has photoelectricity and electromagnetism, and is often used as an adsorbent, a catalyst and a wave-absorbing base material to be widely applied to environmental, biological, photoelectric and catalytic engineering. The magnetic material can be conveniently separated from other materials or media by using an external magnetic field, so that the problems of recycling and recovering the frustules are solved. However, the magnetic nanoparticles have strong interactions, such as van der waals force and magnetic dipole interaction, which easily cause the agglomeration of the magnetic material during the loading process, thereby weakening the performance of the diatomite-based magnetic composite material. In addition, the diatomite-based magnetic composite material can be obtained by further processing the diatomite and the magnetic material, and the diatomite resource is limited and is difficult to form in a short time.
Disclosure of Invention
The embodiment of the invention aims to provide a preparation method of a magnetic diatom shell material, which is used for directly preparing the magnetic diatom shell material from diatom and is simple in preparation method.
The invention provides a preparation method of a magnetic diatom shell material, which comprises the following steps:
1) washing diatom with water to remove water-soluble salts;
2) then carrying out acid washing to remove magnesium hydroxide;
3) then washing with an organic solvent to remove chlorophyll and lutein;
4) washing with water again to remove acid remained in the acid washing and organic solvent remained in the alcohol washing;
5) after drying, heat treatment is carried out, the heat treatment temperature is 300-800 ℃, and the heat treatment time is 0.5-2 h.
Preferably, the above steps 1) -4) are repeated 2-5 times.
Preferably, the acid used for acid washing is selected from at least one of organic acid or inorganic acid.
Preferably, the organic acid is at least one selected from acetic acid, citric acid, tartaric acid, formic acid, lactic acid and gluconic acid, and the inorganic acid is at least one selected from nitric acid and hydrochloric acid.
Preferably, the acid used for the acid washing has a concentration of 0.5 to 2 mol/L.
Preferably, the organic solvent is selected from at least one of ethanol, acetone, and chloroform.
Preferably, the heat treatment temperature is 500-800 ℃, and the heat treatment time is 0.8-1.5 h.
Preferably, the heat treatment is performed in air, nitrogen, or a rare gas atmosphere.
In a second aspect, the invention provides a magnetic diatom shell material prepared by any of the above-described methods.
Preferably, the saturation magnetization of the magnetic diatom shell material is greater than or equal to 0.085 emu/g.
The preparation method of the magnetic diatom shell material provided by the invention comprises the steps of sequentially washing diatom with water, acid washing, washing with an organic solvent, removing residual acid and organic solvent by washing with water so as to remove impurities such as sodium chloride, magnesium hydroxide and chlorophyll coexisting with the diatom, drying and then carrying out heat treatment, thus obtaining the magnetic diatom shell material. The preparation method is simple, other materials do not need to be introduced, and the diatom serving as a preparation raw material is easy to obtain, so that the large-scale production is facilitated. In addition, the magnetic diatom shell material prepared by the preparation method disclosed by the invention has magnetism, other magnetic materials do not need to be introduced, the magnetic diatom shell material is used as an adsorbing material, and under the action of an external magnetic field, the rapid solid-liquid separation can be realized, so that the recovery rate of the magnetic diatom shell material is favorably improved.
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, and it is obvious that the drawings in the following description are only some embodiments of the present invention.
FIG. 1 is a graph showing the hysteresis curves of the diatom shell materials prepared in examples 1-6 and comparative example 1, and of the diatom feedstock and the diatom samples prepared in preparation examples 1-2;
FIG. 2 is an X-ray diffraction pattern of the diatom starting material, preparative examples 1 and 2.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail below with reference to the accompanying drawings and examples. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention.
The invention provides a preparation method of a magnetic diatom shell material, which comprises the following steps:
1) washing diatom with water to remove water-soluble salts;
2) then carrying out acid washing to remove magnesium hydroxide;
3) then washing with an organic solvent to remove chlorophyll and lutein;
4) washing with water again to remove acid remained in the acid washing and organic solvent remained in the alcohol washing;
5) after drying, heat treatment is carried out, the heat treatment temperature is 300-800 ℃, and the heat treatment time is 0.5-2 h.
The diatom mainly grows in rivers, lakes and other water areas, so that the diatom raw material contains inorganic salts, organic matters and other impurities, and the diatom needs to be pretreated to remove the substances when the magnetic diatom shell material is prepared. First, the diatoms are washed with water to remove water soluble salts, such as sodium chloride, from the diatoms. And secondly, removing magnesium hydroxide in the diatom by acid washing, removing organic matters such as chlorophyll and lutein in the diatom by using an organic solvent, and then washing by water to remove acid remained in the acid washing process and the organic solvent remained in the organic solvent washing process. And (3) drying the diatom after the pretreatment of the diatom is finished, and then carrying out heat treatment at the temperature of 300-800 ℃ for 0.5-2h to convert iron ions in the diatom into ferric oxide, thereby obtaining the magnetic diatom shell material. In addition, the preparation method provided by the application does not need to introduce other magnetic materials, and is simple in preparation steps and strong in controllability. Preferably, the heat treatment temperature is 500-.
Preferably, the acid wash is carried out with an acid concentration of 0.5 to 2mol/L, and controlling the acid concentration within the above range allows effective removal of magnesium hydroxide during the acid wash without removing iron-containing compounds from the diatoms.
Preferably, the steps 1) to 4) are repeated for 2 to 5 times, so that impurities such as sodium chloride, magnesium hydroxide, chlorophyll, lutein and the like in the diatom are removed more sufficiently, and the influence of the impurities on the magnetism of the prepared magnetic diatom shell material is weakened.
In the present invention, the acid used for the acid washing is at least one selected from organic acids and inorganic acids. The inorganic acid and the organic acid are not particularly limited as long as the organic acid or the magnesium salt formed by the reaction of the inorganic acid with magnesium hydroxide is a water-soluble magnesium salt. For example, the organic acid is at least one selected from acetic acid, citric acid, tartaric acid, formic acid, lactic acid and gluconic acid, and the inorganic acid is at least one selected from nitric acid and hydrochloric acid.
In the present invention, the organic solvent used when washing diatom algae with the above organic solvent is not particularly limited as long as it can dissolve chlorophyll and lutein. For example, the organic solvent is at least one selected from ethanol, acetone, and chloroform.
In the present invention, the diatom algae can be carried out in air, nitrogen or a rare gas atmosphere at the time of heat treatment. The rare gas may be at least one of helium, neon, argon, krypton, and xenon.
In the present invention, the heat treatment method is not particularly limited as long as the object of the present invention can be achieved. For example, the pretreated diatoms are heat treated in a tube furnace.
In a second aspect, the invention provides a magnetic diatom shell material prepared by any of the above-mentioned methods, wherein the magnetic diatom shell material has a saturation magnetization of 0.085emu/g or more. The magnetic diatom shell material has magnetism, other magnetic materials do not need to be introduced, the magnetic diatom shell material is used as an adsorbing material, and under the action of an external magnetic field, rapid solid-liquid separation can be realized, so that the recovery rate of the magnetic diatom shell material is improved. In addition, the magnetic diatom shell material provided by the invention can also be used for preparing catalytic materials.
The hysteresis curve test method comprises the following steps:
the method is characterized in that a comprehensive magnetic measurement system (MPMS) of the American Quantum Design company is adopted for measurement, a Brass (Brass) rod is selected in the test process, a sample is placed in a capsule and fixed in the Brass rod, a Vibration Sample Magnetometer (VSM) mode is selected for measurement in the test process, and the specific parameters are set as follows: the Peak Amplitude (Peak Amplitude) is 5mm, the average Time is (Averaging Time)2s, Data Acquisition Continuous measurement (Sweep Continuous measurement) is adopted, and a Continuous scanning (Sweep Continuous) mode is selected to take points in the test process. The magnetic field applying sequence selected for each sample is 0-4000-0-4000 Oe, and the hysteresis loop of the brass rod without the sample is used as the background to be deducted to obtain the hysteresis loop of the sample, and the saturation magnetization can be directly measured.
Preparation example 1
1) Weighing 20g of diatom, putting the diatom into a beaker, adding 100mL of water, stirring for 20min, and filtering out the diatom;
2) then placing the diatom into a beaker, adding 100mL of nitric acid with the concentration of 1mol/L, stirring for 20min, and filtering out the diatom;
3) then placing the diatom into a beaker, adding 100mL of absolute ethyl alcohol, stirring for 20min, and filtering out the diatom;
4) the diatoms are then placed in a beaker, 100mL of water is added and stirred for 20min, and the diatoms are filtered out.
Preparation example 2
Steps 1) to 4) in preparation example 1 were repeated 2 times.
Example 1
The diatom in preparation example 2 is dried at 60 ℃ for 18h and put into a tube furnace to be thermally treated at 300 ℃ for 1h to obtain the magnetic diatom shell material, wherein the atmosphere of the thermally treated gas is air.
Examples 2 to 6
The same procedure as in example 1 was repeated, except that the heat treatment temperature in step 5) was changed to 400 ℃, 500 ℃, 600 ℃, 700 ℃ and 800 ℃.
Example 7
The same as example 1 except that nitric acid in step 2) was replaced with acetic acid.
Example 8
The same procedure as in example 1 was repeated, except that the nitric acid concentration in step 2) was changed to 0.8 mol/L.
Example 9
The same procedure as in example 1 was repeated, except that the nitric acid concentration in step 2) was changed to 1.5 mol/L.
Example 10
The same procedure as in example 1 was repeated, except that the diatom in preparation example 2 was replaced with the diatom in preparation example 1.
Example 11
The same as example 1 except that the heat treatment temperature in step 5) was 650 ℃ and the heat treatment gas atmosphere was nitrogen.
Comparative example 1
The same as example 1 except that the heat treatment temperatures in step 5) were 900 ℃ respectively.
TABLE 1 saturated magnetization of the frustules materials obtained in examples 1-11 and comparative example 1
As shown in table 1 and fig. 1, the saturation magnetization of the frustules prepared by the preparation method provided by the present invention is greater than that of the diatom raw material, especially the magnetic frustules of example 5, which have a saturation magnetization much greater than that of the diatom raw material. The diatom starting material itself is non-magnetic, and the diatom samples obtained in preparative examples 1 and 2 were also substantially non-magnetic by subjecting the diatom starting material to water washing, acid washing, organic solvent washing and water washing in this order. By adopting the preparation method of the invention, the diatom shell materials obtained by respectively carrying out heat treatment on the diatom obtained in the preparation example 2 at different temperatures (examples 1-6) have magnetism. And when the heat treatment temperature is 700 ℃ (example 5), the magnetism of the material is strongest, but when the heat treatment temperature is increased to 900 ℃, the obtained diatom shell material is basically nonmagnetic, so that the magnetic diatom shell material can be obtained within the temperature range of the preparation method provided by the invention, and the influence of the heat treatment temperature on the magnetism of the diatom shell material is the largest.
Further, as shown in fig. 2, the diatom raw material contains impurities such as magnesium hydroxide and sodium chloride, and when the diatom is washed with water, acid, organic solvent and water in preparation example 1, the peaks corresponding to magnesium hydroxide and sodium chloride become small, indicating that magnesium hydroxide and sodium chloride are partially washed away but remain partially. The diatom algae of preparation 2 was obtained by repeating all the steps of preparation 1 twice, wherein peaks corresponding to magnesium hydroxide and sodium chloride were substantially disappeared, indicating that magnesium hydroxide and sodium chloride were substantially removed. Therefore, the diatom shell material obtained by carrying out heat treatment on the diatom obtained in preparation example 2 is beneficial to reducing the influence of impurities in the diatom raw material on the magnetism of the diatom shell material.
The above description is only for the preferred embodiment of the present invention, and is not intended to limit the scope of the present invention. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention shall fall within the protection scope of the present invention.
Claims (10)
1. A preparation method of a magnetic diatom shell material comprises the following steps:
1) washing diatom with water to remove water-soluble salts;
2) then carrying out acid washing to remove magnesium hydroxide;
3) then washing with an organic solvent to remove chlorophyll and lutein;
4) washing with water again to remove acid remained in the acid washing and organic solvent remained in the alcohol washing;
5) after drying, heat treatment is carried out, the heat treatment temperature is 300-800 ℃, and the heat treatment time is 0.5-2 h.
2. The method of claim 1, wherein the above steps 1) -4) are repeated 2-5 times.
3. The production method according to claim 1, wherein the acid used for the acid washing is at least one selected from an organic acid and an inorganic acid.
4. The production method according to claim 3, wherein the organic acid is at least one selected from the group consisting of acetic acid, citric acid, tartaric acid, formic acid, lactic acid, and gluconic acid, and the inorganic acid is at least one selected from the group consisting of nitric acid and hydrochloric acid.
5. The production method according to claim 1, wherein the acid is used in an acid washing concentration of 0.5 to 2 mol/L.
6. The production method according to claim 1, wherein the organic solvent is at least one selected from ethanol, acetone, and chloroform.
7. The method as claimed in claim 1, wherein the heat treatment temperature is 500-800 ℃ and the heat treatment time is 0.8-1.5 h.
8. The production method according to claim 1, wherein the heat treatment is performed in air, nitrogen, or a rare gas atmosphere.
9. A magnetic diatom shell material prepared by the method of any one of claims 1-8.
10. The magnetic frustule material of claim 9, having a saturation magnetization of greater than or equal to 0.085 emu/g.
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106955716A (en) * | 2017-03-29 | 2017-07-18 | 重庆大学 | A kind of magnetic coupling diatomite material and preparation method thereof |
| US20170274348A1 (en) * | 2014-08-29 | 2017-09-28 | Imerys Filtration Minerals, Inc. | Methods of making highly purified diatomaceous earth with wide range of filtration rates |
| CN109075325A (en) * | 2015-12-18 | 2018-12-21 | 挪威科技大学 | Anode containing frustule |
| CN109200991A (en) * | 2018-09-14 | 2019-01-15 | 太原理工大学 | A kind of preparation method and applications of red mud one-step synthesis magnetic adsorbent |
| US20190351355A1 (en) * | 2017-01-06 | 2019-11-21 | Ep Minerals, Llc | Ultra-high purity, ultra-high performance diatomite filtration media |
| CN110518197A (en) * | 2019-07-12 | 2019-11-29 | 北京师范大学 | A kind of diatom complex material and preparation method thereof and the application in lithium ion battery |
| US20200001267A1 (en) * | 2017-01-06 | 2020-01-02 | Ep Minerals, Llc | Ultra-high performance and high purity biogenic silica filtration media |
-
2020
- 2020-12-15 CN CN202011473195.3A patent/CN112742342A/en not_active Withdrawn
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20170274348A1 (en) * | 2014-08-29 | 2017-09-28 | Imerys Filtration Minerals, Inc. | Methods of making highly purified diatomaceous earth with wide range of filtration rates |
| CN109075325A (en) * | 2015-12-18 | 2018-12-21 | 挪威科技大学 | Anode containing frustule |
| US20190351355A1 (en) * | 2017-01-06 | 2019-11-21 | Ep Minerals, Llc | Ultra-high purity, ultra-high performance diatomite filtration media |
| US20200001267A1 (en) * | 2017-01-06 | 2020-01-02 | Ep Minerals, Llc | Ultra-high performance and high purity biogenic silica filtration media |
| CN106955716A (en) * | 2017-03-29 | 2017-07-18 | 重庆大学 | A kind of magnetic coupling diatomite material and preparation method thereof |
| CN109200991A (en) * | 2018-09-14 | 2019-01-15 | 太原理工大学 | A kind of preparation method and applications of red mud one-step synthesis magnetic adsorbent |
| CN110518197A (en) * | 2019-07-12 | 2019-11-29 | 北京师范大学 | A kind of diatom complex material and preparation method thereof and the application in lithium ion battery |
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