CN107913670A - A kind of water body lock phosphorus agent and preparation method thereof - Google Patents
A kind of water body lock phosphorus agent and preparation method thereof Download PDFInfo
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- CN107913670A CN107913670A CN201711349151.8A CN201711349151A CN107913670A CN 107913670 A CN107913670 A CN 107913670A CN 201711349151 A CN201711349151 A CN 201711349151A CN 107913670 A CN107913670 A CN 107913670A
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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
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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
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/3078—Thermal treatment, e.g. calcining or pyrolizing
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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
- B01J20/30—Processes for preparing, regenerating, or reactivating
- B01J20/3085—Chemical treatments not covered by groups B01J20/3007 - B01J20/3078
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- 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
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- 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
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J2220/00—Aspects relating to sorbent materials
- B01J2220/40—Aspects relating to the composition of sorbent or filter aid materials
- B01J2220/48—Sorbents characterised by the starting material used for their preparation
- B01J2220/4875—Sorbents characterised by the starting material used for their preparation the starting material being a waste, residue or of undefined composition
- B01J2220/4881—Residues from shells, e.g. eggshells, mollusk shells
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- 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
- C02F2101/105—Phosphorus compounds
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- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
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- Life Sciences & Earth Sciences (AREA)
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- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
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- Physics & Mathematics (AREA)
- Inorganic Chemistry (AREA)
- Solid-Sorbent Or Filter-Aiding Compositions (AREA)
- Water Treatment By Sorption (AREA)
Abstract
The invention discloses a kind of water body lock phosphorus agent and preparation method thereof, water body lock phosphorus agent includes modified oyster shell whiting；Modified oyster shell whiting is modified by oyster shell whiting for raw material through limiting oxygen heating charing, then through ferric chloride solution, adds lye to flocculent deposit is produced, and is then removed liquid drying and is made.Have the beneficial effect that：The oyster shell whiting charcoal physics and chemical adsorption capacity that the present invention is prepared are strong, the avtive spot quantity on surface is more, chelatropic reaction occurs with the P elements in water body, generate the extremely low chelate precipitation of solubility, and then be deposited in deposit surface and form " active coating ", Phosphorus-release From The Sediment passage is blocked to achieve the purpose that phosphorus is consolidated in dephosphorization.
Description
Technical field
The present invention relates to water treatment technical field, is specifically a kind of water body lock phosphorus agent and preparation method thereof.
Background technology
Phosphorus is a kind of essential element of plant growth, among the necessary element such as C, N, P, K, needed for plant growth
P content is minimum so determining the upper limit of water plant.P take part in a variety of physiological and biochemical procedures in plant, can promote to plant
The growth and development of thing, promote respiration, the synthesis for promoting carbohydrate etc. and transport, improve crop anti-adversity, so that water
Overpreading when middle algae encounters the phosphorus largely discharged, produces wawter bloom phenomenon.The outburst of algae reduces the transparency of water, hinders
The photosynthesis of aquatic macrophyte, causes the extinction of macrophyte, so that algae substitutes macrophyte, at this moment water body is changed into
" muddy state body ".Meanwhile the rapid growth of algae makes dissolved oxygen in water decline bed mud under the action of anaerobe that hair occur
The smelly extreme phenomenon of dark hair.The lock phosphorus technology of present China most extensive utilization is mainly chemistry lock phosphorus, and the principle of chemistry lock phosphorus is just
It is that lock phosphorus agent is added into eutrophication water, the phosphorus containg substances such as the phosphate of lock phosphorus agent in water body combine generation precipitation and reach
Lock the purpose of phosphorus.And often efficiency is too low, pH to water body has certain requirement for traditional chemistry lock phosphorus agent, new lock is found
Phosphorus agent is present research hotspot.
The content of the invention
It is strong it is an object of the present invention to providing a kind of physics and chemical adsorption capacity, can be with the P elements hair in water body
Raw chelatropic reaction, the extremely low chelate precipitation of generation solubility, achievees the purpose that the water body lock phosphorus agent of phosphorus is consolidated in dephosphorization.
The second object of the present invention is to provide that a kind of preparation method is simple, and cost of material is low, the water body lock of favorable reproducibility
The preparation method of phosphorus agent.
The present invention is directed to the problem of being mentioned in background technology, and the technical solution taken is：
A kind of water body locks phosphorus agent, including modified oyster shell whiting；Modified oyster shell whiting is carbonized by oyster shell whiting for raw material through limiting oxygen heating, then is passed through
Ferric chloride solution is modified, and adds lye to flocculent deposit is produced, and is then removed liquid drying and is made.
A kind of preparation method of water body lock phosphorus agent, comprises the following steps：
1）Pretreatment：Shellfish material is dipped in 8 ~ 12h of immersion treatment in sodium hydroxide solution, is taken out, in being washed with distilled water to
Property, pulverize to obtain oyster shell whiting after dry；
2）Limit oxygen heating charing：Oyster shell whiting is roasted under limited oxygen condition, is placed under dry environment and cools down after roasting
To oyster shell whiting charcoal；
3）Iron chloride is modified：By oyster shell whiting charcoal and ferric chloride solution according to mass ratio 4 ~ 7:1 mixing, mixes complete back and stirs
The NaOH solution of 0.5 ~ 2.0mol/L of side dropwise addition is mixed to there is flocculent deposit, liquid is then removed, is dried under the conditions of 65 ~ 80 DEG C
Lock phosphorus agent is prepared.Before modified, the surfacing of oyster shell whiting charcoal, glossiness are more uniform, and pore structure enriches, and surrounding is distributed
A small amount of ash impurities.It is modified, oyster shell whiting charcoal surface roughness increase, glossiness reduce, have part hole be capped but
Hole collapse phenomenon unobvious, hole inner wall adhere to the cotton-shaped particle of a small amount of group, these particles arrange scattered, unordered and part
It is overlapping.The avtive spot quantity increase of oyster shell whiting biology carbon surface, occurs chelatropic reaction, generation dissolving with the P elements in water body
Spend extremely low chelate precipitation, and then be deposited in deposit surface and form " active coating ", block Phosphorus-release From The Sediment passage with
Achieve the purpose that phosphorus is consolidated in dephosphorization.
Calcination temperature, which becomes, to be turned to：100 ~ 120 DEG C of 5 ~ 10min of calcining；200 ~ 220 DEG C of 10 ~ 15min of calcining；400 ~ 420 DEG C are forged
Burn 10 ~ 15min；600 ~ 620 DEG C of 100 ~ 120min of calcining；400 ~ 420 DEG C of 40 ~ 50min of calcining；200 ~ 220 DEG C of calcinings 20 ~
30min；100 ~ 120 DEG C of 30 ~ 40min of calcining.Oyster shell whiting is roasted using above-mentioned calcination temperature, obtained oyster shell whiting charcoal has
Larger central hole structure, huge surface area and complexity and the pore structure of prosperity, there is very strong physical absorption and chemisorbed
Function, P elements that can be in quick adsorption water.
To optimize above-mentioned technical proposal, the measure taken further includes：Before high-temperature roasting, in oyster shell whiting add 0.1 ~
0.4% silicates material and 0.0002 ~ 0.0007% aniline -2,4- disulfonic acid, high-temperature roasting, roasting terminate after dry ring
It is cooled to room temperature in border, obtains oyster shell whiting charcoal.Calcination temperature, which becomes, to be turned to：100 DEG C of calcining 10min；200 DEG C of calcining 15min；
400 DEG C of calcining 12min；600 DEG C of calcining 110min；400 DEG C of calcining 50min；200 DEG C of calcining 20min；100 DEG C of calcining 30min.
The addition of silicates material and aniline -2,4- disulfonic acid can improve the porosity of oyster shell whiting, improve physics and the change of oyster shell whiting
Adsorption capacity is learned, is improved.Aniline -2,4- disulfonic acids pyrolytic and oyster shell whiting surface is changed in high-temperature calcination process
Property, silicates material is closely adhered on oyster shell whiting pore surface, and then improves the physics and chemical adsorption capacity of oyster shell whiting.
And the chelating precipitation thing of generation is chelated, can not be absorbed by plants, after being settled down to water bottom, one is formed in water bottom
Layer " coating ", to adsorb and chelate the soluble phosphate from water bottom release, so as to prevent the release of sediment phosphorus.Adopt
The water body of the 0 ~ 10mg/L of lock phosphorus agent processing phosphorus content prepared in aforementioned manners, tp removal rate are up to more than 99%.
Compared with prior art, the advantage of the invention is that：The oyster shell whiting charcoal physics and change that the present invention is prepared
Adsorption capacity is strong, and the avtive spot quantity on surface is more, chelatropic reaction occurs with the P elements in water body, generation solubility is extremely low
Chelate precipitation, and then be deposited in deposit surface formed " active coating ", block Phosphorus-release From The Sediment passage removed with reaching
Phosphorus consolidates the purpose of phosphorus.
Embodiment
The present invention program is described further below by embodiment：
Embodiment 1：
A kind of preparation method of water body lock phosphorus agent, comprises the following steps：
1）Pretreatment：Shellfish material is dipped in immersion treatment 10h in sodium hydroxide solution, takes out, is washed with distilled water to neutrality,
Pulverize to obtain oyster shell whiting after drying；
2）Limit oxygen heating charing：The high-temperature roasting under limited oxygen condition, roasting terminate after being cooled to room temperature in dry environment, obtain
Oyster shell whiting charcoal.Calcination temperature, which becomes, to be turned to：100 DEG C of calcining 10min；200 DEG C of calcining 15min；400 DEG C of calcining 12min；600
DEG C calcining 110min；400 DEG C of calcining 50min；200 DEG C of calcining 20min；100 DEG C of calcining 30min；
3）Iron chloride is modified：By oyster shell whiting charcoal and ferric chloride solution according to mass ratio 5:1 mixing, mixes complete back stirring
The NaOH solution of 1.0mol/L is added dropwise to there is flocculent deposit in side, then removes liquid, dries and be prepared under the conditions of 70 DEG C
Lock phosphorus agent.
Embodiment 2：
A kind of preparation method of water body lock phosphorus agent, comprises the following steps：
1）Pretreatment：Shellfish material is dipped in immersion treatment 10h in sodium hydroxide solution, takes out, is washed with distilled water to neutrality,
Pulverize to obtain oyster shell whiting after drying；
2）Limit oxygen heating charing：0.3% silicates material and 0.0006% aniline -2,4- disulfonic acid is added in oyster shell whiting,
The high-temperature roasting under limited oxygen condition, roasting terminate after being cooled to room temperature in dry environment, obtain oyster shell whiting charcoal.Roasting temperature
Degree change turns to：100 DEG C of calcining 10min；200 DEG C of calcining 15min；400 DEG C of calcining 12min；600 DEG C of calcining 110min；400 DEG C are forged
Burn 50min；200 DEG C of calcining 20min；100 DEG C of calcining 30min；
3）Iron chloride is modified：By oyster shell whiting charcoal and ferric chloride solution according to mass ratio 5:1 mixing, mixes complete back stirring
The NaOH solution of 1.0mol/L is added dropwise to there is flocculent deposit in side, then removes liquid, dries and be prepared under the conditions of 70 DEG C
Lock phosphorus agent.
Embodiment 3：
A kind of preparation method of water body lock phosphorus agent, comprises the following steps：
1）Pretreatment：Shellfish material is dipped in immersion treatment 12h in sodium hydroxide solution, takes out, is washed with distilled water to neutrality,
Pulverize to obtain oyster shell whiting after drying；
2）Limit oxygen heating charing：0.2% silicates material and 0.0005% aniline -2,4- disulfonic acid is added in oyster shell whiting,
The high-temperature roasting under limited oxygen condition, roasting terminate after being cooled to room temperature in dry environment, obtain oyster shell whiting charcoal.Roasting temperature
Degree change turns to：100 DEG C of calcining 10min；200 DEG C of calcining 15min；400 DEG C of calcining 12min；600 DEG C of calcining 110min；400 DEG C are forged
Burn 50min；200 DEG C of calcining 20min；100 DEG C of calcining 30min；
3）Iron chloride is modified：By oyster shell whiting charcoal and ferric chloride solution according to mass ratio 5:1 mixing, mixes complete back stirring
The NaOH solution of 1.0mol/L is added dropwise to there is flocculent deposit in side, then removes liquid, dries and be prepared under the conditions of 70 DEG C
Lock phosphorus agent.
Embodiment 4：
With reference to national standard《The measure ammonium molybdate spectrophotometric method of water quality total phosphorus》（GB/T 11893-1989）, measure use
Total phosphorus content in sewage, measurement result are as shown in table 1 before and after the processing for lock phosphorus agent prepared by embodiment 1,2 and 3：
Table 1
| Before processing total phosphorus in water content/mg/L | Before processing total phosphorus in water content/mg/L | Dephosphorizing rate/% | |
| Embodiment 1 | 8.0 | 0.33 | 96.86 |
| Embodiment 2 | 8.0 | 0.02 | 99.75 |
| Embodiment 3 | 8.0 | 0.05 | 99.38 |
As shown in Table 1 the present invention prepare water body lock phosphorus agent lock phosphorus excellent effect, particularly " before high-temperature roasting add 0.1 ~
0.4% silicates material and 0.0002 ~ 0.0007% aniline -2,4- disulfonic acid, high-temperature roasting, roasting terminate after dry ring
It is cooled to room temperature in border, obtains oyster shell whiting charcoal.Calcination temperature, which becomes, to be turned to：100 DEG C of calcining 10min；200 DEG C of calcining 15min；
400 DEG C of calcining 12min；600 DEG C of calcining 110min；400 DEG C of calcining 50min；200 DEG C of calcining 20min；100 DEG C of calcining 30min.”
Under conditions of the lock phosphorus agent for preparing, lock phosphorus effect is preferable, has preferable market prospects.
Routine operation in the operating procedure of the present invention is well known to those skilled in the art, herein without repeating.
Technical scheme is described in detail in embodiment described above, it should be understood that the above is only
For the specific embodiment of the present invention, it is not intended to limit the invention, all any modifications made in the spirit of the present invention,
Supplement or similar fashion replacement etc., should all be included in the protection scope of the present invention.
Claims (6)
1. a kind of water body locks phosphorus agent, it is characterised in that including modified oyster shell whiting；The modified oyster shell whiting is passed through by oyster shell whiting for raw material
Oxygen heating charing is limited, then is modified through ferric chloride solution, adds lye to flocculent deposit is produced, liquid drying is then removed and is made.
A kind of 2. preparation method of water body lock phosphorus agent, it is characterised in that following steps：
1）Pretreatment：Shellfish material is dipped in 8 ~ 12h of immersion treatment in sodium hydroxide solution, is taken out, in being washed with distilled water to
Property, pulverize to obtain oyster shell whiting after dry；
2）Limit oxygen heating charing：Oyster shell whiting is roasted under limited oxygen condition, is placed under dry environment and cools down after roasting
To oyster shell whiting charcoal；
3）Iron chloride is modified：Oyster shell whiting charcoal is mixed in proportion with ferric chloride solution, is added dropwise while stirring after mixing completely
Lye then removes liquid drying and lock phosphorus agent is prepared to there is flocculent deposit.
A kind of 3. preparation method of water body lock phosphorus agent according to claim 2, it is characterised in that：The calcination temperature becomes
Turn to：100 ~ 120 DEG C of 5 ~ 10min of calcining；200 ~ 220 DEG C of 10 ~ 15min of calcining；400 ~ 420 DEG C of 10 ~ 15min of calcining；600~620
DEG C calcining 100 ~ 120min；400 ~ 420 DEG C of 40 ~ 50min of calcining；200 ~ 220 DEG C of 20 ~ 30min of calcining；100 ~ 120 DEG C of calcinings 30 ~
40min。
A kind of 4. preparation method of water body lock phosphorus agent according to claim 2, it is characterised in that：The oyster shell whiting biology
Charcoal is with ferric chloride solution according to mass ratio 4 ~ 7:1 mixing.
A kind of 5. preparation method of water body lock phosphorus agent according to claim 2, it is characterised in that：The iron chloride is modified
In lye be 0.5 ~ 2.0mol/L NaOH solution.
A kind of 6. preparation method of water body lock phosphorus agent according to claim 2, it is characterised in that：The iron chloride is modified
In obtained flocculent deposit dried under the conditions of 65 ~ 80 DEG C.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711349151.8A CN107913670B (en) | 2017-12-15 | 2017-12-15 | Water phosphorus-locking agent and preparation method thereof |
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|---|---|---|---|
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108911086A (en) * | 2018-08-21 | 2018-11-30 | 上海景青绿环境科技有限公司 | A kind of hi-effect coagulation integration apparatus |
| CN110227409A (en) * | 2019-06-10 | 2019-09-13 | 华侨大学 | A kind of method of purification plant sludge preparation magnetic lock phosphorus agent |
| CN112322298A (en) * | 2020-09-28 | 2021-02-05 | 苏州智泉水处理技术有限公司 | Soil conditioner |
| CN113896260A (en) * | 2021-10-26 | 2022-01-07 | 广州市芦苇环保科技有限责任公司 | Dephosphorization polyaluminum chloride and preparation method thereof |
| CN115594527A (en) * | 2022-10-31 | 2023-01-13 | 北部湾大学（Cn） | Preparation method of biochar-loaded controllable slow-release phosphate fertilizer |
| CN116059967A (en) * | 2023-03-10 | 2023-05-05 | 山东恒智医创医疗器械科技有限公司 | Production process of biochar adsorption material |
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| JP4189492B2 (en) * | 2004-03-22 | 2008-12-03 | 独立行政法人物質・材料研究機構 | Layered double hydroxide / zeolite composite |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108911086A (en) * | 2018-08-21 | 2018-11-30 | 上海景青绿环境科技有限公司 | A kind of hi-effect coagulation integration apparatus |
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| CN115594527A (en) * | 2022-10-31 | 2023-01-13 | 北部湾大学（Cn） | Preparation method of biochar-loaded controllable slow-release phosphate fertilizer |
| CN116059967A (en) * | 2023-03-10 | 2023-05-05 | 山东恒智医创医疗器械科技有限公司 | Production process of biochar adsorption material |
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| CN107913670B (en) | 2020-04-28 |
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