CN113816479A - Slow-release gel aluminum modified wood chip defluorinating agent and preparation method thereof - Google Patents
Slow-release gel aluminum modified wood chip defluorinating agent and preparation method thereof Download PDFInfo
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- CN113816479A CN113816479A CN202111162971.2A CN202111162971A CN113816479A CN 113816479 A CN113816479 A CN 113816479A CN 202111162971 A CN202111162971 A CN 202111162971A CN 113816479 A CN113816479 A CN 113816479A
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- 239000002023 wood Substances 0.000 title claims abstract description 47
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 34
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 34
- 239000003795 chemical substances by application Substances 0.000 title claims abstract description 34
- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- VSCWAEJMTAWNJL-UHFFFAOYSA-K aluminium trichloride Chemical compound Cl[Al](Cl)Cl VSCWAEJMTAWNJL-UHFFFAOYSA-K 0.000 claims abstract description 38
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 claims abstract description 25
- 229910052731 fluorine Inorganic materials 0.000 claims abstract description 25
- 239000011737 fluorine Substances 0.000 claims abstract description 25
- 238000001035 drying Methods 0.000 claims abstract description 18
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000004202 carbamide Substances 0.000 claims abstract description 17
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 16
- 238000000227 grinding Methods 0.000 claims abstract description 10
- 239000000047 product Substances 0.000 claims abstract description 10
- 238000005406 washing Methods 0.000 claims abstract description 8
- 238000000926 separation method Methods 0.000 claims abstract description 7
- 239000007788 liquid Substances 0.000 claims abstract description 6
- 239000000203 mixture Substances 0.000 claims abstract description 6
- 239000002244 precipitate Substances 0.000 claims abstract description 6
- 238000002156 mixing Methods 0.000 claims description 8
- 239000006228 supernatant Substances 0.000 claims description 5
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 5
- 239000012498 ultrapure water Substances 0.000 claims description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- RPNUMPOLZDHAAY-UHFFFAOYSA-N Diethylenetriamine Chemical compound NCCNCCN RPNUMPOLZDHAAY-UHFFFAOYSA-N 0.000 claims description 3
- BUFXWXARYFFAGB-UHFFFAOYSA-N O.O.O.O.O.O.O.O.O.O.[Ca++].[O-][N+]([O-])=O.[O-][N+]([O-])=O Chemical compound O.O.O.O.O.O.O.O.O.O.[Ca++].[O-][N+]([O-])=O.[O-][N+]([O-])=O BUFXWXARYFFAGB-UHFFFAOYSA-N 0.000 claims description 3
- 239000004115 Sodium Silicate Substances 0.000 claims description 3
- 229910021389 graphene Inorganic materials 0.000 claims description 3
- 229940050906 magnesium chloride hexahydrate Drugs 0.000 claims description 3
- DHRRIBDTHFBPNG-UHFFFAOYSA-L magnesium dichloride hexahydrate Chemical compound O.O.O.O.O.O.[Mg+2].[Cl-].[Cl-] DHRRIBDTHFBPNG-UHFFFAOYSA-L 0.000 claims description 3
- 238000012545 processing Methods 0.000 claims description 3
- 230000035484 reaction time Effects 0.000 claims description 3
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 claims description 3
- 229910052911 sodium silicate Inorganic materials 0.000 claims description 3
- 238000005303 weighing Methods 0.000 claims description 3
- 238000001291 vacuum drying Methods 0.000 claims description 2
- 238000001179 sorption measurement Methods 0.000 abstract description 20
- 239000003463 adsorbent Substances 0.000 abstract description 8
- 238000006115 defluorination reaction Methods 0.000 abstract description 7
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 abstract description 3
- 238000000034 method Methods 0.000 description 10
- 230000000694 effects Effects 0.000 description 5
- 238000011069 regeneration method Methods 0.000 description 5
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 229910052761 rare earth metal Inorganic materials 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- 230000008929 regeneration Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 2
- 230000009471 action Effects 0.000 description 2
- 239000003513 alkali Substances 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 230000007547 defect Effects 0.000 description 2
- 239000008394 flocculating agent Substances 0.000 description 2
- 238000012423 maintenance Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 150000003839 salts Chemical class 0.000 description 2
- 239000002351 wastewater Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- 229910052684 Cerium Inorganic materials 0.000 description 1
- 241000207199 Citrus Species 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 159000000007 calcium salts Chemical class 0.000 description 1
- 238000009388 chemical precipitation Methods 0.000 description 1
- 235000020971 citrus fruits Nutrition 0.000 description 1
- 238000005345 coagulation Methods 0.000 description 1
- 230000015271 coagulation Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000001419 dependent effect Effects 0.000 description 1
- 239000003651 drinking water Substances 0.000 description 1
- 235000020188 drinking water Nutrition 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005189 flocculation Methods 0.000 description 1
- 230000016615 flocculation Effects 0.000 description 1
- 230000007062 hydrolysis Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 230000033444 hydroxylation Effects 0.000 description 1
- 238000005805 hydroxylation reaction Methods 0.000 description 1
- 238000011065 in-situ storage Methods 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 229910052746 lanthanum Inorganic materials 0.000 description 1
- 238000011068 loading method Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 229910000402 monopotassium phosphate Inorganic materials 0.000 description 1
- 235000019796 monopotassium phosphate Nutrition 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 238000010979 pH adjustment Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- GNSKLFRGEWLPPA-UHFFFAOYSA-M potassium dihydrogen phosphate Chemical compound [K+].OP(O)([O-])=O GNSKLFRGEWLPPA-UHFFFAOYSA-M 0.000 description 1
- LWIHDJKSTIGBAC-UHFFFAOYSA-K potassium phosphate Substances [K+].[K+].[K+].[O-]P([O-])([O-])=O LWIHDJKSTIGBAC-UHFFFAOYSA-K 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- -1 rare earth metal salts Chemical class 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000004576 sand Substances 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 238000007873 sieving Methods 0.000 description 1
- 239000010802 sludge Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 239000010875 treated wood Substances 0.000 description 1
- 238000001132 ultrasonic dispersion Methods 0.000 description 1
- 238000004065 wastewater treatment Methods 0.000 description 1
- 229910052727 yttrium Inorganic materials 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- 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
- C02F1/58—Treatment of water, waste water, or sewage by removing specified dissolved compounds
- C02F1/583—Treatment of water, waste water, or sewage by removing specified dissolved compounds by removing fluoride or fluorine compounds
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/12—Halogens or halogen-containing compounds
- C02F2101/14—Fluorine or fluorine-containing compounds
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
Abstract
The application discloses a slow-release gel aluminum modified wood chip defluorinating agent and a preparation method thereof, wherein an aluminum chloride solution, a urea solution and wood chips are fully mixed according to a proportion; transferring the mixture into a hydrothermal reaction kettle, and reacting for more than or equal to 9 hours at the temperature of 100 ℃ and 120 ℃; performing centrifugal separation on the product liquid after the hydrothermal reaction, washing the precipitate obtained by the centrifugal separation, drying and grinding to obtain the slow-release gel aluminum modified wood chip defluorinating agent; the prepared gel-like adsorbent is dried and ground for defluorination, so that the pH range of defluorination of aluminum oxide can be widened to 5-8. When fluorine is adsorbed, the fluorine removal rate can reach more than 90 percent, and the adsorption capacity is 60-120 mg/g.
Description
Technical Field
The invention belongs to the technical field of removal of fluoride in water and wastewater, and particularly relates to a slow-release gel aluminum modified wood chip defluorinating agent and a preparation method thereof.
Background
In the present fluorine removal technical field, an adsorption method, a coagulation method, an ion exchange method and a membrane method are commonly used. Among them, the adsorption method is considered as a low-cost, simple and effective defluorination method. However, many of the initiatives relating to fluorine reduction have resulted in frustration and failure. A large number of projects are in practice poorly operated due to limited removal efficiency, high cost, complex operation and laborious maintenance.
The research finds that the rare earth elements Ce, La, Y and the like also have excellent fluorine removal performance, but the high cost of the preparation of the adsorbent and the complicated regeneration process also prevent the large-scale application of the adsorbent in practice. Inorganic metal oxides, organic adsorbents, and other low cost materials have been proposed for fluoride removal. Among these adsorbents, alumina is the most widely used adsorbent, but its further use is limited by low adsorption capacity at neutral pH, poor adsorption kinetics and difficulty in regeneration.
The removal of fluorine is strongly pH dependent and therefore pH adjustment is often used in practice. Although the in-situ preparation and regeneration method can keep the surface adsorption activity as much as possible and overcome some defects involved in the conventional regeneration method, the application pH range is narrow, the fluorine removal efficiency is not high, and further optimization is needed.
Aluminum oxide has good adsorption performance and is a recognized defluorinating agent. The common activated alumina has the adsorption capacity of 10-20 mg/g, the pH application range is narrow, generally between 4 and 6, the adsorption capacity is not high, and the method is limited to be applied under the condition of partial acid.
The sawdust has a natural pore structure and a large specific surface area, is wide in source and low in cost, is well applied to the wood processing industry, and is lack of application reports in the water treatment industry.
Chinese patent CN201910070431.8 discloses a wastewater high-efficiency fluorine removal agent and a preparation method thereof. Is prepared by combining various rare earth metal salts with inorganic metal salts. The rare earth metal salt forms hydroxylation under certain conditions, is dispersed under the combined action of various metal salts to form a fluorine-philic complex, forms floccules under the action of a flocculating agent, and is directly precipitated, so that the defluorination effect is achieved, the advantages of chemical precipitation, flocculation precipitation and adsorption defluorination technologies are taken into consideration, calcium salt does not need to be additionally added, and flocculating agent and adsorbent do not need to be additionally added. The effects of removing fluorine, ss and other harmful substances can be met only by one set of integrated wastewater treatment equipment. Both the early construction cost and the floor space are greatly saved, and the later operation is greatly saved, but the prior art is slightly insufficient considering that the removal efficiency is limited, the cost is high, the operation is complex, the maintenance is laborious, the application pH range is narrow, the fluorine removal efficiency is not high, the adsorption capacity is not high, the adsorption kinetics is poor and the regeneration is difficult. Chinese patent CN201910368930.5 discloses a biochar citrus seedling culture substrate which is prepared by mixing the following raw materials in parts by mass: 30-35 parts of loess, 30-35 parts of sawdust, 10-15 parts of river sand, 10-15 parts of biochar, 3-5 parts of monopotassium phosphate and 3-5 parts of urea; wherein, the main raw materials of the biochar are sludge in a sedimentation tank of a waterworks, wood chips obtained by crushing plant branches and the like; however, the prior art is slightly insufficient in view of the lack of the fluorine removal effect.
Disclosure of Invention
The technical problem to be solved is as follows:
aiming at the defects of the prior art, the method solves the problems of limited removal efficiency, high cost, complex operation, narrow application pH range, low defluorination efficiency, low adsorption capacity and poor adsorption kinetics in the prior art; provides a slow-release gel aluminum modified wood chip defluorinating agent and a preparation method thereof. The aluminum salt can obtain a novel gel aluminum different from other conventional alumina by the forced hydrolysis of urea slow-release alkali under the hydrothermal condition, which is a high-efficiency defluorinating agent and has rich defluorination active sites. The application range is slightly widened, but the cost is probably slightly higher due to more consumption of chemical raw materials.
The technical scheme is as follows:
in order to achieve the purpose, the application is realized by the following technical scheme:
a slow-release gel aluminum modified wood chip defluorinating agent and a preparation method thereof are disclosed, wherein the preparation method comprises the following specific steps:
the first step is as follows: fully mixing the aluminum chloride solution, the urea solution and the wood chips according to the proportion;
secondly, transferring the mixture into a hydrothermal reaction kettle, and reacting for more than or equal to 9 hours at the temperature of 100-120 ℃;
and thirdly, centrifugally separating the product liquid obtained after the hydrothermal reaction in the second step, washing the precipitate obtained by centrifugal separation, drying and grinding to obtain the slow-release gel aluminum modified wood chip defluorinating agent.
As a preferred technical scheme of the invention: in the first step, the molar ratio of the aluminum chloride solution to the urea solution is 1:2-4, the volume ratio is 1:1.1-1.5, and the mass ratio of the aluminum chloride solution to the wood chips is 1: 5-10.
As a preferred technical scheme of the invention: before mixing the wood chips with the aluminum chloride solution and the urea solution in the first step, firstly weighing 100 parts of the wood chips, 1-5 parts of graphene oxide, 3-7 parts of magnesium chloride hexahydrate, 2-6 parts of calcium nitrate decahydrate, 3-5 parts of sodium silicate and 2-4 parts of diethylenetriamine according to the mass parts, ultrasonically dispersing for 2 hours, then centrifuging at the speed of 3000rpm, grinding after vacuum drying, and processing the wood chips through a 200-mesh 400-mesh sieve.
As a preferred technical scheme of the invention: the capacity of the hydrothermal reaction kettle in the second step is 50 mL.
As a preferred technical scheme of the invention: the reaction time in the second step is 9 to 11 hours.
As a preferred technical scheme of the invention: the washing in the third step is specifically as follows: the supernatant was washed with ultrapure water and was transparent.
As a preferred technical scheme of the invention: and the drying temperature in the third step is 90-100 ℃, and the drying time is 6-8 h.
The application also discloses the slow-release gel aluminum modified wood chip defluorinating agent prepared by the preparation method.
Has the advantages that:
the application provides a slow-release gel aluminum modified wood chip defluorinating agent and a preparation method thereof, and compared with the prior art, the slow-release gel aluminum modified wood chip defluorinating agent has the following beneficial effects:
1. the novel gel aluminum modified sawdust defluorinating agent is prepared by utilizing the natural adsorption potential of sawdust and further loading the active gel aluminum high-efficiency defluorinating component, the synergistic effect of the gel aluminum modified sawdust defluorinating agent and the active gel aluminum can be exerted, the cost is reduced, the defluorinating efficiency can be ensured, the product is safe and nontoxic, and the novel gel aluminum modified sawdust defluorinating agent has a good application prospect in the aspects of drinking water sanitation and safety guarantee.
2. The prepared slow-release gel aluminum modified wood chip fluorine removal agent has good adsorption performance and large adsorption capacity, and can keep better fluorine removal performance in a larger acid-base range.
3. Replacing the strong base NaOH commonly used in the preparation of aluminum oxideConversion to weakly basic urea (CO (NH)2)2) The hydroxyl (OH) is hydrothermally generated-) Slowly releases to achieve the effect of slowly adding alkali.
4. And drying and grinding the prepared gel-like adsorbent for removing fluorine.
5. The colloidal Al30 can be more conveniently obtained by controlling the high-temperature hydrothermal reaction conditions of the product.
6. When the fluorine removing agent is used for adsorbing fluorine, the fluorine removing rate can reach more than 90 percent, and the adsorption capacity is 60-120 mg/g.
7. The pH range of the aluminum oxide for removing fluorine can be widened to be 5-8.
8. The adsorption capacity is greatly improved; the application range is widened; the material consumption is less, low-cost sawdust is introduced, and the comprehensive cost performance is high.
Detailed Description
The following will further explain the embodiments and working procedures of the present invention by referring to examples.
Example 1:
a slow-release gel aluminum modified wood chip defluorinating agent and a preparation method thereof are disclosed, which comprises the following steps:
the first step is as follows: weighing 100 parts of wood chips, 1-5 parts of graphene oxide, 3-7 parts of magnesium chloride hexahydrate, 2-6 parts of calcium nitrate decahydrate, 3-5 parts of sodium silicate and 2-4 parts of diethylenetriamine according to the mass parts, performing ultrasonic dispersion for 2 hours, centrifuging at the speed of 3000rpm, drying in vacuum, grinding, sieving with a 200-mesh sieve and a 400-mesh sieve to treat the wood chips, and fully mixing an aluminum chloride solution, a urea solution and the treated wood chips according to the proportion; the molar ratio of the aluminum chloride solution to the urea solution is 1: 4, the volume ratio is 1: 1.5, and the mass ratio of the aluminum chloride solution to the wood chips is 1: 10;
secondly, transferring the mixture into a hydrothermal reaction kettle with the capacity of 50mL, and reacting for 11h at 120 ℃;
and thirdly, centrifugally separating the product liquid obtained after the hydrothermal reaction in the second step, washing the precipitate obtained by centrifugal separation with ultrapure water until the supernatant is transparent, drying and grinding, wherein the drying temperature is 100 ℃, and drying is carried out for 8 hours to obtain the slow-release gel aluminum modified wood chip defluorinating agent.
Example 2:
a slow-release gel aluminum modified wood chip defluorinating agent and a preparation method thereof are disclosed, which comprises the following steps:
the first step is as follows: fully mixing the aluminum chloride solution, the urea solution and the wood chips according to the proportion; the molar ratio of the aluminum chloride solution to the urea solution is 1:3, the volume ratio of the aluminum chloride solution to the urea solution is 1:1.3, and the mass ratio of the aluminum chloride solution to the wood chips is 1: 8;
secondly, transferring the mixture into a hydrothermal reaction kettle with the capacity of 50mL, and reacting for 10 hours at 110 ℃;
and thirdly, centrifugally separating the product liquid obtained after the hydrothermal reaction in the second step, washing the precipitate obtained by centrifugal separation with ultrapure water until the supernatant is transparent, drying and grinding, wherein the drying temperature is 95 ℃, and drying for 7 hours to obtain the slow-release gel aluminum modified wood chip defluorinating agent.
Example 3:
a slow-release gel aluminum modified wood chip defluorinating agent and a preparation method thereof are disclosed, which comprises the following steps:
the first step is as follows: fully mixing the aluminum chloride solution, the urea solution and the wood chips according to the proportion; the molar ratio of the aluminum chloride solution to the urea solution is 1:2, the volume ratio is 1:1.1, and the mass ratio of the aluminum chloride solution to the wood chips is 1: 5;
secondly, transferring the mixture into a hydrothermal reaction kettle with the capacity of 50mL, and reacting for 9 hours at the temperature of 100 ℃;
and thirdly, centrifugally separating the product liquid obtained after the hydrothermal reaction in the second step, washing the precipitate obtained by centrifugal separation with ultrapure water until the supernatant is transparent, drying and grinding, wherein the drying temperature is 90 ℃, and drying for 6 hours to obtain the slow-release gel aluminum modified wood chip defluorinating agent.
Hydrothermal reaction time and temperature; the addition amount of the substance and other parameters are controlled within a set range to obtain different products, and the adsorption capacity of the products is changed between 60 and 120 mg/g.
Finally, the above embodiments are only for illustrating the technical solutions of the present invention and not for limiting, and other modifications or equivalent substitutions made by the technical solutions of the present invention by the person skilled in the art shall be covered by the scope of the claims of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (8)
1. A preparation method of a slow-release gel aluminum modified wood chip defluorinating agent is characterized by comprising the following steps: the preparation method comprises the following specific steps:
the first step is as follows: fully mixing the aluminum chloride solution, the urea solution and the wood chips according to the proportion;
secondly, transferring the mixture into a hydrothermal reaction kettle, and reacting for more than or equal to 9 hours at the temperature of 100-120 ℃;
and thirdly, centrifugally separating the product liquid obtained after the hydrothermal reaction in the second step, washing the precipitate obtained by centrifugal separation, drying and grinding to obtain the slow-release gel aluminum modified wood chip defluorinating agent.
2. The preparation method of the slow-release gel aluminum modified wood chip fluorine removal agent according to claim 1, which is characterized by comprising the following steps: in the first step, the molar ratio of the aluminum chloride solution to the urea solution is 1:2-4, the volume ratio is 1:1.1-1.5, and the mass ratio of the aluminum chloride solution to the wood chips is 1: 5-10.
3. The preparation method of the slow-release gel aluminum modified wood chip fluorine removal agent according to claim 2, characterized in that: before mixing the wood chips with the aluminum chloride solution and the urea solution in the first step, firstly weighing 100 parts of the wood chips, 1-5 parts of graphene oxide, 3-7 parts of magnesium chloride hexahydrate, 2-6 parts of calcium nitrate decahydrate, 3-5 parts of sodium silicate and 2-4 parts of diethylenetriamine according to the mass parts, ultrasonically dispersing for 2 hours, then centrifuging at the speed of 3000rpm, grinding after vacuum drying, and processing the wood chips through a 200-mesh 400-mesh sieve.
4. The preparation method of the slow-release gel aluminum modified wood chip fluorine removal agent according to claim 1, which is characterized by comprising the following steps: the capacity of the hydrothermal reaction kettle in the second step is 50 mL.
5. The preparation method of the slow-release gel aluminum modified wood chip fluorine removal agent according to claim 1, which is characterized by comprising the following steps: the reaction time in the second step is 9-11 h.
6. The preparation method of the slow-release gel aluminum modified wood chip fluorine removal agent according to claim 1, which is characterized by comprising the following steps: the washing in the third step is specifically as follows: the supernatant was washed with ultrapure water and was transparent.
7. The preparation method of the slow-release gel aluminum modified wood chip fluorine removal agent according to claim 1, which is characterized by comprising the following steps: and in the third step, the drying temperature is 90-100 ℃, and the drying time is 6-8 h.
8. The slow-release gel aluminum modified wood chip fluorine removal agent prepared by the preparation method of any one of claims 1 to 7.
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CN106824066A (en) * | 2016-12-30 | 2017-06-13 | 贵州科学院 | Modified zirconium hydroxide composite adsorbing material of the 3D Graphenes of fluorine ion and preparation method thereof in a kind of removal rural potable water |
CN109760172A (en) * | 2019-02-20 | 2019-05-17 | 李小梅 | A kind of preparation method of hydrophobic wood |
CN112121772A (en) * | 2020-09-27 | 2020-12-25 | 南通大学 | Defluorination wood film filtering device |
-
2021
- 2021-09-30 CN CN202111162971.2A patent/CN113816479A/en active Pending
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
CN106268644A (en) * | 2016-09-12 | 2017-01-04 | 方亚鹏 | A kind of High-efficient Water scavenging material and preparation method and application |
CN106824066A (en) * | 2016-12-30 | 2017-06-13 | 贵州科学院 | Modified zirconium hydroxide composite adsorbing material of the 3D Graphenes of fluorine ion and preparation method thereof in a kind of removal rural potable water |
CN109760172A (en) * | 2019-02-20 | 2019-05-17 | 李小梅 | A kind of preparation method of hydrophobic wood |
CN112121772A (en) * | 2020-09-27 | 2020-12-25 | 南通大学 | Defluorination wood film filtering device |
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Application publication date: 20211221 |