CN105854800A - Method for preparing modified charcoal by utilizing aquatic plant wastes and hydrochloric acid - Google Patents
Method for preparing modified charcoal by utilizing aquatic plant wastes and hydrochloric acid Download PDFInfo
- Publication number
- CN105854800A CN105854800A CN201610274484.8A CN201610274484A CN105854800A CN 105854800 A CN105854800 A CN 105854800A CN 201610274484 A CN201610274484 A CN 201610274484A CN 105854800 A CN105854800 A CN 105854800A
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- Prior art keywords
- charcoal
- hydrochloric acid
- water plant
- aquatic plant
- garbage
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—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
-
- 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
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/283—Treatment of water, waste water, or sewage by sorption using coal, charred products, or inorganic mixtures containing them
-
- 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
- C02F2101/16—Nitrogen compounds, e.g. ammonia
- C02F2101/163—Nitrates
Abstract
The invention belongs to the technical field of water treatment and specifically relates to a method for preparing modified charcoal by utilizing aquatic plant wastes and hydrochloric acid. The method comprises the following steps: (1) naturally drying aquatic plants, and then grinding, thereby acquiring aquatic plant powder; (2) weighing the aquatic plant powder, putting into a box-type atmosphere furnace and introducing nitrogen, increasing the temperature of the program to target temperature and keeping end temperature for pyrogenic decomposition, thereby acquiring the aquatic plant charcoal; (3) repeatedly cleaning the aquatic plant charcoal with deionized water till the aquatic plant charcoal is neutral, and drying; (4) weighing the aquatic plant charcoal, soaking into hydrochloric acid and stirring; (5) putting the mixture into a reaction kettle and modifying by using a microwave digestion instrument; and (6) taking out the aquatic plant charcoal, repeatedly washing with deionized water and putting into an air drying oven for drying, thereby acquiring the target product of modified charcoal. The modified charcoal prepared according to the method provided by the invention has strong nitrate adsorption capacity, high stability, reusability and no secondary pollution.
Description
Technical field
The invention belongs to water-treatment technology field, be specifically related to a kind of method utilizing water plant garbage and hydrochloric acid to prepare modification biological charcoal.
Background technology
Along with socioeconomic fast development, a large amount of waste water and agricultural run-off enter natural water, cause water body nitrate content to raise, and eutrophication problem is on the rise, and human health will be had a negative impact by the water body that long-term drink nitrate content exceeds standard.
Artificial swamp becomes to receive an acclaim as a kind of simple and economic mode, by absorption and the Denitrification of root system of water plant, effectively reduces and comprises agricultural run-off and the nitrate of Treating Municipal Sewage high-load.Artificial swamp removes that the nitrate in water body is important depends on plant absorption and Denitrification.Wherein, temperature is very important factor.
Reducing in northern China artificial wet land system in winter temperature, Denitrification weakens, and the clearance of nitrate nitrogen reduces.Further, owing to emergent aquactic plant can be become feeble and die in autumn and winter decomposition, water body is caused secondary pollution.How to ensure that north of china in winter artificial swamp is properly functioning, and improve resource utilization, be focus and the difficult point of north of china in winter artificial wetland treatment height nitrate wastewater now.
Study both at home and abroad and prepared charcoal for plant refuse and carry out the research of adsorbed water body pollutant.Charcoal is the class that under anaerobic conditions produces through high temperature pyrolysis of the biological residuum solid mixt rich in carbon element, is a kind of novel, cheap adsorbing material.Therefore the water plant litter of autumn and winter can be prepared as charcoal and remove the high nitrate nitrogen in water body, studies have shown that, owing to charcoal surface is with negative charge, its cation exchange capacity (CEC) is higher than anion exchange capacity, charcoal primary attachment cation and can not adsorpting anion, charcoal itself is the lowest to nitrate absorbability absorbability.
Charcoal is modified, to improve its absorbability to nitrate by the method that has now.Such as, a kind of common method is to utilize pyrolysis FeCl3Charcoal is carried out load iron process, the charcoal absorbability to water body nitrate can be heightened greatly.But, the iron ion of charcoal load likely can produce certain impact to water body, and the method is relatively complicated and expensive.
Summary of the invention
It is contemplated that provide a kind of method utilizing water plant garbage and hydrochloric acid to prepare modification biological charcoal in place of overcoming the deficiencies in the prior art.Modification biological charcoal prepared by this method is to nitrate high adsorption capacity, and stability is high, reusable, and non-secondary pollution can be used for removing artificial swamp height nitrate wastewater in northern China winter.
For solving above-mentioned technical problem, the present invention is realized in.
The method utilizing water plant garbage and hydrochloric acid to prepare modification biological charcoal, can implement as follows.
(1) by water plant natural air drying so that it is inner aqueous rate is less than 10%, then pulverizes 100 mesh sieve, it is thus achieved that water plant powder.
(2) weigh step (1) described water plant powder, be placed in box atmosphere furnace, in stove, be passed through nitrogen；Temperature programming, to target temperature, keeps final temperature pyrolysis；After pyrolytic process terminates, obtain water plant charcoal.
(3) step (2) described water plant charcoal deionized water is cleaned repeatedly 80 DEG C of drying in air drying cabinet to neutrality.
(4) weigh step (3) a certain amount of water plant charcoal, be immersed in a certain amount of hydrochloric acid, stir certain time.
(5) step (4) gained mixture is put in reactor, place in immersion microwave dissolver and be modified certain time.
(6) take out through the water plant charcoal of hydrochloric Acid Modification, after repeatedly rinsing with deionized water, put in air drying cabinet 80 DEG C and be dried；Obtain purpose product modification charcoal.
As a kind of preferred version, water plant of the present invention is the one in phragmites communis, Herba Typhae or hay grass.
Further, in step of the present invention (2), in stove, nitrogen flow rate is 400 mL/min；Programmed rate controls 10 DEG C/min；Target temperature is 700 DEG C；At 700 DEG C, final temperature pyrolysis continues 20 min.
Further, in step of the present invention (4), the mass volume ratio of charcoal and hydrochloric acid is 1:20；Wherein the mass unit of water plant charcoal is gram, and the unit of hydrochloric acid volume is milliliter.
Further, step of the present invention is stirred by agitator in (4), and mixing time is 2 h, and stir speed (S.S.) is 200 rpm.
Further, in step of the present invention (5), in microwave dissolver, modification time is 24 h.
Therefore, in artificial swamp, the water plant in winter is abundant and cheap low cost natural material, and the hydrochloric Acid Modification water plant charcoal prepared by the method is with low cost.And water plant can be collected at artificial swamp situ and prepare charcoal, and again be moved in artificial swamp, decrease cost of transportation.
Compared with prior art, the present invention has following features.
(1) compared with existing charcoal or class charcoal adsorber technologies, the hydrochloric Acid Modification water plant charcoal that the present invention provides has possessed the strongest absorbability to nitrate, and absorption property is the highest；Phragmites communis and Herba Typhae by hydrochloric Acid Modification are respectively 14.6661mg g to the maximum adsorption value of nitrate− 1 and 5.5559 mg·g− 1.And other people document is by preparing the modification biological charcoal maximum adsorption value to nitrate only at 1-3
mg·g− 1Between.
(2) the hydrochloric Acid Modification charcoal that the present invention provides, the water plant garbage of utilization is very cheap and is readily available raw material.
(3) modification that the present invention is carried out by chemical modification method, has suitable stability, desorption and regeneration can reusing after absorption.
(4) preparation method that the present invention provides is simple, it is easy to industrialized production.
Modification biological charcoal prepared by the present invention has particularly excellent treatment effect for nitrate nitrogen waste water high in northern China artificial swamp in winter.
20 g modification phragmites communis charcoals are added to concentration is 12.5 mg L-11 L high nitrate nitrogen waste water in, nitrate nitrogen content reduces rapidly, has reached 46.22% at 5min nitrate nitrogen clearance, and at the 320th min, nitrate nitrogen clearance reaches the highest, sees Fig. 2 for 74.35%().Through the adsorption of modification biological charcoal, absorption quickly reaches balance, and nitrate is removed by quick adsorption, and the modification biological charcoal after absorption can be recycled by after acid solution eluting.The higher rate of adsorption has great significance for reality application, and the rate of adsorption comparatively fast may insure that higher removal efficiency.By the water plant litter collected from artificial swamp, after being prepared into modification biological charcoal, put into again in artificial swamp, can effectively remove the nitrate nitrogen in sewage, promote the operational paradigm of artificial swamp autumn and winter, and promote the recycling of water plant.
Be can be seen that by scanning electron microscope result (seeing Fig. 3), modification biological carbon surface prepared by water plant garbage and hydrochloric acid is smooth, there is many holes, and hole presents irregular shape more, it may be possible to before 700 DEG C, high temperature causes cellulose etc. by considerable damage, makes surface deposits start to tail off, it is smooth that surface becomes, and form micropore, high temperature and hydrochloric acid activation and cause charcoal specific surface area to expand, so it is more beneficial for providing more adsorption site into modification biological charcoal.
Accompanying drawing explanation
The invention will be further described with detailed description of the invention below in conjunction with the accompanying drawings.Protection scope of the present invention is not only limited to the statement of following content.
Fig. 1 is the process flow diagram of the present invention.
Fig. 2 is the adsorption effect figure that 1 L is taken from artificial swamp height nitrate wastewater by 20 g hydrochloric Acid Modification phragmites communis charcoals.
Fig. 3 is the modification biological charcoal scanning electron microscope (SEM) photograph that water plant phragmites communis is prepared with hydrochloric acid.
Detailed description of the invention
As it can be seen, the present invention uses the ETHOS that Milestone company produces in an embodiment
UP type microwave dissolver carries out micro-wave digestion, the CJJ78-1 type precision reinforcement motor stirrer using Ai Ce company limited to produce is stirred, the box atmosphere furnace of MXQ using Shanghai travel incognito Lu Ye company limited to produce carries out high temperature anaerobic cracking, uses the concentration of the UV-2450 UV spectrophotometer measuring nitrate of Shimadzu SHIMADZU company production.The JSM-6360LA type scanning electron microscope using JEOL company to produce measures the surface topography of modification biological charcoal.
Embodiment
Al
。
(1) by phragmites communis natural air drying so that it is inner aqueous rate is less than 10%, 100 mesh sieve are crossed after then pulverizer is pulverized, it is thus achieved that phragmites communis powder.
(2) weighing step (1) described phragmites communis powder, be placed in box atmosphere furnace, be passed through nitrogen in stove, in stove, nitrogen flow rate is 400 mL/min, and programmed rate controls 10 DEG C/min, and target temperature is 700 DEG C；At 700 DEG C, final temperature pyrolysis continues 20 min.After pyrolytic process terminates, obtain phragmites communis charcoal.
(3) phragmites communis charcoal deionized water is cleaned repeatedly 80 DEG C of drying in air drying cabinet to neutrality.
(4) weighing step (3) 10 g phragmites communis charcoal, be immersed in the hydrochloric acid of 200 mL, stir 2 h by blender, stir speed (S.S.) is 200 rpm.
(5) step (4) gained mixture is put in reactor, place in immersion microwave dissolver and be modified 24 h.
(6) take out through the phragmites communis charcoal of hydrochloric Acid Modification, after repeatedly rinsing with deionized water, put in air drying cabinet 80 DEG C and be dried, final obtain hydrochloric Acid Modification phragmites communis charcoal.
Embodiment
A2
。
(1) by Herba Typhae natural air drying so that it is inner aqueous rate is less than 10%, 100 mesh sieve are crossed after then pulverizer is pulverized, it is thus achieved that typha powder.
(2) weighing step (1) described typha powder, be placed in box atmosphere furnace, be passed through nitrogen in stove, in stove, nitrogen flow rate is 400 mL/min, and programmed rate controls 10 DEG C/min, and target temperature is 700 DEG C；At 700 DEG C, final temperature pyrolysis continues 20 min.After pyrolytic process terminates, obtain Herba Typhae charcoal.
(3) Herba Typhae charcoal deionized water is cleaned repeatedly 80 DEG C of drying in air drying cabinet to neutrality.
(4) weighing step (3) 10g Herba Typhae charcoal, be immersed in the hydrochloric acid of 200 mL, stir 2 h by blender, stir speed (S.S.) is 200 rpm.
(5) step (4) gained mixture is put in reactor, place in immersion microwave dissolver and be modified 24h.
(6) take out through the modified phragmites communis charcoal of Herba Typhae, after repeatedly rinsing with deionized water, put in air drying cabinet 80 DEG C and be dried, final obtain hydrochloric Acid Modification Herba Typhae charcoal.
Embodiment
A3
。
(1) by hay grass natural air drying so that it is inner aqueous rate is less than 10%, 100 mesh sieve after then pulverizer is pulverized, are crossed, it is thus achieved that hay grass meal end.
(2) weighing step (1) described hay grass meal end, be placed in box atmosphere furnace, be passed through nitrogen in stove, in stove, nitrogen flow rate is 400 mL/min, and programmed rate controls 10 DEG C/min, and target temperature is 700 DEG C；At 700 DEG C, final temperature pyrolysis continues 20 min.After pyrolytic process terminates, obtain hay grass charcoal.
(3) hay grass charcoal deionized water is cleaned repeatedly 80 DEG C of drying in air drying cabinet to neutrality.
(4) weighing step (3) 10 g hay grass charcoal, be immersed in the hydrochloric acid of 200 mL, stir 2 h by blender, stir speed (S.S.) is 200 rpm.
(5) step (4) gained mixture is put in reactor, place in immersion hay grass solution instrument and be modified 24 h.
(6) take out through the modified phragmites communis charcoal of hay grass, after repeatedly rinsing with deionized water, put in air drying cabinet 80 DEG C and be dried.Final acquisition hydrochloric Acid Modification hay grass charcoal.
The foregoing is only the preferred embodiments of the present invention, be not limited to the present invention, for a person skilled in the art, the present invention can have various modifications and variations.All within the spirit and principles in the present invention, any modification, equivalent substitution and improvement etc. made, should be included within the scope of the present invention.
Claims (6)
1. utilize the method that water plant garbage and hydrochloric acid prepare modification biological charcoal, it is characterised in that implement as follows:
(1) by water plant natural air drying so that it is inner aqueous rate is less than 10%, then pulverizes 100 mesh sieve, it is thus achieved that water plant powder；
(2) weigh step (1) described water plant powder, be placed in box atmosphere furnace, be passed through nitrogen；Temperature programming, to target temperature, keeps final temperature pyrolysis；After pyrolytic process terminates, obtain water plant charcoal；
(3) step (2) described water plant charcoal deionized water is cleaned repeatedly to neutrality, 80 DEG C of drying in air drying cabinet；
(4) weigh the described a certain amount of water plant charcoal of step (3), be immersed in hydrochloric acid, stirring；
(5) step (4) gained mixture is put in reactor, be modified through microwave dissolver；
(6) take out step (5) the described water plant charcoal through hydrochloric Acid Modification, after repeatedly rinsing with deionized water, put to air drying cabinet 80 DEG C and be dried, obtain purpose product modification charcoal.
The method utilizing water plant garbage and hydrochloric acid to prepare modification biological charcoal the most according to claim 1, it is characterised in that: described water plant is the one in phragmites communis, Herba Typhae or hay grass.
The method utilizing water plant garbage and hydrochloric acid to prepare modification biological charcoal the most according to claim 2, it is characterised in that: in described step (2), in stove, nitrogen flow rate is 400 mL/min；Programmed rate controls 10 DEG C/min；Target temperature is 700 DEG C；At 700 DEG C, final temperature pyrolysis continues 20 min.
The method utilizing water plant garbage and hydrochloric acid to prepare modification biological charcoal the most according to claim 3, it is characterised in that: in described step (4), water plant charcoal is 1:20 with the mass volume ratio of hydrochloric acid；Wherein the mass unit of water plant charcoal is gram, and the unit of hydrochloric acid is milliliter.
The method utilizing water plant garbage and hydrochloric acid to prepare modification biological charcoal the most according to claim 4, it is characterised in that: described step is stirred by agitator in (4), and mixing time is 2 h, and stir speed (S.S.) is 200 rpm.
The method utilizing water plant garbage and hydrochloric acid to prepare modification biological charcoal the most according to claim 5, it is characterised in that: in described step (5), in microwave dissolver, modification time is 24
h。
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| Application Number | Priority Date | Filing Date | Title |
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| CN201610274484.8A CN105854800A (en) | 2016-04-28 | 2016-04-28 | Method for preparing modified charcoal by utilizing aquatic plant wastes and hydrochloric acid |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111661943A (en) * | 2020-06-11 | 2020-09-15 | 浙江恒美环保科技有限公司 | Comprehensive utilization method of biogas slurry |
| CN111701566A (en) * | 2020-06-30 | 2020-09-25 | 广东工业大学 | Adsorbent and preparation method and application thereof |
| CN112588262A (en) * | 2020-11-24 | 2021-04-02 | 河南永泽环境科技有限公司 | Preparation method of modified biochar for removing nitrogen and phosphorus in water |
| CN113336217A (en) * | 2021-06-29 | 2021-09-03 | 上海市园林设计研究总院有限公司 | Method for recycling wetland aquatic plants |
| CN114940564A (en) * | 2022-05-31 | 2022-08-26 | 太原理工大学 | Method for controlling nitrogen release in landscape water body sediment by coupling iron-type autotrophic denitrification with biochar |
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Cited By (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111661943A (en) * | 2020-06-11 | 2020-09-15 | 浙江恒美环保科技有限公司 | Comprehensive utilization method of biogas slurry |
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| CN111701566A (en) * | 2020-06-30 | 2020-09-25 | 广东工业大学 | Adsorbent and preparation method and application thereof |
| CN111701566B (en) * | 2020-06-30 | 2022-07-12 | 广东工业大学 | Adsorbent and preparation method and application thereof |
| CN112588262A (en) * | 2020-11-24 | 2021-04-02 | 河南永泽环境科技有限公司 | Preparation method of modified biochar for removing nitrogen and phosphorus in water |
| CN113336217A (en) * | 2021-06-29 | 2021-09-03 | 上海市园林设计研究总院有限公司 | Method for recycling wetland aquatic plants |
| CN114940564A (en) * | 2022-05-31 | 2022-08-26 | 太原理工大学 | Method for controlling nitrogen release in landscape water body sediment by coupling iron-type autotrophic denitrification with biochar |
| CN114940564B (en) * | 2022-05-31 | 2023-12-22 | 太原理工大学 | Method for controlling release of nitrogen in bottom mud of landscape water body by coupling iron-type autotrophic denitrification with biochar |
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