CN116059970A - Heavy metal ion adsorption material and preparation method thereof - Google Patents
Heavy metal ion adsorption material and preparation method thereof Download PDFInfo
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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- 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
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0211—Compounds of Ti, Zr, Hf
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- B01J20/0274—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04 characterised by the type of anion
- B01J20/0292—Phosphates of compounds other than those provided for in B01J20/048
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
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- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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Abstract
The invention relates to a heavy metal ion adsorption material and a preparation method thereof. The heavy metal ion adsorption material comprises: a porous organic composite matrix, and an amorphous TiPO adsorbent distributed in the pore size of the porous organic composite matrix; the porous organic composite matrix is obtained by solidifying medical waste slag and inorganic cementing materials, wherein the medical waste slag is metal oxide or/and carbonate; preferably, the content of the amorphous TiPO adsorbent accounts for 0.5-3 wt% of the total mass of the heavy metal ion adsorption material.
Description
Technical Field
The invention relates to a heavy metal ion adsorption material and a preparation method thereof, in particular to a method for preparing a heavy metal ion adsorption material by taking medical waste slag as a main material, and belongs to the technical field of solid waste resource utilization.
Background
Along with the improvement of the technological level, the industry in China is rapidly developed, so that the living standard of people is continuously improved, but the development of the industry also causes pressure on the ecological environment in China: the amount of industrial wastewater directly discharged into natural environment is increased, the self-cleaning capability of the water body is destroyed, the heavy metal pollutant content of the water body is seriously out of standard, and the damage is caused to the life of aquatic organisms and agricultural production. Therefore, the problem of heavy metal pollution of the water body cannot be ignored.
The yellow rich subject group of Shanghai silicate institute has invented a high-efficiency heavy metal ion adsorption material through many years of technical attack: amorphous Phosphorylated Titanium Oxide (FAPTO) (application number: 201710452750.6), the material has high adsorption efficiency to heavy metal ions in water up to 99%, but is a porous material with extremely low apparent density, and can be used alone in natural water to easily float and influence the collection of heavy metal ions.
Disclosure of Invention
In order to enable FAPTO to effectively adsorb and collect heavy metal ions in water, the invention embeds and fixes amorphous phosphorylated titanium oxide in gaps of a permeable porous material with certain strength, and provides a heavy metal ion adsorption material and a preparation method thereof.
In one aspect, the present invention provides a heavy metal ion adsorption material comprising: a porous organic composite matrix, and an amorphous TiPO adsorbent distributed in the pore size of the porous organic composite matrix; the porous organic composite matrix is obtained by solidifying medical waste slag and inorganic cementing materials, wherein the medical waste slag is metal oxide or/and carbonate; preferably, the content of the amorphous TiPO adsorbent accounts for 0.5-3 wt% of the total mass of the heavy metal ion adsorption material.
In the invention, the main component of the medical waste slag is inorganic nonmetallic materials (metal oxides or/and carbonates, such as aluminum oxide, ferric oxide, silicon oxide, magnesium oxide, calcium carbonate and the like), and the slag does not belong to dangerous wastes, and has great potential for recycling. The slag is treated at high temperature, has stable chemical property and is insoluble in water, and is a good raw material for preparing porous materials. The high-strength water-permeable porous material is prepared by taking the slag as a main raw material, so that the FAPTO can effectively play a role in adsorbing and collecting heavy metal ions, and the medical waste slag can be effectively utilized, thereby achieving the aim of changing waste into valuables.
Preferably, the inorganic cementing material is cement; the mass ratio of the inorganic cementing material to the medical waste slag is (1-5): 1.
preferably, the porosity of the heavy metal ion adsorption material is 30% -50%, preferably 40%.
Preferably, the pore size is 500 μm to 3mm, preferably 1mm to 3mm.
Preferably, the amorphous TiPO adsorbent consists of amorphous TiPO particles; the grain diameter of the amorphous TiPO particles is 100 nm-5 mu m.
Preferably, the strength of the heavy metal ion adsorption material is 10-35 MPa.
In another aspect, the present invention provides a method for preparing a heavy metal ion adsorption material, comprising:
(1) Adding water into the medical waste slag and the inorganic cementing material to mix, and preparing a pasty raw material;
(2) Mixing the amorphous TiPO adsorbent with the pasty raw material, and then placing the mixture in air to harden for 14-28 days to obtain the heavy metal ion adsorption material.
Preferably, the mass of the amorphous TiPO adsorbent is 5-20wt% of the pasty raw material.
Preferably, the mass of the water is 10-30 wt% of the total mass of the medical waste slag and the inorganic cementing material.
In still another aspect, the present invention provides a method for preparing a heavy metal ion adsorption material, comprising:
(1) Adding water into the medical waste slag and the inorganic cementing material to mix, and preparing a pasty raw material;
(2) Mixing an amorphous TiPO adsorbent and an organic coating material, melting and stirring for 20-60 minutes at 80-100 ℃, and crushing and screening after cooling to obtain 40-80 meshes of organic powder;
(3) Mixing the organic powder and the obtained pasty raw material, placing the mixture in air for hardening for 14-28 days, immersing the mixture in an organic solution to remove the organic coating material, and washing and drying the mixture to obtain the heavy metal ion adsorption material. The organic coating material is added, so that the functional group of the FAPTO can be protected, the FAPTO is not changed or damaged in the hardening process of the inorganic cementing material, and in addition, the organic coating material is also an effective pore-forming material, holes can be formed after the organic coating material is dissolved by an organic solvent, and the structure can increase the adsorption efficiency of the FAPTO on heavy metal ions.
Preferably, the mass of the water is 10-30 wt% of the total mass of the medical waste slag and the inorganic cementing material.
Preferably, in the step (2), the organic coating material is at least one selected from paraffin wax, microcrystalline paraffin wax and beeswax; preferably, the mass of the organic coating material is 10-20 times of that of the amorphous TiPO adsorbent.
Preferably, the mass of the organic powder is 5-20wt% of the pasty raw material.
Preferably, in the step (3), the organic solvent is at least one of diethyl ether, aviation kerosene, n-hexane, n-heptane and tribromopropane; the mass of the organic solvent is 1-10 times of that of the hardened composite material, and the soaking time is 4-12 hours.
The beneficial effects are that:
the invention relates to a preparation method for preparing a heavy metal ion adsorption material by taking medical waste slag as a main raw material, which comprises the following steps: organic coating is carried out on FAPTO with high-efficiency heavy metal ion adsorption performance, then coated organic particles and treated medical waste slag powder are compounded in a porous inorganic cementing material, after molding, the porous inorganic cementing material is soaked in an organic solvent, an organic wax film on the surface of the FAPTO is dissolved, and then the organic solvent is dried in an oven, so that the material with heavy metal ion adsorption performance can be prepared.
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Detailed Description
The invention is further illustrated by the following embodiments, which are to be understood as merely illustrative of the invention and not limiting thereof.
In the present disclosure, a method for preparing a heavy metal ion adsorption material by using medical waste slag as a main raw material is selected.
The following exemplifies a method for preparing the heavy metal ion adsorption material.
The preparation of amorphous TiPO adsorbent (FAPTO) is described in the prior patent (application No. 201710452750.6).
And (3) organically coating the surface of the FAPTO with the high-efficiency heavy metal ion adsorption performance, and then crushing the FAPTO into organic particles. The main organic matters (organic coating materials) used for coating are one or more of paraffin, microcrystalline paraffin and beeswax. The mass of the coated organic matter is 10-20 times of the mass of the adsorbent. Wherein, the organic matter coating material is less, the coating effect is poor, and too much FAPTO in the composite material is too little, thereby affecting the adsorption efficiency of the sample.
The organic coating material is melted at 80-100 ℃ and then the amorphous TiPO adsorbent is added into the melted organic matter, stirred for 20-60 min, and the mixture is crushed after cooling and is sieved to obtain 40-80 mesh organic powder.
Mixing the medical waste slag and the inorganic cementing material in a certain proportion with water to prepare the pasty raw material. The inorganic cementing material used is cement. The slag is powder which is crushed and sieved by a 60-mesh screen. The mass of the cement can be 1 to 5 times of that of the medical waste slag. The mass of the water is 10-30wt% of the total mass of the medical waste slag and the inorganic cementing material. Mixing the water, the medical waste slag and the inorganic cementing material, and then continuously stirring in a stirrer for 5-20 min.
Mixing the organic powder and the pasty raw material to obtain the slurry. The mass of the organic particles is 5-20% of the mass of the paste raw material, and the paste raw material and the organic particles are stirred in a stirrer for 10-30 min. Or directly mixing the amorphous TiPO adsorbent and the pasty raw material to obtain the slurry. The mass of the amorphous TiPO adsorbent is 5-20% of the mass of the pasty raw material, and the amorphous TiPO adsorbent and the pasty raw material are stirred in a stirrer for 10-30min
The mixed slurry is put in air to harden for 14-28 days.
And soaking and washing the hardened material in an organic solvent. And then placing the washed material in an oven for drying treatment to obtain the material with heavy metal ion adsorption performance. The organic solvent is one or more of diethyl ether, aviation kerosene, n-hexane, n-heptane or tribromopropane, the mass of the organic solvent is 1-10 times of that of the composite material, and the soaking time is 4-12 hours. The number of times of washing may be 3 to 5. The drying temperature can be 80-100 ℃, and the drying time can be 2-10 h.
The present invention will be further illustrated by the following examples. It is also to be understood that the following examples are given solely for the purpose of illustration and are not to be construed as limitations upon the scope of the invention, since numerous insubstantial modifications and variations will now occur to those skilled in the art in light of the foregoing disclosure. The specific process parameters and the like described below are also merely examples of suitable ranges, i.e., one skilled in the art can make a suitable selection from the description herein and are not intended to be limited to the specific values described below.
Example 1
1) Weighing 50 g of No. 58 semi-refined paraffin, placing in a heated beaker, melting at 100 ℃, then adding 3.0 g of FAPTO, and stirring for 30min;
2) Cooling the mixture, crushing the mixture by using a dispersing disc, sieving the crushed powder with a 40-80 mesh sieve, and taking a part with the particle size range of 40-80 meshes;
3) Ball milling and crushing medical waste slag, sieving with a 60-mesh sieve, weighing 30 g of sieved slag, weighing 30 g of cement, mixing the slag and the cement, and adding 10 g of water to stir uniformly;
4) Taking 5 g of the organic particles prepared in the step 2), and stirring the organic particles and the pasty inorganic mixture obtained in the step 3 in a stirrer for 10-30min;
5) Placing the mixture prepared in the step 4) in a plastic mould, and sealing and placing for 14 days after jolt ramming;
6) Soaking the block material with higher strength prepared in the step 5) in n-heptane for 4 hours, wherein the mass of the n-heptane is 100 g;
7) Taking out the material etched by the n-heptane in the step 6), and washing 3 times by using a pure n-heptane solvent;
8) And (3) drying the washed material in the step (7) at 80 ℃ for 4 hours to obtain the material capable of adsorbing heavy metal ions in water. The content of the amorphous TiPO adsorbent in the obtained heavy metal ion adsorption material accounts for 0.5 percent of the total mass of the heavy metal ion adsorption material, the porosity is 35 percent, and the pore size distribution is 1 mm-3 mm.
9) The compressive strength of the material prepared in this example was 17MPa. Samples prepared in this batch, in 3L Pb 2+ The solution with the concentration of 54mg/L is placed for 12 hours, and the concentration of heavy metal ions in the solution can be reduced to 0.1mg/L.
Example 2
1) Weighing 50 g of No. 58 semi-refined paraffin, placing in a heated beaker, melting at 100 ℃, then adding 3.0 g of FAPTO, and stirring for 30min;
2) Cooling the mixture, crushing the mixture by using a dispersing disc, sieving the crushed powder with a 40-80 mesh sieve, and taking a part with the particle size range of 40-80 meshes;
3) Ball milling and crushing medical waste slag, sieving with a 60-mesh sieve, weighing 20 g of sieved slag, weighing 40 g of cement, mixing the slag and the cement, and adding 10 g of water to stir uniformly;
4) Taking 10 g of the organic particles prepared in the step 2), and stirring the organic particles and the pasty inorganic mixture obtained in the step 3 in a stirrer for 10-30min;
5) Placing the mixture prepared in the step 4) in a plastic mould, and sealing and placing for 14 days after jolt ramming;
6) Soaking the block material with higher strength prepared in the step 5) in n-heptane for 4 hours, wherein the mass of the n-heptane is 100 g;
7) Taking out the material etched by the n-heptane in the step 6), and washing 3 times by using a pure n-heptane solvent;
8) And (3) drying the washed material in the step (7) at 80 ℃ for 4 hours to obtain the material capable of adsorbing heavy metal ions in water. The content of the amorphous TiPO adsorbent in the obtained heavy metal ion adsorption material accounts for 1% of the total mass of the heavy metal ion adsorption material, the porosity is 45%, and the pore size distribution is 1-5 mm;
9) The compressive strength of the material prepared in this example was 18MPa.
Example 3
1) Weighing 50 g of microcrystalline paraffin, placing in a heated beaker to be melted at 100 ℃, then adding 3.0 g of FAPTO, and stirring for 30min;
2) Cooling the mixture, crushing the mixture by using a dispersing disc, sieving the crushed powder with a 60-80 mesh sieve, and taking a part with the particle size range of 60-80 meshes;
3) Ball milling and crushing medical waste slag, sieving with a 60-mesh sieve, weighing 40 g of sieved slag, weighing 20 g of cement, mixing the slag and the cement, and adding 10 g of water to stir uniformly;
4) Taking 5 g of the organic particles prepared in the step 2), and stirring the organic particles and the pasty inorganic mixture obtained in the step 3 in a stirrer for 10-30min;
5) Placing the mixture prepared in the step 4) in a plastic mould, and sealing and placing for 28 days after jolt ramming;
6) Soaking the block material with higher strength prepared in the step 5) in n-heptane for 8 hours, wherein the mass of the n-heptane is 100 g;
7) Taking out the material etched by the n-heptane in the step 6), and washing 3 times by using a pure n-heptane solvent;
8) And (3) drying the washed material in the step (7) at 80 ℃ for 4 hours to obtain the material capable of adsorbing heavy metal ions in water. The content of the amorphous TiPO adsorbent in the obtained heavy metal ion adsorption material accounts for 0.5 percent of the total mass of the heavy metal ion adsorption material, the porosity is 40 percent, and the pore size distribution is 0.5 mm-3 mm;
9) The compressive strength of the material prepared in this example was 16MPa.
Example 4
1) Ball milling and crushing medical waste slag, sieving with a 60-mesh sieve, weighing 40 g of sieved slag, weighing 20 g of cement, mixing the slag and the cement, and adding 10 g of water to stir uniformly;
2) Taking 0.6 g of FAPTO, and stirring the FAPTO and the pasty inorganic mixture obtained in the step 3 in a stirrer for 10-30min;
3) Placing the mixture prepared in the step 4) in a plastic mould, sealing and placing for 28 days after jolt ramming, wherein the content of the amorphous TiPO adsorbent in the obtained heavy metal ion adsorption material accounts for 1% of the total mass of the heavy metal ion adsorption material, the porosity is 15%, and the pore size distribution is 0.5-1 mm;
4) Samples prepared in this batch, in 3L Pb 2+ Placing in 54mg/L solutionAfter 12h, the concentration of heavy metal ions in the solution can be reduced to 0.9mg/L.
Example 5
1) Weighing 60 g of 58# semi-refined paraffin, placing in a heated beaker, melting at 90 ℃, then adding 3.0 g of FAPTO, and stirring for 30min;
2) Cooling the mixture, crushing the mixture by using a dispersing disc, sieving the crushed powder with a 60-80 mesh sieve, and taking a part with the particle size range of 60-80 meshes;
3) Ball milling and crushing medical waste slag, sieving with a 60-mesh sieve, weighing 30 g of sieved slag, weighing 30 g of cement, mixing the slag and the cement, and adding 10 g of water to stir uniformly;
4) Taking 6 g of the organic particles prepared in the step 2), and stirring the organic particles and the pasty inorganic mixture obtained in the step 3 in a stirrer for 10-30min;
5) Placing the mixture prepared in the step 4) in a plastic mould, and sealing and placing for 28 days after jolt ramming;
6) Soaking the block material with higher strength prepared in the step 5) in aviation kerosene, wherein the mass of the aviation kerosene is 150 g, and the soaking time is 8h;
7) Taking out the material etched by the n-heptane in the step 6), and washing 3 times by using aviation kerosene;
8) And (3) drying the washed material in the step (7) at 80 ℃ for 4 hours to obtain the material capable of adsorbing heavy metal ions in water. The content of the amorphous TiPO adsorbent in the obtained heavy metal ion adsorption material accounts for 0.5 percent of the total mass of the heavy metal ion adsorption material, the porosity is 48 percent, and the pore size distribution is 0.5 mm-5 mm;
9) Samples prepared in this batch, in 3L Pb 2+ The solution with the concentration of 54mg/L is placed for 12 hours, and the concentration of heavy metal ions in the solution can be reduced to 0.1mg/L.
Example 6
1) 40 g of 58# semi-refined paraffin was weighed, placed in a heated beaker and melted at 90 ℃, then 3.0 g of FAPTO was added and stirred for 30min;
2) Cooling the mixture, crushing the mixture by using a dispersing disc, sieving the crushed powder with a 60-80 mesh sieve, and taking a part with the particle size range of 60-80 meshes;
3) Ball milling and crushing medical waste slag, sieving with a 60-mesh sieve, weighing 30 g of sieved slag, weighing 30 g of cement, mixing the slag and the cement, and adding 10 g of water to stir uniformly;
4) Taking 5 g of the organic particles prepared in the step 2), and stirring the organic particles and the pasty inorganic mixture obtained in the step 3 in a stirrer for 10-30min;
5) Placing the mixture prepared in the step 4) in a plastic mould, and sealing and placing for 28 days after jolt ramming;
6) Soaking the block material with higher strength prepared in the step 5) in aviation kerosene, wherein the mass of the aviation kerosene is 150 g, and the soaking time is 8h;
7) Taking out the material etched by the n-heptane in the step 6), and washing 3 times by using aviation kerosene;
8) And (3) drying the washed material in the step (7) at 80 ℃ for 4 hours to obtain the material capable of adsorbing heavy metal ions in water. The content of the amorphous TiPO adsorbent in the obtained heavy metal ion adsorption material accounts for 0.6 percent of the total mass of the heavy metal ion adsorption material, the porosity is 40 percent, and the pore size distribution is 0.5 mm-5 mm;
9) Samples prepared in this batch, in 3L Pb 2+ The solution with the concentration of 54mg/L is placed for 12 hours, and the concentration of heavy metal ions in the solution can be reduced to 0.15mg/L.
Example 7
1) 30 g of 58# semi-refined paraffin was weighed, placed in a heated beaker and melted at 90 ℃, then 3.0 g of FAPTO was added and stirred for 30min;
2) Cooling the mixture, crushing the mixture by using a dispersing disc, sieving the crushed powder with a 60-80 mesh sieve, and taking a part with the particle size range of 60-80 meshes;
3) Ball milling and crushing medical waste slag, sieving with a 60-mesh sieve, weighing 30 g of sieved slag, weighing 30 g of cement, mixing the slag and the cement, and adding 10 g of water to stir uniformly;
4) Taking 6 g of the organic particles prepared in the step 2), and stirring the organic particles and the pasty inorganic mixture obtained in the step 3 in a stirrer for 10-30min;
5) Placing the mixture prepared in the step 4) in a plastic mould, and sealing and placing for 28 days after jolt ramming;
6) Soaking the block material with higher strength prepared in the step 5) in aviation kerosene, wherein the mass of the aviation kerosene is 150 g, and the soaking time is 8h;
7) Taking out the material etched by the n-heptane in the step 6), and washing 3 times by using aviation kerosene;
8) And (3) drying the washed material in the step (7) at 80 ℃ for 4 hours to obtain the material capable of adsorbing heavy metal ions in water. The content of the amorphous TiPO adsorbent in the obtained heavy metal ion adsorption material accounts for 1 percent of the total mass of the heavy metal ion adsorption material, the porosity is 30 percent, and the pore size distribution is 0.5 mm-3 mm;
9) Samples prepared in this batch, in 3L Pb 2+ The solution with the concentration of 54mg/L is placed for 12 hours, and the concentration of heavy metal ions in the solution can be reduced to 0.1mg/L.
Claims (10)
1. A heavy metal ion adsorbing material, characterized by comprising: a porous organic composite matrix, and an amorphous TiPO adsorbent distributed in the pore size of the porous organic composite matrix; the porous organic composite matrix is obtained by solidifying medical waste slag and inorganic cementing materials, wherein the medical waste slag is metal oxide or/and carbonate; preferably, the content of the amorphous TiPO adsorbent accounts for 0.5-3 wt% of the total mass of the heavy metal ion adsorption material.
2. The heavy metal ion adsorbing material according to claim 1, wherein the inorganic gel material is cement; the mass ratio of the inorganic cementing material to the medical waste slag is (1-5): 1.
3. the heavy metal ion adsorption material according to claim 1, wherein the porosity of the heavy metal ion adsorption material is 30% -50%, preferably 40%; the pore size is 500 μm to 3mm, preferably 1mm to 3mm.
4. The heavy metal ion adsorption material of claim 1, wherein the amorphous TiPO adsorbent is composed of amorphous TiPO particles; the grain diameter of the amorphous TiPO particles is 0.1-5 mu m.
5. The heavy metal ion adsorption material according to any one of claims 1 to 4, wherein the compressive strength of the heavy metal ion adsorption material is 10 to 35MPa.
6. A method for producing the heavy metal ion adsorption material according to any one of claims 1 to 5, comprising:
(1) Adding water into the medical waste slag and the inorganic cementing material to mix, and preparing a pasty raw material;
(2) Mixing the amorphous TiPO adsorbent with the pasty raw material, and then placing the mixture in air to harden for 14-28 days to obtain the heavy metal ion adsorption material;
preferably, the mass of the amorphous TiPO adsorbent is 5-20wt% of the pasty raw material.
7. A method for producing the heavy metal ion adsorption material according to any one of claims 1 to 5, comprising:
(1) Adding water into the medical waste slag and the inorganic cementing material to mix, and preparing a pasty raw material;
(2) Mixing an amorphous TiPO adsorbent and an organic coating material, melting and stirring for 20-60 minutes at 80-100 ℃, and crushing and screening after cooling to obtain 40-80 meshes of organic powder;
(3) Mixing the organic powder and the obtained pasty raw material, placing the mixture in air to harden for 14-28 days, immersing the mixture in an organic solution to remove the organic coating material, and washing and drying the mixture to obtain the heavy metal ion adsorption material;
preferably, the mass of the organic powder is 5-20wt% of the paste raw material.
8. The method according to claim 6 or 7, wherein in the step (1), the mass of the water is 10 to 30wt% of the total mass of the medical waste slag and the inorganic binder.
9. The method according to claim 7, wherein in the step (2), the organic coating material is at least one selected from paraffin wax, microcrystalline paraffin wax and beeswax; preferably, the mass of the organic coating material is 10-20 times of that of the amorphous TiPO adsorbent.
10. The method according to claim 7, wherein in the step (3), the organic solvent is at least one of diethyl ether, aviation kerosene, n-hexane, n-heptane and tribromopropane; the mass of the organic solvent is 1-10 times of that of the hardened composite material, and the soaking time is 4-12 hours.
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