CN103464117B - Preparation method of ethanediamine based porous dextrangel adsorbent - Google Patents
Preparation method of ethanediamine based porous dextrangel adsorbent Download PDFInfo
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Abstract
The invention discloses a preparation method and an application of an ethanediamine based porous dextrangel adsorbent. The preparation method comprises the following steps: immersing the dextrangel in de-ionized water, freezing rapidly, treating by using NaOH solution; oxidizing by epoxy chloropropane to obtain epoxy porous dextrangel; then, stirring sodium carbonate, ethanediamine, absolute ethyl alcohol and epoxy porous dextrangel at the constant temperature of 60+/-2 DEG C, carrying out backflow reaction for 2-4h, cooling, washing by using de-ionized water, carrying out suction filtering until the filtrate is neutral, washing by using a small amount of ethanol, drying in vacuum, so as to obtain the ethanediamine based porous dextrangel adsorbent. The preparation method is simple, the specific area is large, the number of quadrol groups is high, the adsorbing capacity to heavy metal is high; the dextrangel has the characteristics of light weight, low cost, good stability, degradability, environment friendliness and the like; the adsorbent provided by the invention has excellent effects when used for heavy metal treatment in wastewater and heavy metal separation and enrichment in analytical chemistry.
Description
Technical field
The invention belongs to water-treatment technology field, particularly hole, a kind of ethylenediamine Quito dextrangel adsorbent preparation method and in water treatment the application technology of heavy metal ionic adsorption.
Background technology
Along with the progress of science and technology and the fast development of industrial or agricultural, the living standard of people improves constantly, and global environment pollutes and increasingly sharpens, and environmental protection and environmental improvement problem more and more receive 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 machining, mining, the smelting of non-ferrous metal and chemical enterprise.Heavy metal pollution, compared with other pollutant, has it unique.One is have toxic, can cause poisoning, carcinogenic etc.; Two is have duplicity, and most heavy metal wastewater thereby is 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; Three is have enriching, and heavy metal, by food chain enrichment at double, finally enters human body, can not be decomposed and excretion in human body; Four is have chronicity in improvement, and water body and soil are once contaminated by heavy metals, and difficulty of governance is large, and the cycle is very long; Five is that 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 current process 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 control, 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, be separated after heavy metal be easily separated, removing effective, adsorbent can Reusability, stable and be subject to the favor of Environmental Chemistry worker, has broad application prospects in water treatment field.
Sephadex has the cancellated macromolecular compound in porous three-dimensional space, belong to soft gel, its micropore can suck a large amount of solvent, and specific area is large, and glucan contains hydrophily, also with abundant dentate, be easy to carry out chemical modification, sephadex is obtained by glucose fermentation, belongs to natural polymer, can biodegradation, abundance environmental protection, can Reusability.Domestic at Wang Qi superfine (analytical chemistry, 1986,14(8) in 1986,584 ~ 586) be connected to by sulfydryl first and sephadex synthesizes Sulfhydryl dex-tran Gel be used for separation of metal ions enrichment, Sulfhydryl dex-tran 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, ethylenediamine is a kind of complexones, and heavy metal ion (as antimony, bismuth, cadmium, cobalt, copper, mercury, silver and uranium) has stronger sequestering power.The high-molecular organic material ethylenediamine modifications such as cellulose, starch, shitosan and application thereof have been reported, as: ethylenediamine modified starch GMA copolymer is to the absorption property of Pb (II), it is 0.481 mol/g to lead ion adsorption capacity, (Xie Guoren etc., Journal of Chemical Industry and Engineering, 2011,62(4): 970 ~ 975); The preparation of ethylenediamine chelating cotton cellulose and Study on adsorption properties, it is to Cu
2+, Cd
2+adsorption capacity respectively 5.15 mg/g, 4.96 mg/g, (Lian Hongfang etc., chemical industry environmental protection, 2004,24(supplementary issue): 368 ~ 370); Ethylenediamine modification of chitosan to the absorption of Cu (II), (Ge Huacai etc., Guangdong chemical industry, 21012,39(13): 181 ~ 182); Ethylenediamine material silica gel composite is to Zn
2+characterization of adsorption, (Fan Zhonglei etc., applied chemistry, 2010,27(11): 1260 ~ 1363); Ethylenediamine polymer-modified magnetic microsphere absorption Co
2+, it reaches 50.0 mg/g to the maximal absorptive capacity of cobalt ions, (Jianping, the village etc., Chemical Engineering and equipment, 2011, (9): 12 ~ 15); The preparation of ethylenediamine chelating bacteria cellulose and Adsorption of Cu thereof
2+research, it is to Cu
2+adsorption capacity be 8.68 mg/g, (Ma Bo etc., Treatment of Industrial Water, 2009,29(7): 60 ~ 62); Its heavy metal ionic adsorption effect of the macromolecular material of these ethylenediamine modifications is all relatively good, but its mechanical performance is poor, is difficult in the treatment of waste water reclaim, the shortcomings such as Reusability rate is low.Ethylenediamine modified with functional group inorganic material also there is is relevant report, as: hydrochloride naphthodiamide modified alta-mud is studied the absorption of crystal violet, (Ma Tongsen etc., Journal of Henan University (natural science edition), 2011,41(6): 583 ~ 587); Excellent than high score material of the mechanical performance of the inorganic material of ethylenediamine modification, but be not easy to reclaim in waste water, waste discharge is easily taken away.
Sephadex fully soaks activation, freezing, alkalization in water, ethylenediamine modification prepares hole, ethylenediamine Quito sephadex, because porous sephadex has larger specific area, so connect more ethylenediamine groups, namely it have the advantage of the good mechanical property of inorganic material, there are again all advantages of organic material, have no the report of hole, ethylenediamine Quito sephadex preparation method and application at present.
Summary of the invention
The object of the present invention is to provide the preparation method of hole, a kind of ethylenediamine Quito dextrangel adsorbent and apply in water treatment.
An object of the present invention is the preparation method of hole, a kind of ethylenediamine Quito dextrangel adsorbent, is achieved through the following technical solutions, and feature is that the method has following processing step:
(1) prepared by the porous sephadex that alkalizes, feature is: in the reactor, by sephadex distilled water immersion 24 ~ 48h, fully wash to neutrality by deionized water, filter, be placed in-12 ~-18 DEG C of quick freeze 20 ~ 50h, thaw at RT, be 100 ~ 200g/L by it by solid-to-liquid ratio again, be the NaOH aqueous solution soaking of 2.0 ~ 3.5mol/L by molar concentration, stir, calorify isothermal reaction 2 ~ 4 h within the scope of 50 ~ 60 DEG C, cool to room temperature, spend deionized water to neutral, filtration, drying, obtain alkalization porous sephadex; Its specific area can reach 450 ~ 700m
2/ g;
(2) epoxidation porous sephadex preparation, feature is: in the reactor, adds, water: 45 ~ 70%, NaOH:4 ~ 10% by following composition mass percent, after dissolving, cool to room temperature, then add epoxychloropropane: 6 ~ 14%; Absolute ethyl alcohol: 16 ~ 25%, alkalization porous sephadex: 2 ~ 10%, each component sum is absolutely, in 50 ± 2 DEG C of constant temperature, stirring, back flow reaction 4 ~ 8 h, after cooling, spend deionized water, suction filtration, to filtrate is neutrality, after a small amount of ethanol washing, be placed in 70 ± 5 DEG C of vacuum drying chambers dry, obtain epoxidation porous sephadex, wherein the volume ratio of epoxychloropropane and absolute ethyl alcohol is 1:2 ~ 3;
(3) hole, ethylenediamine Quito sephadex preparation, feature is: in the reactor, and add by following composition mass percent, water: 52 ~ 82%, sodium carbonate: 1.0 ~ 6.0%, after dissolving, then adds ethylenediamine: 6 ~ 16%; Absolute ethyl alcohol: 6 ~ 15%, epoxidation porous sephadex: 1.5 ~ 10%, each component sum is absolutely, in 60 ± 2 DEG C of constant temperature, stirring, back flow reaction 2 ~ 4 h, after cooling, spend deionized water, suction filtration, to filtrate is neutrality, after a small amount of ethanol washing, be placed in 70 ± 5 DEG C of vacuum drying chambers dry, obtain hole, ethylenediamine Quito sephadex, wherein the volume ratio of ethylenediamine and absolute ethyl alcohol is 1:0.8 ~ 2.
Hole, ethylenediamine Quito sephadex prepared by the present invention, in product, the content of ethylenediamine base is measured by chemico-analytic method, show that ethylenediamine base can well be connected on sephadex, and the quantity of porous sephadex connection ethylenediamine base is sephadex 2 times, and there is good stability.
Another object of the present invention is to provide the application of hole, ethylenediamine Quito sephadex in the treatment of waste water in Adsorption of Heavy Metal Ions.Be characterized as: hole, the ethylenediamine Quito dextrangel adsorbent deionized water prepared is soaked 2 ~ 4h, directly in aqueous medium, adsorbs by static method; Hole, the ethylenediamine Quito dextrangel adsorbent prepared can also be made into adsorption column, by dynamic method absorption, its flow velocity be will depending on the diameter of adsorption column, hole, ethylenediamine Quito dextrangel adsorbent in post in height and processed water the content of heavy metal determine.Adsorb rear 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 prepares hole, ethylenediamine Quito dextrangel adsorbent, owing to being ethylenediamine base in the finishing of porous sephadex, because the specific area of porous glucan is large, the quantity of the ethylenediamine base connected is many, heavy metal ion adsorption capacity is strong, efficiency is high, adsorption capacity is large, and it is to Cu
2+, Cd
2+, Pb
2+maximum adsorption capacity be respectively 115.8mg/g, 208.9mg/g, 316.2mg/g, adsorption rate can reach 98%, is better than the adsorbent of various ethylenediamine base, processed waste water reach country discharge standard.
(2) raw material of the present invention is sephadex, is to be prepared by glucan, biodegradable, and is regenerated resources, this material environmental protection, has good physical and chemical stability and excellent mechanical stability.
(3) hole, ethylenediamine Quito of the present invention sephadex preparation process is simple, and condition is easy to control, and production cost is low, has power of regeneration simultaneously, can Reusability more than 10 times, and heavy metal ion easily reclaims.
Detailed description of the invention
Embodiment 1
(1) prepared by the porous sephadex that alkalizes, feature is: in the reactor, sephadex is used distilled water immersion 30h, fully wash to neutrality by deionized water, filter, be placed in-15 DEG C of quick freeze 30h, thaw at RT, the sephadex 10g thawed 20, by the NaOH aqueous solution soaking of 100mL 2.5 mol/L, stirs, calorifies 55 DEG C of isothermal reaction 3h, cool to room temperature, spend deionized water to neutral, filtration, drying, obtain alkalization porous sephadex;
(2) epoxidation porous sephadex preparation, feature is: in the reactor, adds respectively, water: 54mL, NaOH:6g, after dissolving, cool to room temperature, then add epoxychloropropane: 10mL; Absolute ethyl alcohol: 20mL, alkalization porous sephadex: 10g, stir, in 50 ± 2 DEG C of constant temperature, back flow reaction 5 h, after cooling, spend deionized water, suction filtration, to filtrate is neutrality, after a small amount of ethanol washing, be placed in 70 ± 5 DEG C of vacuum drying chambers dry, obtain epoxidation porous sephadex;
(3) hole, ethylenediamine Quito sephadex preparation, feature is: in the reactor, adds water: 70mL, sodium carbonate: 2g, after dissolving, then adds ethylenediamine: 10mL; Absolute ethyl alcohol: 12mL, epoxidation porous sephadex: 6g, in 60 ± 2 DEG C of constant temperature, stirring, back flow reaction 3h, after cooling, spend deionized water, suction filtration, to filtrate is neutrality, after a small amount of ethanol washing, be placed in 70 ± 5 DEG C of vacuum drying chambers dry, obtain hole, ethylenediamine Quito sephadex.
Embodiment 2
(1) prepared by the porous sephadex that alkalizes, feature is: in the reactor, sephadex is used distilled water immersion 48h, fully wash to neutrality by deionized water, filter, be placed in-18 DEG C of quick freeze 20h, thaw at RT, by the sephadex 20g after thawing, by the NaOH aqueous solution soaking of 100mL3.0 mol/L, stir, calorify 50 DEG C of isothermal reaction 2h, cool to room temperature, spend deionized water to neutral, filtration, drying, obtain alkalization porous sephadex;
(2) epoxidation porous sephadex preparation, feature is: in the reactor, adds respectively, water: 47mL, NaOH:10g, after dissolving, cool to room temperature, then add epoxychloropropane: 14mL; Absolute ethyl alcohol: 25mL, alkalization porous sephadex: 4g, stir, in 50 ± 2 DEG C of constant temperature, back flow reaction 4 h, after cooling, spend deionized water, suction filtration, to filtrate is neutrality, after a small amount of ethanol washing, be placed in 70 ± 5 DEG C of vacuum drying chambers dry, obtain epoxidation porous sephadex;
(3) hole, ethylenediamine Quito sephadex preparation, feature is: in the reactor, adds water: 57mL, sodium carbonate: 5g, after dissolving, then adds ethylenediamine: 16mL; Absolute ethyl alcohol: 14mL, epoxidation porous sephadex: 8g, in 60 ± 2 DEG C of constant temperature, stirring, back flow reaction 2h, after cooling, spend deionized water, suction filtration, to filtrate is neutrality, after a small amount of ethanol washing, be placed in 70 ± 5 DEG C of vacuum drying chambers dry, obtain hole, ethylenediamine Quito sephadex.
Embodiment 3
(1) prepared by the porous sephadex that alkalizes, feature is: in the reactor, sephadex is used distilled water immersion 24h, fully wash to neutrality by deionized water, filter, be placed in-12 DEG C of quick freeze 50h, thaw at RT, by the sephadex 25g after thawing, by the NaOH aqueous solution soaking of 100mL2.0mol/L, stir, calorify 60 DEG C of isothermal reaction 4h, cool to room temperature, spend deionized water to neutral, filtration, drying, obtain alkalization porous sephadex;
(2) epoxidation porous sephadex preparation, feature is: in the reactor, adds respectively, water: 64mL, NaOH:4g, after dissolving, cool to room temperature, then add epoxychloropropane: 6mL; Absolute ethyl alcohol: 16mL, alkalization porous sephadex: 10g, stir, in 50 ± 2 DEG C of constant temperature, back flow reaction 8h, after cooling, spend deionized water, suction filtration, to filtrate is neutrality, after a small amount of ethanol washing, be placed in 70 ± 5 DEG C of vacuum drying chambers dry, obtain epoxidation porous sephadex;
(3) hole, ethylenediamine Quito sephadex preparation, feature is: in the reactor, adds water: 75mL, sodium carbonate: 4g, after dissolving, then adds ethylenediamine: 6mL; Absolute ethyl alcohol: 10mL, epoxidation porous sephadex: 5g, in 60 ± 2 DEG C of constant temperature, stirring, back flow reaction 2h, after cooling, spend deionized water, suction filtration, to filtrate is neutrality, after a small amount of ethanol washing, be placed in 70 ± 5 DEG C of vacuum drying chambers dry, obtain hole, ethylenediamine Quito sephadex.
Embodiment 4
(1) prepared by the porous sephadex that alkalizes, feature is: in the reactor, sephadex is used distilled water immersion 36h, fully wash to neutrality by deionized water, filter, be placed in-15 DEG C of quick freeze 40h, thaw at RT, by the sephadex 20g after thawing, by the NaOH aqueous solution soaking of 200mL2.5 mol/L, stir, calorify 50 DEG C of isothermal reaction 2h, cool to room temperature, spend deionized water to neutral, filtration, drying, obtain alkalization porous sephadex;
(2) epoxidation porous sephadex preparation, feature is: in the reactor, adds respectively, water: 60mL, NaOH:8g, after dissolving, cool to room temperature, then add epoxychloropropane: 8mL; Absolute ethyl alcohol: 22mL, alkalization porous sephadex: 2g, stir, in 50 ± 2 DEG C of constant temperature, back flow reaction 6 h, after cooling, spend deionized water, suction filtration, to filtrate is neutrality, after a small amount of ethanol washing, be placed in 70 ± 5 DEG C of vacuum drying chambers dry, obtain epoxidation porous sephadex;
(3) hole, ethylenediamine Quito sephadex preparation, feature is: in the reactor, adds water: 80mL, sodium carbonate: 1g, after dissolving, then adds ethylenediamine: 8mL; Absolute ethyl alcohol: 7mL, epoxidation porous sephadex: 4g, in 60 ± 2 DEG C of constant temperature, stirring, back flow reaction 3h, after cooling, spend deionized water, suction filtration, to filtrate is neutrality, after a small amount of ethanol washing, be placed in 70 ± 5 DEG C of vacuum drying chambers dry, obtain hole, ethylenediamine Quito sephadex.
Embodiment 5
(1) prepared by the porous sephadex that alkalizes, feature is: in the reactor, sephadex is used distilled water immersion 48h, fully wash to neutrality by deionized water, filter, be placed in-18 DEG C of quick freeze 20h, thaw at RT, by the sephadex 20g after thawing, by the NaOH aqueous solution soaking of 100mL3.0 mol/L, stir, calorify 50 DEG C of isothermal reaction 2h, cool to room temperature, spend deionized water to neutral, filtration, drying, obtain alkalization porous sephadex;
(2) epoxidation porous sephadex preparation, feature is: in the reactor, adds respectively, water: 94mL, NaOH:20g, after dissolving, cool to room temperature, then add epoxychloropropane: 28mL; Absolute ethyl alcohol: 50mL, alkalization porous sephadex: 8g, stir, in 50 ± 2 DEG C of constant temperature, back flow reaction 4 h, after cooling, spend deionized water, suction filtration, to filtrate is neutrality, after a small amount of ethanol washing, be placed in 70 ± 5 DEG C of vacuum drying chambers dry, obtain epoxidation porous sephadex;
(3) hole, ethylenediamine Quito sephadex preparation, feature is: in the reactor, adds water: 114mL, sodium carbonate: 10g, after dissolving, then adds ethylenediamine: 32mL; Absolute ethyl alcohol: 28mL, epoxidation porous sephadex: 16g, in 60 ± 2 DEG C of constant temperature, stirring, back flow reaction 2h, after cooling, spend deionized water, suction filtration, to filtrate is neutrality, after a small amount of ethanol washing, be placed in 70 ± 5 DEG C of vacuum drying chambers dry, obtain hole, ethylenediamine Quito sephadex.
Embodiment 6
(1) prepared by the porous sephadex that alkalizes, feature is: in the reactor, sephadex is used distilled water immersion 40h, fully wash to neutrality by deionized water, filter, be placed in-18 DEG C of quick freeze 36h, thaw at RT, by the sephadex 40g after thawing, by the NaOH aqueous solution soaking of 200mL3.0 mol/L, stir, calorify 55 DEG C of isothermal reaction 4h, cool to room temperature, spend deionized water to neutral, filtration, drying, obtain alkalization porous sephadex;
(2) epoxidation porous sephadex preparation, feature is: in the reactor, adds respectively, water: 70mL, NaOH:4g, after dissolving, cool to room temperature, then add epoxychloropropane: 6mL; Absolute ethyl alcohol: 16mL, alkalization porous sephadex: 4g, stir, in 50 ± 2 DEG C of constant temperature, back flow reaction 6 h, after cooling, spend deionized water, suction filtration, to filtrate is neutrality, after a small amount of ethanol washing, be placed in 70 ± 5 DEG C of vacuum drying chambers dry, obtain epoxidation porous sephadex;
(3) hole, ethylenediamine Quito sephadex preparation, feature is: in the reactor, adds water: 56mL, sodium carbonate: 4g, after dissolving, then adds ethylenediamine: 15mL; Absolute ethyl alcohol: 15mL, epoxidation porous sephadex: 10g, in 60 ± 2 DEG C of constant temperature, stirring, back flow reaction 4h, after cooling, spend deionized water, suction filtration, to filtrate is neutrality, after a small amount of ethanol washing, be placed in 70 ± 5 DEG C of vacuum drying chambers dry, obtain hole, ethylenediamine Quito sephadex.
Embodiment 7
Hole, ethylenediamine Quito of the present invention sephadex is to the adsorption test of leaded ions mimic water: select 6 kinds of products prepared by above-described embodiment as adsorbent, by following waste water treatment process, experimental result lists table 1. in
(1) initial concentration got containing lead ion is simulated wastewater 200 mL of 500mg/L;
(2) adjust ph is in 2.0 ~ 8.5 scopes;
(3) in simulated water sample, add hole, ethylenediamine Quito sephadex, adsorbent amount is 1.0g/L water sample, and stirred at ambient temperature adsorbs 30 min;
(4) static concentration of getting supernatant Aas Determination of Lead In China ion, calculates adsorption capacity.
Hole, table 1 ethylenediamine Quito sephadex is to the adsorption capacity of lead ion
| Adsorbent | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 | Ethylenediamine base sephadex |
| Adsorption capacity (mg/g) | 312.6 | 313.7 | 315.2 | 312.8 | 316.2 | 315.5 | 182.6 |
As seen from Table 1, hole, ethylenediamine Quito of the present invention sephadex is 316.2mg/g to the maximum adsorption capacity of lead ion, and ethylenediamine base sephadex adsorption capacity is 182.6mg/g.
Embodiment 8
Hole, ethylenediamine Quito of the present invention sephadex is to containing the adsorption test of cadmium ion Simulated Water: select 6 kinds of products prepared by above-described embodiment as adsorbent, by the waste water treatment process of embodiment 7, the initial concentration of cadmium ion is 300mg/L, and experimental result lists table 2 in.
Hole, table 2 ethylenediamine Quito sephadex is to the adsorption capacity of cadmium ion
| Adsorbent | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 | Ethylenediamine base sephadex |
| Adsorption capacity (mg/g) | 206.2 | 208.1 | 207.5 | 206.8 | 208.9 | 207.6 | 121.2 |
As seen from Table 2, hole, ethylenediamine Quito of the present invention sephadex is 208.9mg/g to the maximum adsorption capacity of cadmium ion, and ethylenediamine base sephadex adsorption capacity is 121.2mg/g.。
Embodiment 9
Hole, ethylenediamine Quito of the present invention sephadex is to the adsorption test of copper ions Simulated Water: select 5 kinds of products prepared by above-described embodiment as adsorbent, by the waste water treatment process of embodiment 7, the initial concentration of copper ion is 200mg/L, and experimental result lists table 3 in.
Hole, table 3 ethylenediamine Quito sephadex is to the adsorption capacity of copper ion
| Adsorbent | Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Embodiment 6 | Ethylenediamine base sephadex |
| Adsorption capacity (mg/g) | 114.1 | 115.2 | 115.9 | 113.9 | 113.2 | 115.8 | 66.5 |
As seen from Table 3, hole, ethylenediamine Quito of the present invention sephadex is 115.8mg/g to the maximum adsorption capacity of cadmium ion, and ethylenediamine base sephadex adsorption capacity is 66.5mg/g.
When in wastewater sample, the content of heavy metal ion is less than the adsorption capacity of hole, ethylenediamine Quito dextrangel adsorbent, adsorption rate can reach 98%, 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.
Absorption property is measured by dynamic method, hole, a certain amount of ethylenediamine Quito sephadex is loaded adsorption column in a wet process, get the metal ion solution of variable concentrations, by diluted acid and diluted alkaline adjust ph, adsorption column is passed through with the flow velocity of 2 mL/min, by the amount of metal ion that atomic absorption detecting filtered fluid and post adsorb, calculate adsorption rate thus.
Claims (5)
1. a preparation method for hole, ethylenediamine Quito dextrangel adsorbent, is characterized in that: the method specific embodiment is as follows:
(1) prepared by the porous sephadex that alkalizes, feature is: in the reactor, by sephadex distilled water immersion 24 ~ 48h, fully wash to neutrality by deionized water, filter, be placed in-12 ~-18 DEG C of quick freeze 20 ~ 50h, thaw at RT, be 100 ~ 200g/L by it by solid-to-liquid ratio again, be the NaOH aqueous solution soaking of 2.0 ~ 3.5mol/L by molar concentration, stir, calorify isothermal reaction 2 ~ 4h within the scope of 50 ~ 60 DEG C, cool to room temperature, spend deionized water to neutral, filtration, drying, obtain alkalization porous sephadex; Its specific area can reach 450 ~ 700m
2/ g;
(2) epoxidation porous sephadex preparation, feature is: in the reactor, adds, water: 45 ~ 70%, NaOH:4 ~ 10% by following composition mass percent, after dissolving, cool to room temperature, then add epoxychloropropane: 6 ~ 14%; Absolute ethyl alcohol: 16 ~ 25%, alkalization porous sephadex: 2 ~ 10%, each component sum is absolutely, in 50 ± 2 DEG C of constant temperature, stirring, back flow reaction 4 ~ 8h, after cooling, spend deionized water, suction filtration, to filtrate is neutrality, after a small amount of ethanol washing, be placed in 70 ± 5 DEG C of vacuum drying chambers dry, obtain epoxidation porous sephadex;
(3) hole, ethylenediamine Quito sephadex preparation, feature is: in the reactor, and add by following composition mass percent, water: 52 ~ 82%, sodium carbonate: 1.0 ~ 6.0%, after dissolving, then adds ethylenediamine: 6 ~ 16%; Absolute ethyl alcohol: 6 ~ 15%, epoxidation porous sephadex: 1.5 ~ 10%, each component sum is absolutely, in 60 ± 2 DEG C of constant temperature, stirring, back flow reaction 2 ~ 4h, after cooling, spend deionized water, suction filtration, to filtrate is neutrality, after a small amount of ethanol washing, be placed in 70 ± 5 DEG C of vacuum drying chambers dry, obtain hole, ethylenediamine Quito sephadex.
2. the preparation method of hole, a kind of ethylenediamine Quito according to claim 1 dextrangel adsorbent, is characterized in that: described sephadex is sephadex g-100, sephadex G-200.
3. the preparation method of hole, a kind of ethylenediamine Quito according to claim 1 dextrangel adsorbent, is characterized in that: the epoxychloropropane described in step (2) and the volume ratio of absolute ethyl alcohol are 1:2 ~ 3.
4. the preparation method of hole, a kind of ethylenediamine Quito according to claim 1 dextrangel adsorbent, is characterized in that: the ethylenediamine described in step (3) and the volume ratio of absolute ethyl alcohol are 1:0.8 ~ 2.
5. adopt the purposes of hole, a kind of ethylenediamine Quito dextrangel adsorbent prepared by method described in claim 1, it is characterized in that: this adsorbent is used for heavy metal ions in wastewater process and separation of heavy metal ions enrichment.
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| CN106064081A (en) * | 2016-06-13 | 2016-11-02 | 王金明 | A kind of preparation method of nickel plating solution detin adsorbent |
| CN106215881B (en) * | 2016-09-07 | 2018-02-09 | 济南大学 | A kind of preparation method of cyanurotriamide modified porous magnetic dextran microspheres |
| CN107096509B (en) * | 2017-04-13 | 2019-06-25 | 艾美科健（中国）生物医药有限公司 | It is a kind of containing α-amido succinic acid function base sephadex and preparation method |
| CN110038525A (en) * | 2019-03-21 | 2019-07-23 | 济南大学 | A kind of preparation method of cucurbit (7) urea modified magnetic porous adsorbent |
| CN110255568B (en) * | 2019-06-28 | 2022-06-10 | 广西大学 | Internal and external double-layer amino modified SiO2Aerogel synthesis method and application thereof |
| CN112892478A (en) * | 2021-01-17 | 2021-06-04 | 桂林理工大学 | Preparation method and application of biomass dye adsorbent |
| CN116671516A (en) * | 2023-08-04 | 2023-09-01 | 云南熙乐科技有限公司 | Preparation method of aqueous self-degradation antibacterial spray |
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| CN102908998B (en) * | 2012-11-09 | 2014-07-30 | 济南大学 | Preparation method of xanthate macro-pore dextrangel adsorbent |
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