CN102908998B - Preparation method of xanthate macro-pore dextrangel adsorbent - Google Patents
Preparation method of xanthate macro-pore dextrangel adsorbent Download PDFInfo
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- CN102908998B CN102908998B CN201210445733.7A CN201210445733A CN102908998B CN 102908998 B CN102908998 B CN 102908998B CN 201210445733 A CN201210445733 A CN 201210445733A CN 102908998 B CN102908998 B CN 102908998B
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Abstract
The invention discloses a preparation method of a xanthate macro-pore dextrangel adsorbent and an application thereof. The preparation method comprises the steps of 1) rapidly cooling dextrangel immersed by distilled water to obtain macro-pore dextrangel; 2) placing the macro-pore dextrangel into an NaOH solution with the concentration of 10-30% and reacting at a constant temperature in a range of 50-60 DEG C for 15-60 min to obtain alkalified macro-pore dextrangel; and 3) enabling the alkalified macro-pore dextrangel and carbon disulfide to react to obtain the xanthate macro-pore dextrangel adsorbent. The preparation method disclosed by the invention has the characteristics of simple preparation method, large specific surface area, great quantity of xanthate, and high adsorption capability of adsorbing heavy metal, and the dextrangel has the characteristics of light weight and low cost, good stability, degradability, environmental friendliness and the like; and the adsorbent disclosed by the invention is used for treating the heavy metal in wastewater and analyzing the separation and enriching effect of the heavy metal in chemistry.
Description
Technical field
The invention belongs to water-treatment technology field, particularly a kind of preparation method of xanthogen macropore sephadex adsorbent and in water treatment to heavy metal ion adsorbed application technology.
Background technology
Along with scientific and technical progress and the fast development of industrial or agricultural, people's living standard improves constantly, and global environment pollutes and increasingly sharpens, and environmental protection and environmental improvement problem are more and more received the attention of various circles of society.One of important pollution sources of contaminated environment water quality are heavy metals in industrial wastewater ions, and heavy metal wastewater thereby is mainly derived from smelting and the chemical enterprise of machining, mining, non-ferrous metal.Heavy metal pollution, compared with other pollutant, has its uniqueness.The one, there is toxic, can cause poisoning, carcinogenic etc.; The 2nd, there is duplicity, most heavy metal wastewater therebies are water white, and uncomprehending meeting is heavy metal-containing waste water as clean water, and some peasants directly irrigate, and some livestocks are directly drunk, and enrichment seriously can cause poisoning in animal body; The 3rd, there is enriching, heavy metal can pass through food chain enrichment at double, finally enters human body, can not be decomposed and drain in human body; The 4th, on administering, there is chronicity, once water body and soil are contaminated by heavy metals, difficulty of governance is large, the cycle is very long; The 5th, heavy metal ion can not be decomposed in water sweetening of the soil.Therefore, except the heavy metal ion tool in anhydrating is of great significance.The method of processing at present heavy metal wastewater thereby has chemical precipitation method, electrolysis, ion floatation method, ion-exchange, electroosmose process, solvent extraction, absorption method etc.Traditional wastewater processing technology exists that inorganic agent use amount is large mostly, price, reaction should not be controlled, reaction speed is slow, residue is not easily separated, and the use of some inorganic agent also can cause the weak points such as secondary pollution.And absorption method is easy to get because of its material, reasonable price, heavy metal after separating easily separate, and removing effective, adsorbent can Reusability, stable and be subject to Environmental Chemistry worker's favor, in water treatment field, have broad application prospects.
Sephadex is to have the cancellated macromolecular compound in porous three-dimensional space, belong to soft gel, its micropore can suck a large amount of solvents, and specific area is large, and glucan contains hydrophily, also with abundant dentate, be easy to carry out chemical modification, sephadex is made by glucose fermentation, belongs to natural polymer, can biodegradation, environmental protection is enriched in source, can Reusability.Domestic in Wang Qi superfine (analytical chemistry, 1986,14(8) in 1986,584 ~ 586) first sulfydryl is connected on sephadex and synthesizes sulfhydryl dextran gel for separation of metal ions enrichment, sulfhydryl dextran gel is to Hg
2+, Cu
2+, Ag
+, Sb
3+maximum adsorption capacity be respectively 72.2mg/g, 20.48 mg/g, 75.6 mg/g, 35.38 mg/g.
As everyone knows, xanthic acid anionic functional group, has stronger adsorption capacity to metal ion.The high-molecular organic material xanthogenation such as cellulose, starch, shitosan and application thereof have been reported, as: when insoluble starch xanthate Treatment of Copper waste water, copper absorption capacity is 31.27 mg/g; When cellulose xanthate is processed heavy metal wastewater thereby, copper absorption capacity is 1.49mg/g.Crosslinked xanthic acid shitosan is that 238.9mg/g(Wang Chong is chivalrous etc. to lead ion adsorption capacity, chemical research and application, 2012,24(2): 301 ~ 304); What be most widely used is that cotton its of xanthan ester has very strong suction-operated to various heavy and noble metal, it is all relatively good to heavy metal ion adsorbed effect for the macromolecular material of these xanthic acid esterifications, but its mechanical performance is poor, in wastewater treatment, be difficult to reclaim the shortcoming such as Reusability rate is low.Xanthic acid modified with functional group inorganic material is also had to relevant report, as: in the patent that application number is 200710018213.7, disclose a kind of xanthogenation bentone adsorbent and preparation method thereof, in this patent, provided xanthogenation bentone adsorbent the maximum adsorption capacity of Cu in waste water ion, lead ion is respectively to 39mg/g, 247mg/g; The preparation of sulfonic functional magnetic nano-particle and except anhydrating research (imperial court's brightness etc. of middle copper ion, Chemical Engineer, 2012,7:15 ~ 19), the mechanical performance of the inorganic material of xanthogenation is better than high score material, also relatively good to heavy metal ion adsorbed effect, but in waste water, be not easy to reclaim, waste discharge is easily taken away.
Sephadex fully soaks activation, freezing, alkalization, xanthic acid modification in water to be prepared xanthogen macropore sephadex and has macropore sephadex and connect more xanthic acid groups, it have advantages of the good mechanical property of inorganic material, there are again all advantages of organic material, have no at present the report of xanthogen macropore sephadex preparation method and application.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of xanthogen macropore sephadex adsorbent and apply in water treatment.
One of object of the present invention is a kind of preparation method of xanthogen macropore sephadex adsorbent, is achieved through the following technical solutions, and feature is that the method has following processing step:
(1) macropore sephadex preparation, feature is: in reactor, by distilled water immersion 24 ~ 48h for sephadex, fully wash to neutrality with distilled water, filter, be placed in-12 ~-18 DEG C of rapid freezing 20 ~ 50h, after taking out, room temperature is thawed, obtain macropore sephadex, its specific area can reach 450 ~ 700m
2/ g;
(2) alkalization macropore sephadex preparation, feature is: in reactor, macropore sephadex is pressed to 30% ~ 60% of gross mass, the sodium hydrate aqueous solution that is 10% ~ 30% by concentration dipping, stir, calorify isothermal reaction 15min ~ 60min within the scope of 50 ~ 60 DEG C, cool to room temperature, filters, washs, is dried, and macropore sephadex obtains alkalizing;
(3) xanthogen macropore sephadex preparation, feature is: in reactor, add 5 ~ 30% chloroforms, 40 ~ 65% carbon disulfide, mix, then add 20 ~ 48% alkalization macropore sephadexes, system temperature is down to 6 ~ 10 DEG C, slowly add 5% ~ 10% ethylene glycol, room temperature reaction 8 ~ 15h, before reaction finishes, 15min ~ 30min adds 2% ~ 8% calcium chloride, each constituent content sum is absolutely, suction filtration, extremely neutral with 2% ~ 5% calcium chloride solution washing, using absolute ethanol washing, dry in 60 DEG C, obtain xanthogen macropore sephadex.
The pattern of xanthogen macropore sephadex product prepared by the present invention arrives by scanning electron microscopic observation, in product, the content of xanthogen is measured by chemico-analytic method, show that xanthogen can well be connected on sephadex, and macropore sephadex to connect the quantity of xanthogen be 1.8 times of sephadexes, and there is good stability.
Another object of the present invention is to provide the application in Adsorption of Heavy Metal Ions in wastewater treatment of xanthogen macropore sephadex.Be characterized as: the xanthogen macropore sephadex adsorbent preparing directly in aqueous medium, is adsorbed by static method; The xanthogen macropore sephadex adsorbent preparing can also be made into adsorption column, by dynamic method absorption, its flow velocity be the diameter that will look adsorption column, xanthogen macropore sephadex adsorbent in post in height and processed water the content of heavy metal determine.After absorption, with hydrochloric acid, salpeter solution wash-out, get final product separation of heavy metal ions.
The invention has the beneficial effects as follows:
(1) the present invention obtains xanthogen macropore sephadex adsorbent, heavy metal ion is had to very strong adsorption capacity and ion-exchange capacity, during required heavy metal ions in wastewater is processed, adsorption capacity is large, high adsorption capacity, and processed waste water reaches national discharge standard.
(2) raw material of the present invention is sephadex, is to be prepared by glucan, biodegradable, and is regenerated resources, and this material environmental protection has good physical and chemical stability and excellent mechanical stability.
(3) xanthogen macropore sephadex preparation process of the present invention is simple, and condition is easy to control, and production cost is low.
(4) the present invention prepares xanthogen macropore sephadex adsorbent, owing to being xanthogen in the finishing of macropore sephadex, because the specific area of macropore glucan is large, the quantity of the xanthogen connecting is many, strong to heavy metal ion adsorbed ability, efficiency is high, adsorption capacity is large, its maximum adsorption capacity to copper ion, lead ion and cadmium ion is respectively 86mg/g, 302mg/g and 163mg/g, adsorption rate can reach 99%, is better than the adsorbent of various xanthogens.
(5) there is power of regeneration simultaneously, can Reusability more than 10 times, heavy metal ion easily reclaims,
Brief description of the drawings
Fig. 1 is the scanning electron microscope (SEM) photograph of xanthogen macropore sephadex.
Detailed description of the invention
Embodiment 1
(1) macropore sephadex preparation, feature is: in reactor, by sephadex distilled water immersion 40h, fully wash to neutrality with distilled water, filter, be placed in-12 DEG C of rapid freezing 48h, take out room temperature afterwards and thaw, obtain macropore sephadex;
(2) alkalization macropore sephadex preparation, feature is: in reactor, 10g NaOH is dissolved in 50mL water, sodium hydroxide solution is down to room temperature, add 20g macropore sephadex, constant temperature, stirring reaction 40min within the scope of 60 DEG C, cool to room temperature, filter, wash, be dried, macropore sephadex obtains alkalizing;
(3) xanthogen macropore sephadex preparation, feature is: in reactor, adding concentration is 60% carbon disulfide (CS
2) chloroformic solution 20mL, add 6g alkalization macropore sephadex, system temperature is down to 10 DEG C, slowly add 2mL ethylene glycol, room temperature reaction 10h, 15min before reaction finishes, under agitation add 20% calcium chloride water 5mL, suction filtration, extremely neutral with 2% calcium chloride solution washing, using absolute ethanol washing, in 60 DEG C dry, obtain xanthogen macropore sephadex, output is 6.21g.
Embodiment 2
(1) macropore sephadex preparation, feature is: in reactor, by sephadex distilled water immersion 40h, fully wash to neutrality with distilled water, filter, be placed in-18 DEG C of rapid freezing 30h, take out room temperature afterwards and thaw, obtain macropore sephadex;
(2) alkalization macropore sephadex preparation, feature is: in reactor, 12g NaOH is dissolved in 50mL water, sodium hydroxide solution is down to room temperature, add 30g macropore sephadex, constant temperature, stirring reaction 60min within the scope of 55 DEG C, cool to room temperature, filter, wash, be dried, macropore sephadex obtains alkalizing;
(3) xanthogen macropore sephadex preparation, feature is: in reactor, adding concentration is 70% carbon disulfide (CS
2) chloroformic solution 30mL, add 15g alkalization macropore sephadex, system temperature is down to 8 DEG C, slowly add 5mL ethylene glycol, room temperature reaction 15h, 30min before reaction finishes, under agitation add 20% calcium chloride water 10mL, suction filtration, extremely neutral with 2% calcium chloride solution washing, using absolute ethanol washing, in 60 DEG C dry, obtain xanthogen macropore sephadex, output is 15.8g.
Embodiment 3
(1) macropore sephadex preparation, feature is: in reactor, by sephadex distilled water immersion 48h, fully wash to neutrality with distilled water, filter, be placed in-15 DEG C of rapid freezing 40h, take out room temperature afterwards and thaw, obtain macropore sephadex;
(2) alkalization macropore sephadex preparation, feature is: in reactor, 15g NaOH is dissolved in 50mL water, sodium hydroxide solution is down to room temperature, add 35g macropore sephadex, constant temperature, stirring reaction 45min within the scope of 50 DEG C, cool to room temperature, filter, wash, be dried, macropore sephadex obtains alkalizing;
(3) xanthogen macropore sephadex preparation, feature is: in reactor, adding concentration is 80% carbon disulfide (CS
2) chloroformic solution 30mL, add 18g alkalization macropore sephadex, system temperature is down to 6 DEG C, slowly add 5mL ethylene glycol, room temperature reaction 12h, 20min before reaction finishes, under agitation add 20% calcium chloride water 10mL, suction filtration, extremely neutral with 2% calcium chloride solution washing, using absolute ethanol washing, in 60 DEG C dry, obtain xanthogen macropore sephadex, output is 18.9g.
Embodiment 4
(1) macropore sephadex preparation, feature is: in reactor, by sephadex distilled water immersion 40h, fully wash to neutrality with distilled water, filter, be placed in-15 DEG C of rapid freezing 48h, take out room temperature afterwards and thaw, obtain macropore sephadex;
(2) alkalization macropore sephadex preparation, feature is: in reactor, 17g NaOH is dissolved in 50mL water, sodium hydroxide solution is down to room temperature, add 24g macropore sephadex, constant temperature, stirring reaction 60min within the scope of 50 DEG C, cool to room temperature, filter, wash, be dried, macropore sephadex obtains alkalizing;
(3) xanthogen macropore sephadex preparation, feature is: in reactor, adding concentration is 90% carbon disulfide (CS
2) chloroformic solution 20mL, add 20g alkalization macropore sephadex, system temperature is down to 10 DEG C, slowly add 4mL ethylene glycol, room temperature reaction 10h, 15min before reaction finishes, under agitation add 20% calcium chloride water 5mL, suction filtration, extremely neutral with 2% calcium chloride solution washing, using absolute ethanol washing, in 60 DEG C dry, obtain xanthogen macropore sephadex, output is 21.10g.
Embodiment 5
(1) macropore sephadex preparation, feature is: in reactor, by sephadex distilled water immersion 48h, fully wash to neutrality with distilled water, filter, be placed in-15 DEG C of rapid freezing 48h, take out room temperature afterwards and thaw, obtain macropore sephadex;
(2) alkalization macropore sephadex preparation, feature is: in reactor, 16g NaOH is dissolved in 50mL water, sodium hydroxide solution is down to room temperature, add 25g macropore sephadex, constant temperature, stirring reaction 40min within the scope of 60 DEG C, cool to room temperature, filter, wash, be dried, macropore sephadex obtains alkalizing;
(3) xanthogen macropore sephadex preparation, feature is: in reactor, adding concentration is 85% carbon disulfide (CS
2) chloroformic solution 20mL, add 23g alkalization macropore sephadex, system temperature is down to 8 DEG C, slowly add 3mL ethylene glycol, room temperature reaction 15h, 15min before reaction finishes, under agitation add 20% calcium chloride water 10mL, suction filtration, extremely neutral with 5% calcium chloride solution washing, using absolute ethanol washing, in 60 DEG C dry, obtain xanthogen macropore sephadex, output is 24g.
Embodiment 6
Xanthogen macropore sephadex of the present invention is to containing the adsorption test of lead ion Simulated Water: select 5 kinds of prepared products of above-described embodiment as adsorbent, by following waste water treatment process, experimental result is listed table 1. in
(1) simulated wastewater 200 mL that to get containing the initial concentration of lead ion be 600mg/L;
(2) regulate pH value in 3.5 ~ 8.5 scopes;
(3) in simulated water sample, add xanthogen macropore sephadex, adsorbent consumption is 1.0g/L water sample, stirring and adsorbing 30 min under room temperature;
(4) static concentration of getting supernatant Aas Determination of Lead In China ion, calculates adsorption capacity.
The adsorption capacity of table 1 xanthogen macropore sephadex to lead ion
| Adsorbent | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Xanthogen sephadex |
| Adsorption capacity (mg/g) | 302.82 | 303.17 | 302.10 | 303.68 | 302.89 | 165.77 |
As seen from Table 1, xanthogen macropore sephadex of the present invention is to the adsorption capacity of lead ion more than 302mg/g, and xanthogen sephadex adsorption capacity is 165.77mg/g.
Embodiment 7
Xanthogen macropore sephadex of the present invention is to containing the adsorption test of cadmium ion Simulated Water: select 5 kinds of prepared products of above-described embodiment as adsorbent, press the waste water treatment process of embodiment 6, the initial concentration of cadmium ion is 350mg/L, and experimental result is listed table 2 in.
The adsorption capacity of table 2 xanthogen macropore sephadex to cadmium ion
| Adsorbent | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Xanthogen sephadex |
| Adsorption capacity (mg/g) | 163.85 | 164.12 | 163.56 | 165.12 | 163.98 | 96.12 |
As seen from Table 2, xanthogen macropore sephadex of the present invention is to the adsorption capacity of cadmium ion more than 163.56mg/g, and xanthogen sephadex adsorption capacity is 96.12mg/g.。
Embodiment 8
The adsorption test of xanthogen macropore sephadex of the present invention to copper ions Simulated Water: select 5 kinds of prepared products of above-described embodiment as adsorbent, press the waste water treatment process of embodiment 6, the initial concentration of copper ion is 200mg/L, and experimental result is listed table 3 in.
The adsorption capacity of table 3 xanthogen macropore sephadex to copper ion
| Adsorbent | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Xanthogen sephadex |
| Adsorption capacity (mg/g) | 86.21 | 87.05 | 86.56 | 87.89 | 86.67 | 48.78 |
As seen from Table 3, xanthogen macropore sephadex of the present invention is to the adsorption capacity of cadmium ion more than 86mg/g, and xanthogen sephadex adsorption capacity is 48.78mg/g.
When in wastewater sample, the content of heavy metal ion is less than the adsorption capacity of xanthogen macropore sephadex adsorbent, adsorption rate can reach 99%, is a kind of adsorbent of good Adsorption of Heavy Metal Ions; Also can be used in the separation of heavy metal ions enrichment in analytical chemistry.
Claims (4)
1. a preparation method for xanthogen macropore sephadex adsorbent, is characterized in that the method specific embodiment is as follows:
(1) macropore sephadex preparation, feature is: in reactor, by distilled water immersion 24～48h for sephadex, fully wash to neutrality with distilled water, filter, be placed in-12～-18 DEG C of rapid freezing 20～50h, after taking out, room temperature is thawed, and obtains macropore sephadex;
(2) alkalization macropore sephadex preparation, feature is: in reactor, adding mass percentage concentration is 10%～30% sodium hydrate aqueous solution, add again 30%～60% the macropore sephadex that accounts for sodium hydroxide solution gross mass, stir, calorify isothermal reaction 15min～60min within the scope of 50～60 DEG C, cool to room temperature, filters, washs, is dried, and macropore sephadex obtains alkalizing;
(3) xanthogen macropore sephadex preparation, feature is: in reactor, add 5～30% chloroforms, 40～65% carbon disulfide, mix, then add 20～48% alkalization macropore sephadexes, system temperature is down to 6～10 DEG C, slowly add 5%～10% ethylene glycol, room temperature reaction 8～15h, before reaction finishes, 15min～30min adds 2%～8% calcium chloride, each constituent content sum is absolutely, suction filtration, extremely neutral with 2%～5% calcium chloride solution washing, use again absolute ethanol washing, dry in 60 DEG C, obtain xanthogen macropore sephadex.
2. the preparation method of a kind of xanthogen macropore sephadex adsorbent according to claim 1, is characterized in that: alkalization macropore sephadex and carbon disulfide mass ratio are between 1:0.9～3.1.
3. the preparation method of a kind of xanthogen macropore sephadex adsorbent according to claim 1, is characterized in that: described sephadex is sephadex G-75 and sephadex g-100.
4. the xanthogen macropore sephadex adsorbent of preparing according to claim 1, is characterized in that: xanthogen macropore sephadex adsorbent is for heavy metal ions in wastewater separation and concentration.
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| CN104250054B (en) * | 2013-06-28 | 2015-10-21 | 桐乡市高桥皮革有限责任公司 | A kind of leather-making waste water diversion processing method |
| CN103464117B (en) * | 2013-09-26 | 2015-05-06 | 济南大学 | Preparation method of ethanediamine based porous dextrangel adsorbent |
| CN103611507A (en) * | 2013-12-16 | 2014-03-05 | 武汉纺织大学 | Polysaccharide-based gel adsorbent for dye wastewater treatment and preparation method thereof |
| CN105195099B (en) * | 2015-09-21 | 2017-06-23 | 济南大学 | A kind of preparation method of the modified macroporous GAG adsorbent of beta cyclodextrin |
| CN105561940B (en) * | 2016-02-17 | 2017-09-22 | 济南大学 | A kind of preparation of the modified porous sephadex of VTES |
| CN106064081A (en) * | 2016-06-13 | 2016-11-02 | 王金明 | A kind of preparation method of nickel plating solution detin adsorbent |
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|---|---|---|---|---|
| US2736652A (en) * | 1954-08-18 | 1956-02-28 | Ohio Commw Eng Co | Fibrous products comprising fibers bonded with dextran xanthate |
| CN1583838A (en) * | 2004-06-02 | 2005-02-23 | 武汉大学 | Preparing method for macroporous konjaku gel |
| CN101081359A (en) * | 2007-06-21 | 2007-12-05 | 西北师范大学 | Xanthation bentonite absorbingsubstance and method for preparing the same |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2736652A (en) * | 1954-08-18 | 1956-02-28 | Ohio Commw Eng Co | Fibrous products comprising fibers bonded with dextran xanthate |
| CN1583838A (en) * | 2004-06-02 | 2005-02-23 | 武汉大学 | Preparing method for macroporous konjaku gel |
| CN101081359A (en) * | 2007-06-21 | 2007-12-05 | 西北师范大学 | Xanthation bentonite absorbingsubstance and method for preparing the same |
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