CN112892479B - Preparation method of high-adsorptivity biochar - Google Patents
Preparation method of high-adsorptivity biochar Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 claims abstract description 49
- 239000002243 precursor Substances 0.000 claims abstract description 36
- 238000000034 method Methods 0.000 claims abstract description 35
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 23
- 238000001035 drying Methods 0.000 claims abstract description 17
- 238000002791 soaking Methods 0.000 claims abstract description 16
- 238000010438 heat treatment Methods 0.000 claims abstract description 15
- 239000003292 glue Substances 0.000 claims abstract description 11
- 230000005855 radiation Effects 0.000 claims abstract description 11
- 238000007598 dipping method Methods 0.000 claims abstract description 5
- 239000007789 gas Substances 0.000 claims description 42
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 18
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 10
- 239000001301 oxygen Substances 0.000 claims description 10
- 229910052760 oxygen Inorganic materials 0.000 claims description 10
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical compound [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 claims description 9
- 239000001569 carbon dioxide Substances 0.000 claims description 9
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 9
- 229910002091 carbon monoxide Inorganic materials 0.000 claims description 9
- 239000010902 straw Substances 0.000 claims description 8
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 7
- 239000012535 impurity Substances 0.000 claims description 7
- 229910052757 nitrogen Inorganic materials 0.000 claims description 7
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 7
- 238000003756 stirring Methods 0.000 claims description 7
- 238000002679 ablation Methods 0.000 claims description 5
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 4
- 239000004917 carbon fiber Substances 0.000 claims description 4
- 239000006087 Silane Coupling Agent Substances 0.000 claims description 3
- 239000002585 base Substances 0.000 claims description 3
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 3
- 239000002253 acid Substances 0.000 claims description 2
- 239000003513 alkali Substances 0.000 claims description 2
- 239000003822 epoxy resin Substances 0.000 claims description 2
- 229920000647 polyepoxide Polymers 0.000 claims description 2
- 239000002023 wood Substances 0.000 claims description 2
- 235000013399 edible fruits Nutrition 0.000 claims 1
- 238000001179 sorption measurement Methods 0.000 abstract description 27
- 239000002245 particle Substances 0.000 abstract description 8
- 239000000203 mixture Substances 0.000 description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 11
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 10
- 230000000052 comparative effect Effects 0.000 description 10
- 229910017604 nitric acid Inorganic materials 0.000 description 10
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 description 10
- 238000005406 washing Methods 0.000 description 10
- 239000010410 layer Substances 0.000 description 9
- 239000000463 material Substances 0.000 description 9
- 239000011148 porous material Substances 0.000 description 9
- 238000002955 isolation Methods 0.000 description 6
- 239000000243 solution Substances 0.000 description 6
- 230000008595 infiltration Effects 0.000 description 5
- 238000001764 infiltration Methods 0.000 description 5
- 239000011259 mixed solution Substances 0.000 description 5
- 235000019353 potassium silicate Nutrition 0.000 description 5
- 239000004317 sodium nitrate Substances 0.000 description 5
- 235000010344 sodium nitrate Nutrition 0.000 description 5
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 241000209140 Triticum Species 0.000 description 4
- 235000021307 Triticum Nutrition 0.000 description 4
- 239000012790 adhesive layer Substances 0.000 description 4
- 239000003610 charcoal Substances 0.000 description 3
- 238000010835 comparative analysis Methods 0.000 description 3
- 238000003795 desorption Methods 0.000 description 3
- 239000002912 waste gas Substances 0.000 description 3
- 239000002351 wastewater Substances 0.000 description 3
- 239000002028 Biomass Substances 0.000 description 2
- 239000003463 adsorbent Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000002485 combustion reaction Methods 0.000 description 2
- 238000005520 cutting process Methods 0.000 description 2
- 230000002349 favourable effect Effects 0.000 description 2
- 239000002737 fuel gas Substances 0.000 description 2
- 125000000524 functional group Chemical group 0.000 description 2
- 238000005470 impregnation Methods 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- YCOZIPAWZNQLMR-UHFFFAOYSA-N pentadecane Chemical compound CCCCCCCCCCCCCCC YCOZIPAWZNQLMR-UHFFFAOYSA-N 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 239000002356 single layer Substances 0.000 description 2
- 238000005303 weighing Methods 0.000 description 2
- 206010021143 Hypoxia Diseases 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 239000010903 husk Substances 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- -1 on the other hand Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 230000003014 reinforcing effect Effects 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000007788 roughening Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- ALVYUZIFSCKIFP-UHFFFAOYSA-N triethoxy(2-methylpropyl)silane Chemical compound CCO[Si](CC(C)C)(OCC)OCC ALVYUZIFSCKIFP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- 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
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
-
- 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
-
- 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
- B01J2220/4806—Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character
-
- 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
-
- 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
- B01J2220/4825—Polysaccharides or cellulose materials, e.g. starch, chitin, sawdust, wood, straw, cotton
Abstract
The invention discloses a preparation method of high-adsorbability biochar, which belongs to the field of biochar preparation and comprises the following steps: the method comprises the following steps: carrying out heat treatment on the carbon source to prepare biochar; step two: preparing silica sol, soaking biochar in the silica sol, taking out and drying to prepare a precursor; step three: dipping the precursor in the second step in organic glue, taking out the precursor to be placed in a multilayer gap, and ablating the precursor in the continuously flowing blast furnace tail gas to prepare an intermediate; step four: and (4) carrying out ultraviolet radiation treatment on the intermediate in the third step to prepare the high-adsorbability biochar. The method enables the surface of the biological carbon to be attached with carbon particles, so that the surface of the biological carbon is roughened, more adsorption sites of an adsorbed medium are provided, and high adsorption performance is realized.
Description
Technical Field
The invention relates to the technical field of charcoal preparation, and particularly relates to a preparation method of high-adsorptivity charcoal.
Background
Biochar is the solid matter left after the biomass material is pyrolyzed under the condition of oxygen deficiency or oxygen limitation to remove oil and gas in the biomass. Due to the unique physical and chemical properties of developed pores, large specific surface area, strong ion exchange capacity and the like, the heavy metal ions in the wastewater can be better and directly adsorbed and the waste gas can be better purified. However, the traditional preparation method of the biochar is easy to cause the collapse of pores, so that the adsorption performance is poor.
Disclosure of Invention
The invention aims to solve at least one technical problem in the prior art and provide a preparation method of high-adsorptivity biochar.
The technical solution of the invention is as follows:
a preparation method of high-adsorptivity biochar comprises the following steps:
the method comprises the following steps: carrying out heat treatment on a carbon source to prepare biochar;
step two: preparing silica sol, dipping the biochar in the silica sol, taking out and drying to prepare a precursor;
step three: dipping the precursor in the second step in organic glue, taking out the precursor to be placed in a multilayer gap, and ablating the precursor in the continuously circulating blast furnace tail gas to prepare an intermediate;
step four: and (4) carrying out ultraviolet radiation treatment on the intermediate in the third step to prepare the high-adsorbability biochar.
Preferably, in the first step, the carbon source is straw, husk or wood.
Preferably, in the second step, the volume ratio of the mass of the biochar to the silica sol is 1:3-10
Preferably, in the second step, before the biochar is immersed in the silica sol, the silica sol needs to be modified, specifically, a silane coupling agent is added into the silica sol, and the modified silica sol is obtained by stirring and acid-base adjustment.
Preferably, the pH value adjusted by acid and alkali is 2-6.
Preferably, in the third step, the organic glue is polyvinyl alcohol or epoxy resin.
Preferably, in the third step, the gas components of the blast furnace tail gas are as follows by volume: 25-36% of carbon monoxide, 18-39% of carbon dioxide, 42-68% of nitrogen, 0.1-0.4% of oxygen and the balance of impurity gas.
Preferably, in step three, carbon fibers are added to the precursor during the ablation process.
Preferably, in the third step, the specific gap of the multilayer gap is 10-30 cm.
Preferably, in the third step, the volume flow rate of the blast furnace tail gas is 60-80 mL/min.
The invention has at least one of the following beneficial effects:
(1) according to the preparation method of the biochar with high adsorbability, the biochar is pretreated in the silica sol, and the network structure of the silica sol supports the pore channels of the biochar, so that the collapse of the pore channels is prevented, and the enhancement effect is achieved; and then dipping the precursor in organic glue to coat a layer of adhesive layer on the surface of the precursor, then attaching carbon particles in blast furnace tail gas to the adhesive layer on one hand, reducing carbon dioxide in the blast furnace tail gas into carbon monoxide to form fuel gas to facilitate combustion, using a heat source for the second time, volatilizing the organic glue during burning to further provide a carbon source, and simultaneously attaching carbon particles to a multi-layer biochar intermediate to roughen the biochar surface and generate more adsorption sites.
(2) According to the preparation method of the high-adsorbability biochar, the biochar surface is provided with oxygen-containing functional groups through ultraviolet radiation treatment, so that the hydrophilicity is improved, and the attachment of liquid drops is facilitated.
(3) According to the preparation method of the high-adsorptivity biochar, the silica sol is modified in advance, so that the subsequent impregnation of organic glue is facilitated, and the compatibility between the silicon dioxide and the organic resin in the silica sol can be greatly improved.
Detailed Description
The present invention is further specifically described below with reference to examples, but the technical solution of the present invention is not limited to the scope of the following examples.
The following parts are to be construed in accordance with the parts by weight.
Example 1
A preparation method of high-adsorptivity biochar comprises the following steps:
the method comprises the following steps: carrying out heat treatment on the carbon source to prepare biochar; specifically, the rape straws are cut into about 1 cm, dried and heated to 510 ℃ under the condition of air isolation, and the temperature is maintained for 3.5 hours to obtain biochar;
step two: preparing silica sol, soaking biochar in the silica sol, taking out and drying to prepare a precursor; specifically, 100ml of water glass with the modulus of 3.2 is diluted in 200ml of water and stirred for 30min, and dilute nitric acid is added in the stirring process to ensure that the pH value of the mixed solution is 4.5, so as to obtain silica sol; 1 part of biochar is placed in 10 parts of silica sol for infiltration, and the mixture is cured for 5 days under the conditions that the temperature is 30 ℃ and the humidity is 65 percent, so that the mixture is fully cured and dried; and (3) soaking and washing the mixture by using water, washing out residual nitric acid and generated sodium nitrate, and airing to obtain a precursor.
Step three: and (2) soaking the precursor in the second step in polyvinyl alcohol for 1h, drying, taking out, placing in a gap of 3 layers, wherein the gap is 20cm, and ablating in continuously flowing blast furnace tail gas, wherein the volume flow of the blast furnace tail gas is 65 mL/min. Preparing an intermediate; wherein, according to the volume ratio, the gas composition of the blast furnace tail gas is as follows: 25% of carbon monoxide, 18% of carbon dioxide, 42% of nitrogen, 0.1% of oxygen and the balance of impurity gases.
Step four: and (4) carrying out ultraviolet radiation treatment on the intermediate in the third step to prepare the high-adsorbability biochar.
Example 2
A preparation method of high-adsorptivity biochar comprises the following steps:
the method comprises the following steps: carrying out heat treatment on the carbon source to prepare biochar; the method specifically comprises the steps of cutting wheat straws to about 1 cm, drying, heating to 530 ℃ under the condition of air isolation, and maintaining the temperature for 4 hours to obtain charcoal;
step two: preparing silica sol, soaking biochar in the silica sol, taking out and drying to prepare a precursor; specifically, 100ml of water glass with the modulus of 3.2 is diluted in 200ml of water and stirred for 30min, and dilute nitric acid is added during stirring to ensure that the pH value of the mixed solution is 4.5, so as to obtain silica sol; 1.5 parts of biochar is placed in 10 parts of silica sol for infiltration, and the mixture is cured for 5 days under the conditions that the temperature is 30 ℃ and the humidity is 65 percent, so that the mixture is fully cured and dried; and (3) soaking and washing the mixture by using water, washing out residual nitric acid and generated sodium nitrate, and airing to obtain a precursor.
Step three: and (3) soaking the precursor in the second step in polyvinyl alcohol for 1h, drying, taking out, placing in 3 layers of gaps with the gaps being 20cm, and ablating in continuously circulating blast furnace tail gas with the volume flow of 65 mL/min. Preparing an intermediate; wherein, according to the volume ratio, the gas composition of the blast furnace tail gas is as follows: 28% of carbon monoxide, 21% of carbon dioxide, 46% of nitrogen, 0.15% of oxygen and the balance of impurity gases.
Step four: and (4) carrying out ultraviolet radiation treatment on the intermediate in the third step to prepare the high-adsorbability biochar.
Example 3
A preparation method of high-adsorptivity biochar comprises the following steps:
the method comprises the following steps: carrying out heat treatment on a carbon source to prepare biochar; cutting the rice straw to about 1 cm, drying, heating to 480 ℃ under the condition of air isolation, and maintaining the temperature for 4 hours to obtain biochar;
step two: preparing silica sol, soaking biochar in the silica sol, taking out and drying to prepare a precursor; specifically, 100ml of water glass with the modulus of 3.2 is diluted in 200ml of water and stirred for 30min, and dilute nitric acid is added during stirring to ensure that the pH value of the mixed solution is 5.2, so as to obtain silica sol; placing 3 parts of biochar in 10 parts of silica sol for infiltration, and maintaining for 5 days under the conditions that the temperature is 30 ℃ and the humidity is 65% to fully solidify and dry the mixture; and (3) soaking and washing the mixture by using water, washing out residual nitric acid and generated sodium nitrate, and airing to obtain a precursor.
Step three: and (3) soaking the precursor in the second step in polyvinyl alcohol for 1h, drying, taking out, placing in 3 layers of gaps with the gaps being 20cm, and ablating in continuously circulating blast furnace tail gas with the volume flow of 65 mL/min. Preparing an intermediate; wherein, according to the volume ratio, the gas composition of the blast furnace tail gas is as follows: the carbon monoxide content is 31 percent, the carbon dioxide content is 19 percent, the nitrogen content is 41 percent, the oxygen content is 0.2 percent, and the balance is impurity gas.
Step four: and (4) carrying out ultraviolet radiation treatment on the intermediate in the third step to prepare the high-adsorbability biochar.
Example 4
In this embodiment, a change is made on the basis of embodiment 2, specifically, in the second step, before the biochar is immersed in the silica sol, the silica sol needs to be modified, specifically, 0.05 part of a silane coupling agent, specifically, isobutyltriethoxysilane, is added to the silica sol, and the mixture is stirred and acid-base adjusted to 4, so as to obtain the modified silica sol.
Example 5
In this embodiment, a change is made on the basis of embodiment 4, specifically, in the third step, 0.6 part of carbon fiber is added to the precursor during the ablation process.
Comparative example 1 (No blast furnace exhaust treatment)
A preparation method of high-adsorptivity biochar comprises the following steps:
the method comprises the following steps: carrying out heat treatment on a carbon source to prepare biochar; specifically, the method comprises the steps of chopping wheat straws to about 1 cm, drying, heating to 530 ℃ under the condition of air isolation, and maintaining the temperature for 4 hours to obtain biochar;
step two: preparing silica sol, soaking biochar in the silica sol, taking out and drying to prepare a precursor; specifically, 100ml of water glass with the modulus of 3.2 is diluted in 200ml of water and stirred for 30min, and dilute nitric acid is added during stirring to ensure that the pH value of the mixed solution is 4.5, so as to obtain silica sol; 1.5 parts of biochar is placed in 10 parts of silica sol for infiltration, and the mixture is cured for 5 days under the conditions that the temperature is 30 ℃ and the humidity is 65 percent, so that the mixture is fully cured and dried; and (3) soaking and washing the mixture by using water, washing out residual nitric acid and generated sodium nitrate, and airing to obtain a precursor.
Step three: and carrying out ultraviolet radiation treatment on the precursor to prepare the high-adsorbability biochar.
Comparative example 2 (without silica sol)
A preparation method of high-adsorptivity biochar comprises the following steps:
the method comprises the following steps: carrying out heat treatment on the carbon source to prepare biochar; specifically, the method comprises the steps of chopping wheat straws to about 1 cm, drying, heating to 530 ℃ under the condition of air isolation, and maintaining the temperature for 4 hours to obtain biochar;
step two: the biochar is firstly soaked in polyvinyl alcohol for 1h, then is dried and taken out to be placed in 3 layers of gaps, the gaps are 20cm, ablation is carried out in continuously circulating blast furnace tail gas, and the volume flow of the blast furnace tail gas is 65 mL/min. Preparing an intermediate; wherein, according to the volume ratio, the gas composition of the blast furnace tail gas is as follows: 28% of carbon monoxide, 21% of carbon dioxide, 46% of nitrogen, 0.15% of oxygen and the balance of impurity gases.
Step three: and carrying out ultraviolet radiation treatment on the intermediate to prepare the high-adsorbability biochar.
Comparative example 3 (Single layer precursor Placement)
A preparation method of high-adsorptivity biochar comprises the following steps:
the method comprises the following steps: carrying out heat treatment on a carbon source to prepare biochar; specifically, the method comprises the steps of chopping wheat straws to about 1 cm, drying, heating to 530 ℃ under the condition of air isolation, and maintaining the temperature for 4 hours to obtain biochar;
step two: preparing silica sol, soaking biochar in the silica sol, taking out and drying to prepare a precursor; specifically, 100ml of water glass with the modulus of 3.2 is diluted in 200ml of water and stirred for 30min, and dilute nitric acid is added in the stirring process to ensure that the pH value of the mixed solution is 4.5, so as to obtain silica sol; placing 1.5 parts of biochar in 10 parts of silica sol for infiltration, and maintaining for 5 days under the conditions that the temperature is 30 ℃ and the humidity is 65% to fully solidify and dry the mixture; and (3) soaking and washing the mixture by using water, washing out residual nitric acid and generated sodium nitrate, and airing to obtain a precursor.
Step three: and (3) soaking the precursor in the second step in polyvinyl alcohol for 1h, drying, taking out, placing in a single layer manner, and ablating in continuously circulating blast furnace tail gas, wherein the volume flow of the blast furnace tail gas is 65 mL/min. Preparing an intermediate; wherein, according to the volume ratio, the gas composition of blast furnace tail gas is: 28% of carbon monoxide, 21% of carbon dioxide, 46% of nitrogen, 0.15% of oxygen and the balance of impurity gases.
Step four: and (4) carrying out ultraviolet radiation treatment on the intermediate in the third step to prepare the high-adsorbability biochar.
Respectively testing the adsorption performance of the wastewater and the waste gas in the above examples and comparative examples; the specific test method is as follows:
and (3) wastewater testing: 5g of samples of examples and comparative examples were placed at 1mg/L (W) Before adsorption ) CdCl of (2) 2 In the solution, the solution was adsorbed at 30 ℃ for 12 hours, and the concentration (W) of the adsorbed solution was measured After adsorption ) The removal rate (%) was calculated, and the removal rate (%) was (W) Before adsorption -W After adsorption )/W Before adsorption ×100％。
And (3) waste gas testing: placing the mixture in a gas generator to statically adsorb organic gas (n-pentadecane gas) under the condition that the water bath temperature is 25 ℃; weighing after the adsorption is saturated, and testing the first adsorption capacity of the sample;
desorption performance: and (3) putting the adsorption material after adsorption saturation into a vacuum oven, desorbing for 1 hour under the condition that the vacuum degree is not lower than 95kPa, then adjusting the temperature of the oven to 70 ℃, and heating and desorbing for 2 hours under vacuum. And finally, adjusting the temperature of the oven to room temperature, cooling the adsorption material, raising the pressure of the oven to normal pressure, weighing the adsorption material, and circularly desorbing the adsorption material for 100 times to obtain the adsorption capacity of the adsorption material.
The adsorption capacity (qe) of the adsorbent material is calculated by the following formula:
q e ＝(m 2 -m 1 )/m 1
wherein: q. q.s e The mass of oil gas adsorbed by the unit mass of adsorption material is g/g; m is 1 Mass (g) of the adsorbing material before adsorption; m is a unit of 2 The mass (g) of the adsorbent after saturation.
Specific test values are shown in table 1.
TABLE 1 Performance test values of examples and comparative examples
As can be seen from table 1, the adsorption performance of the examples is better than that of the comparative examples, which shows that the samples of the examples have abundant gaps and high specific surface area, and is mainly obtained by the following reasons, according to comparative analysis of comparative example 1, the precursors are first soaked in organic glue, so that a layer of adhesive layer is coated on the surfaces of the precursors, then carbon particles in blast furnace tail gas are attached to the adhesive layer, on the other hand, carbon dioxide in the blast furnace tail gas is reduced into carbon monoxide, which becomes fuel gas and is beneficial to combustion, and secondary use of a heat source is facilitated, meanwhile, in the ablation process, the organic glue is combusted and volatilized to further provide a carbon source, and simultaneously, the carbon particles are attached to a multi-layer biochar intermediate, so that the biochar surface is roughened, more adsorption sites are generated, and the adsorption performance is improved. Comparative analysis of comparative example 2 shows that the silica sol is added in the example, and the network structure of the silica sol supports the pore channels of the biochar, so that the pore channels are prevented from collapsing and have a reinforcing effect. Comparative analysis of comparative example 3 shows that in the embodiment, the precursor is placed in the gaps of the plurality of layers, so that more carbon particles can be contacted, namely more carbon particles are attached to the surface of the biochar body, the roughening degree is higher, the carbon particles are favorable for the attachment of an adsorbed medium, and meanwhile, ultraviolet radiation treatment is carried out, so that the biochar surface is provided with oxygen-containing functional groups, the hydrophilicity is improved, the attachment of liquid drops is more favorable, and the adsorption performance is improved; meanwhile, the performances of the embodiments 4 and 5 are superior to those of the embodiments 1 to 3, and the subsequent impregnation of organic glue is facilitated mainly by modifying the silica sol in advance, so that the compatibility between the silicon dioxide and the organic resin in the silica sol can be greatly improved, and the stability of the pore channel can be further improved by the carbon fiber added in the embodiment 5. And it can also be seen from the table that the adsorption performance of the example is still excellent after desorption for 100 times, mainly because the pore structure in the example has better stability, the operation of desorption is more facilitated, and the collapse of the pore channel is avoided.
The above additional technical features can be freely combined and used in superposition by those skilled in the art without conflict.
In the description of the embodiments of the present invention, it should be understood that "-" and "-" indicate the same range as two numerical values, and the range includes the endpoints. For example: "A-B" means a range of greater than or equal to A and less than or equal to B. "A to B" means a range of not less than A and not more than B.
In the description of the embodiments of the present invention, the term "and/or" herein is only one kind of association relationship describing an associated object, and means that there may be three kinds of relationships, for example, a and/or B, and may mean: a exists alone, A and B exist simultaneously, and B exists alone. In addition, the character "/" herein generally indicates that the former and latter associated objects are in an "or" relationship.
The above description is only a preferred embodiment of the present invention, and the technical solutions that achieve the objects of the present invention by basically the same means are all within the protection scope of the present invention.
Claims (9)
1. A preparation method of high-adsorptivity biochar is characterized by comprising the following steps: comprises the following steps:
the method comprises the following steps: carrying out heat treatment on the carbon source to prepare biochar;
step two: preparing silica sol, soaking biochar in the silica sol, taking out and drying to prepare a precursor;
step three: dipping the precursor in the second step in organic glue, taking out the precursor to be placed in a multilayer gap, and ablating the precursor in the continuously circulating blast furnace tail gas to prepare an intermediate;
step four: carrying out ultraviolet radiation treatment on the intermediate in the third step to prepare high-adsorbability biochar;
the organic glue is polyvinyl alcohol or epoxy resin.
2. The method for preparing high adsorptivity biochar according to claim 1, wherein: in the first step, the carbon source is straw, fruit shell or wood.
3. The method for preparing high adsorptivity biochar according to claim 1, wherein the method comprises the following steps: in the second step, the volume ratio of the mass of the biochar to the silica sol is 1: 3-10.
4. The method for preparing high adsorptivity biochar according to claim 1, wherein the method comprises the following steps: in the second step, before the biochar is immersed in the silica sol, the silica sol needs to be modified, specifically, a silane coupling agent is added into the silica sol, and the modified silica sol is obtained by stirring and acid-base adjustment.
5. The method for preparing high adsorptivity biochar according to claim 4, wherein the method comprises the following steps: the pH value adjusted by the acid and the alkali is 2-6.
6. The method for preparing high adsorptivity biochar according to claim 1, wherein the method comprises the following steps: in the third step, the gas components of the blast furnace tail gas are as follows according to the volume ratio: 25-36% of carbon monoxide, 18-39% of carbon dioxide, 42-68% of nitrogen, 0.1-0.4% of oxygen and the balance of impurity gas.
7. The method for preparing high adsorptivity biochar according to claim 1, wherein the method comprises the following steps: and in the third step, carbon fiber is added into the precursor in the ablation process.
8. The method for preparing high adsorptivity biochar according to claim 1, wherein the method comprises the following steps: in the third step, the specific gap for placing the multiple layers of gaps is 10-30 cm.
9. The method for preparing high adsorptivity biochar according to claim 1, wherein the method comprises the following steps: in the third step, the volume flow of the blast furnace tail gas is 60-80 mL/min.
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