CN106824111A - The method that stalk prepares heavy metal chelant - Google Patents
The method that stalk prepares heavy metal chelant Download PDFInfo
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- CN106824111A CN106824111A CN201710109529.0A CN201710109529A CN106824111A CN 106824111 A CN106824111 A CN 106824111A CN 201710109529 A CN201710109529 A CN 201710109529A CN 106824111 A CN106824111 A CN 106824111A
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- stalk
- heavy metal
- filtrate
- total amount
- metal chelant
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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
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
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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
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
-
- 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
- C02F1/286—Treatment of water, waste water, or sewage by sorption using natural organic sorbents or derivatives thereof
-
- 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
-
- 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
- C02F2101/20—Heavy metals or heavy metal compounds
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Analytical Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Engineering & Computer Science (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The present invention discloses a kind of method that stalk prepares heavy metal chelant.Comprise the following steps：Stalk pretreatment, the stalk after crushing is placed in the NaOH solution of 0.05mol/L 0.1mol/L, immersion treatment 2~3 days, and filtrate is stand-by after filtering；Adjust filtrate pH value to 11 12, and under the initiation of hydrogen peroxide or ozone, adding epoxychloropropane and ethylenediamine carries out aminating reaction, amination is carried out to the functional group in cellulose, albumen, the carbohydrate side chain of dissolving in stalk, wherein the dosage of epoxychloropropane is the 1wt% 2wt% of filtrate total amount, and the dosage of ethylenediamine is the 2wt% 4wt% of filtrate total amount；Mixed solution pH value after aminating reaction is adjusted to 10 12, carbon disulfide is slowly added under normal temperature, fully obtain heavy metal chelant after reaction；Wherein, the addition of carbon disulfide is the 0.5wt% 1wt% of mixed liquor total amount.The stalk method for preparing heavy metal chelant that the present invention is provided, the metal-chelator for preparing has multiple complexing centers, and the complex compound generated with heavy metal can leaching concentration it is low.
Description
【Technical field】
The present invention relates to metal-chelator technical field, and in particular to a kind of method that stalk prepares heavy metal chelant.
【Background technology】
Heavy metal chelant can form the chelate of stabilization with most of heavy metal ion, so as to by heavy metal ion from useless
Separated in water, or for the capture of heavy metal ion.It is at present, more to the adsorbent for heavy metal research containing S atom,
Reason is that S atom is both coordination atom, it is also possible to generate sulfide precipitation with heavy metal ion.
Dithiocar-bamate abbreviation DTC, the high adsorption capacity of heavy metal ion can apply to a huge sum of money in waste water
Category ionic adsorption, metal ion is collected and the solidification to heavy metal ion in incineration of refuse flyash in mineral.
The chelation of chelating agent and heavy metal ion, the strand of chelating agent is more long, the Stability of Metal Complexes for being generated
It is stronger, and with lower leaching concentration.For the chelating agent fixed for heavy metal, synthesis with polymer more long two
Thiocarbamate class compound, such compound requires there is multiple complexing centers simultaneously, reaches more heavy metals and consolidates
Constant volume.
In correlation technique, DTC quasi-chelate compounds are made of chemical synthesis process, with high cost, and belong to not high
Molecular compound, unit formula amount contains that complexing center is few, the complex compound generated with heavy metal can leaching concentration it is high, heavy metal from
Sub- inferior separating effect.
Therefore, it is necessary to providing a kind of new technique solves above-mentioned technical problem.
【The content of the invention】
The purpose of the present invention is to overcome above-mentioned technical problem, there is provided a kind of method that stalk prepares heavy metal chelant, system
The standby metal-chelator for obtaining has multiple complexing centers, and the complex compound generated with heavy metal can leaching concentration it is low.
The technical scheme is that：
A kind of method that stalk prepares heavy metal chelant, comprises the following steps：
Step S1：Stalk pretreatment, the stalk after crushing is placed in the NaOH solution of 0.05mol/L-0.1mol/L, leaching
Bubble treatment 2~3 days, filtrate is stand-by after filtering；
Step S2：Regulation filtrate pH value to 11-12, and under the initiation of hydrogen peroxide or ozone, add epoxychloropropane and
Ethylenediamine carries out aminating reaction, and amination is carried out to the functional group in cellulose, albumen, the carbohydrate side chain of dissolving in stalk, wherein
The dosage of epoxychloropropane is the 1wt%-2wt% of filtrate total amount, and the dosage of ethylenediamine is the 2wt%-4wt% of filtrate total amount；
Step S3：Mixed solution pH value after aminating reaction is adjusted to 10-12, carbon disulfide is slowly added under normal temperature,
Fully heavy metal chelant is obtained after reaction；Wherein, the addition of carbon disulfide is the 0.5wt%-1wt% of mixed liquor total amount.
Preferably, aminating reaction reacts 24-48 hours under normal temperature state in step S2.
Preferably, in step S3, the reaction time is more than 12 hours.
Preferably, pH adjusting agent is NaOH solution or HCl solution.
Compared with correlation technique, the stalk method for preparing heavy metal chelant that the present invention is provided, beneficial effect is：
First, with stalk as primary raw material, main component is cellulose compound in stalk, and it is organic polymer chemical combination
Thing, strand reaches thousands of to 100,000, and the chelating agent for preparing belongs to macromolecular compound class material, monomolecular substance
There are multiple complexing centers, and the heavy metal ion capacity that unit formula amount can be chelated is big.
2nd, the chelating agent and the complex compound leaching concentration of heavy metal generation are low, are more beneficial for the fixation of heavy metal ion,
Reduce the pollution of heavy metal ion.
3rd, with stalk as primary raw material, preparation method is simple, low production cost for the chelating agent；And the chela for preparing
The chelation of mixture heavy metal ion is smaller with the change influence of pH value.
【Specific embodiment】
Below will the invention will be further described by specific embodiment.
Embodiment one
A kind of method that stalk prepares heavy metal chelant, comprises the following steps：
Step S1：Stalk pretreatment, the stalk after crushing is placed in the NaOH solution of 0.05mol/L, and immersion treatment 2~
3 days, filtrate was stand-by after filtering；
Wherein, main component is cellulose compound in stalk, and it is organic high molecular compound, and strand reaches several
Thousand arrive hundreds of thousands, are degraded in alkaline environment, molecular chain length is constantly reduced, and degradation time is more long, and strand is shorter；
Step S2：Regulation filtrate pH value adds epoxychloropropane and ethylenediamine to 11-12, and under the initiation of hydrogen peroxide
Aminating reaction is carried out, all or part of amination is carried out to the functional group in cellulose, albumen, the carbohydrate side chain of dissolving in stalk,
Wherein the dosage of epoxychloropropane is the 1wt% of filtrate total amount, and the dosage of ethylenediamine is the 2wt% of filtrate total amount；
Wherein, aminating reaction condition is reaction 24-48 hour under normal temperature；
Step S3：Mixed solution pH value after aminating reaction is adjusted to 10-12, carbon disulfide is slowly added under normal temperature,
Fully reaction obtains heavy metal chelant after 12 hours；Wherein, the addition of carbon disulfide is the 0.5wt% of mixed liquor total amount；
Wherein, pH adjusting agent determines according to the acid-base property of mixed solution, and selection NaOH solution is used as alkaline conditioner,
HCl solution is used as acid regulator.
Embodiment two
A kind of method that stalk prepares heavy metal chelant, comprises the following steps：
Step S1：Stalk pretreatment, the stalk after crushing is placed in the NaOH solution of 0.1mol/L, immersion treatment 2~3
My god, filtrate is stand-by after filtering；
Step S2：Regulation filtrate pH value adds epoxychloropropane and ethylenediamine to enter to 11-12, and under the initiation of ozone
Row aminating reaction, all or part of amination is carried out to the functional group in cellulose, albumen, the carbohydrate side chain of dissolving in stalk, its
The dosage of middle epoxychloropropane is the 2wt% of filtrate total amount, and the dosage of ethylenediamine is the 3wt% of filtrate total amount；
Wherein, aminating reaction condition is reaction 24-48 hour under normal temperature；
Step S3：Mixed solution pH value after aminating reaction is adjusted to 10-12, carbon disulfide is slowly added under normal temperature,
Fully reaction obtains heavy metal chelant after 12 hours；Wherein, the addition of carbon disulfide is the 0.8wt% of mixed liquor total amount.
Embodiment three
A kind of method that stalk prepares heavy metal chelant, comprises the following steps：
Step S1：Stalk pretreatment, the stalk after crushing is placed in the NaOH solution of 0.08mol/L, and immersion treatment 2~
3 days, filtrate was stand-by after filtering；
Step S2：Regulation filtrate pH value adds epoxychloropropane and ethylenediamine to 11-12, and under the initiation of hydrogen peroxide
Aminating reaction is carried out, all or part of amination is carried out to the functional group in cellulose, albumen, the carbohydrate side chain of dissolving in stalk,
Wherein the dosage of epoxychloropropane is the 1.5wt% of filtrate total amount, and the dosage of ethylenediamine is the 4wt% of filtrate total amount；
Wherein, aminating reaction condition is reaction 24-48 hour under normal temperature；
Step S3：Mixed solution pH value after aminating reaction is adjusted to 10-12, carbon disulfide is slowly added under normal temperature,
Fully reaction obtains heavy metal chelant after 12 hours；Wherein, the addition of carbon disulfide is the 1wt% of mixed liquor total amount.
Example IV
A kind of method that stalk prepares heavy metal chelant, comprises the following steps：
Step S1：Stalk pretreatment, the stalk after crushing is placed in the NaOH solution of 0.06mol/L, and immersion treatment 2~
3 days, filtrate was stand-by after filtering；
Step S2：Regulation filtrate pH value adds epoxychloropropane and ethylenediamine to 11-12, and under the initiation of hydrogen peroxide
Aminating reaction is carried out, all or part of amination is carried out to the functional group in cellulose, albumen, the carbohydrate side chain of dissolving in stalk,
Wherein the dosage of epoxychloropropane is the 1.8wt% of filtrate total amount, and the dosage of ethylenediamine is the 2.5wt% of filtrate total amount；
Wherein, aminating reaction condition is reaction 24-48 hour under normal temperature；
Step S3：Mixed solution pH value after aminating reaction is adjusted to 10-12, carbon disulfide is slowly added under normal temperature,
Fully reaction obtains heavy metal chelant after 12 hours；Wherein, the addition of carbon disulfide is the 0.6wt% of mixed liquor total amount.
The chelating agent that the method for preparing heavy metal chelant by the stalk described in above-described embodiment is prepared is compound
Type chelating agent, it is strong to chelation of metal ion, it is particularly well-suited to the fixation of heavy metal ion, extracts.
The chelating agent that the method that stalk described in above-described embodiment prepares heavy metal chelant is prepared is applied to rubbish
In rubbish flying ash in electric power plant heavy metals immobilization, the consumption of chelating agent is that 2%-3% can make fly-ash heavy metal and leaching concentration reach life
Garbage loading embeading Environmental capacity standard (GB16889-2008) living；In same Application Example, prepared by the method for the present invention
The chelating agent solidification for obtaining is with cement solidification while when using, the consumption of chelating agent is can to work as to be reduced to 1.5%-2%.
Compared with correlation technique, the stalk method for preparing heavy metal chelant that the present invention is provided, beneficial effect is：
First, with stalk as primary raw material, main component is cellulose compound in stalk, and it is organic polymer chemical combination
Thing, strand reaches thousands of to 100,000, and the chelating agent for preparing belongs to macromolecular compound class material, monomolecular substance
There are multiple complexing centers, and the heavy metal ion capacity that unit formula amount can be chelated is big.
2nd, the chelating agent and the complex compound leaching concentration of heavy metal generation are low, are more beneficial for the fixation of heavy metal ion,
Reduce the pollution of heavy metal ion.
3rd, the stalk of the chelating agent one is primary raw material, and preparation method is simple, low production cost；And the chela for preparing
The chelation of mixture heavy metal ion is smaller with the change influence of pH value.
Above-described is only embodiments of the present invention, it should be noted here that for one of ordinary skill in the art
For, without departing from the concept of the premise of the invention, improvement can also be made, but these belong to protection model of the invention
Enclose.
Claims (4)
1. a kind of method that stalk prepares heavy metal chelant, it is characterised in that comprise the following steps：
Step S1：Stalk pretreatment, the stalk after crushing is placed in the NaOH solution of 0.05mol/L-0.1mol/L, at immersion
Reason 2~3 days, filtrate is stand-by after filtering；
Step S2：Regulation filtrate pH value adds epoxychloropropane and second two to 11-12, and under the initiation of hydrogen peroxide or ozone
Amine carries out aminating reaction, and amination, wherein epoxy are carried out to the functional group in cellulose, albumen, the carbohydrate side chain of dissolving in stalk
The dosage of chloropropane is the 1wt%-2wt% of filtrate total amount, and the dosage of ethylenediamine is the 2wt%-4wt% of filtrate total amount；
Step S3：Mixed solution pH value after aminating reaction is adjusted to 10-12, carbon disulfide is slowly added under normal temperature, fully
Heavy metal chelant is obtained after reaction；Wherein, the addition of carbon disulfide is the 0.5wt%-1wt% of mixed liquor total amount.
2. the method that stalk according to claim 1 prepares heavy metal chelant, it is characterised in that amination is anti-in step S2
Should be reacted 24-48 hours under normal temperature state.
3. the method that stalk according to claim 1 prepares heavy metal chelant, it is characterised in that in step S3, reaction
Time is more than 12 hours.
4. the method that the stalk according to any one of claim 1-3 prepares heavy metal chelant, it is characterised in that step
In S3, pH adjusting agent is NaOH solution or HCl solution.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201710109529.0A CN106824111A (en) | 2017-02-27 | 2017-02-27 | The method that stalk prepares heavy metal chelant |
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| Application Number | Priority Date | Filing Date | Title |
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| CN201710109529.0A CN106824111A (en) | 2017-02-27 | 2017-02-27 | The method that stalk prepares heavy metal chelant |
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| CN106824111A true CN106824111A (en) | 2017-06-13 |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110124624A (en) * | 2019-05-27 | 2019-08-16 | 济南大学 | A kind of preparation method of the dithiocar-bamate adsorbent based on corn stalk fiber element |
| CN110665467A (en) * | 2018-07-03 | 2020-01-10 | 武汉纺织大学 | Preparation method of straw-based adsorbent for adsorbing anions/cations |
| CN110947366A (en) * | 2018-09-26 | 2020-04-03 | 南京林业大学 | Preparation method of adsorbent for complexing heavy metal in water |
| CN111498972A (en) * | 2020-04-27 | 2020-08-07 | 李洪 | Heavy metal polluted wastewater treatment agent and preparation method and application thereof |
| CN113019335A (en) * | 2021-03-30 | 2021-06-25 | 南昌大学 | Bifunctional modified corn straw cellulose adsorbent, control synthesis method and application |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101215250A (en) * | 2007-12-28 | 2008-07-09 | 上海电力学院 | Chelating agent containing double DTC group and preparation method thereof |
| CN103143328A (en) * | 2013-03-07 | 2013-06-12 | 西安科技大学 | Preparation method of heavy metal chelating adsorbent |
| CN103224472A (en) * | 2013-04-07 | 2013-07-31 | 许昌学院 | Preparation method of heavy metal capturing agent |
| CN104528910A (en) * | 2014-12-18 | 2015-04-22 | 淄博金鼎光电科技有限公司 | Synthetic process of heavy metal chelating agent |
-
2017
- 2017-02-27 CN CN201710109529.0A patent/CN106824111A/en not_active Withdrawn
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101215250A (en) * | 2007-12-28 | 2008-07-09 | 上海电力学院 | Chelating agent containing double DTC group and preparation method thereof |
| CN103143328A (en) * | 2013-03-07 | 2013-06-12 | 西安科技大学 | Preparation method of heavy metal chelating adsorbent |
| CN103224472A (en) * | 2013-04-07 | 2013-07-31 | 许昌学院 | Preparation method of heavy metal capturing agent |
| CN104528910A (en) * | 2014-12-18 | 2015-04-22 | 淄博金鼎光电科技有限公司 | Synthetic process of heavy metal chelating agent |
Non-Patent Citations (1)
| Title |
|---|
| 周彤: "改性壳聚糖和麦秆对水体中污染物的吸附研究", 《中国优秀硕士学位论文全文数据库工程科技I辑》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110665467A (en) * | 2018-07-03 | 2020-01-10 | 武汉纺织大学 | Preparation method of straw-based adsorbent for adsorbing anions/cations |
| CN110947366A (en) * | 2018-09-26 | 2020-04-03 | 南京林业大学 | Preparation method of adsorbent for complexing heavy metal in water |
| CN110124624A (en) * | 2019-05-27 | 2019-08-16 | 济南大学 | A kind of preparation method of the dithiocar-bamate adsorbent based on corn stalk fiber element |
| CN111498972A (en) * | 2020-04-27 | 2020-08-07 | 李洪 | Heavy metal polluted wastewater treatment agent and preparation method and application thereof |
| CN113019335A (en) * | 2021-03-30 | 2021-06-25 | 南昌大学 | Bifunctional modified corn straw cellulose adsorbent, control synthesis method and application |
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