CN108816198A - A kind of cadmium sorption agent and preparation method thereof - Google Patents
A kind of cadmium sorption agent and preparation method thereof Download PDFInfo
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- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28047—Gels
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- 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
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- C02F1/285—Treatment of water, waste water, or sewage by sorption using synthetic organic sorbents
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- 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
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- 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
- B01J2220/4806—Sorbents characterised by the starting material used for their preparation the starting material being of inorganic character
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- 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
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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
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Abstract
The invention discloses a kind of cadmium sorption agent and preparation method thereof, functional reagent I (alginate) is connected with functional reagent II by the condensation reaction of carboxyl and amino first, cadmium sorption agent hydrogel is made in alkaline-earth metal ions solution again, cadmium sorption agent is prepared by drying, the invention also discloses the cadmium sorption agent and its applications, the cadmium sorption agent is easy to be separated by solid-liquid separation, cadmium ion that can efficiently in adsorbed water body, it is high to the adsorption capacity of cadmium ion, and after being recycled for multiple times, its absorption property keeps stablizing, processing suitable for industrial wastewater and environmental water sample containing cadmium ion, application value with higher.
Description
Technical field
The invention belongs to solid phase adsorption fields, and in particular to a kind of cadmium sorption agent and preparation method thereof.
Background technique
With metallurgy, the rapid development of plating and chemical industry (such as battery, preservative, pigment), many is containing cadmium ion
Waste water is discharged into natural water.Cadmium ion into water body cannot be not only biodegradable, but also can pass through food chain
It into human body, is accumulated in human body, so that a series of serious physiological maladies are caused, such as osteomalacia, kidney injury and maincenter mind
Through damage etc..Therefore, the cadmium ion removed in water body is of great significance.
Currently, the method for removal Cadmium In The Water Body ion mainly has ion-exchange, membrane filter method, electrochemistry, absorption method, change
Learn the precipitation method, bioanalysis etc..Relative to other processing methods, with processing capacity, big, easy to operate, adsorbent can follow absorption method
The advantages that ring uses, especially when handling low concentration waste water containing cadmium ion, treatment effeciency and operating cost are with apparent excellent
Gesture.The inorganic nano material of reported cadmium sorption the agent mainly industrial and agricultural waste, clay of functionalization and some functionalization
Material etc..Wherein the industrial and agricultural waste of functionalization is low in cost, but absorption stability is not high, after being recycled for multiple times, absorption
Performance decline is very fast.For the clay of functionalization because being powder body material, recycling and reusing process is relatively complicated.The nanometer material of functionalization
Material is higher to the adsorption capacity and the rate of adsorption of cadmium ion due to specific surface area with higher, but nano material is because of size
It is small, reactivity is high, recycling and storage and transport process are more demanding, and the preparation cost of nano material is usually higher, these limitations
The further industrial applications of nano material absorbent.Therefore, develop it is a kind of it is being easily recycled, have compared with Gao Bibiao
Area and adsorption capacity, the cadmium sorption agent material with higher absorption stability it is particularly significant.In addition, so far,
Using alginate and melamine prepare cadmium sorption agent and be applied to the wastewater treatment containing cadmium ion relevant report it is less.
Summary of the invention
It is an object of the invention to：A kind of cadmium sorption agent and preparation method thereof is provided, prepared cadmium ion is inhaled
The attached dose of cadmium ion suitable for adsorbed water body, and be easily recycled, adsorption capacity and absorption stability are high, can be recycled.
In order to achieve the above-mentioned object of the invention, the present invention provides the following technical solutions：
A kind of cadmium sorption agent can be by chemical coordination side containing amino, carboxyl and hydroxyl and alkaline-earth metal ions
Formula and ion-exchange method combination cadmium ion.
A kind of preparation method of cadmium sorption agent, includes the following steps：
(1) functional reagent I is dissolved in acidic buffer solution, under stirring condition, be added condensing agent and functional reagent II into
Row reaction；
(2) under stirring condition, mixed liquor made from step (1) is instilled in the solution of alkaline including earth metal ion, has been reacted
The cadmium sorption agent is made through separation of solid and liquid, washing, drying in Quan Hou；
Wherein, functional reagent I is at least one of potassium alginate, sodium alginate or alginic acid；Acidic buffer solution is
2-morpholine ethane sulfonic acid-sodium hydroxide buffer solution, disodium hydrogen phosphate-citric acid solution, citric acid-sodium citrate buffering are molten
One of liquid, acetic acid-sodium acetate buffer solution, disodium hydrogen phosphate-potassium dihydrogen phosphate buffer solution；Condensing agent is 1- ethyl-
(3- dimethylaminopropyl) carbodiimide hydrochloride, 2- (7- aoxidizes benzotriazole)-N, N, N', N'- tetramethylurea hexafluoro
At least one of phosphate, n-hydroxysuccinimide and I-hydroxybenzotriazole；Functional reagent II is melamine, 2,4-
At least one of diamino -6- phenyl -1,3,5- triazine, N- cyclopropyl -1,3,5- triazine -2,4,6- triamine；Containing alkaline earth gold
The solution for belonging to ion is the solution of one of calcium ions, strontium ion, barium ions or different kinds of ions.
Preferably, the functional reagent I is sodium alginate；Acidic buffer solution is 2-morpholine ethane sulfonic acid-sodium hydroxide
Buffer solution；Condensing agent is 1- ethyl-(3- dimethylaminopropyl) carbodiimide hydrochloride；Functional reagent II is melamine
Amine；The solution of alkaline including earth metal ion is the aqueous solution of calcium ions.
Preferably, reaction temperature is 5~80 DEG C in step (1)；Reaction time is greater than 6h.
Preferably, reaction temperature is 10~40 DEG C in step (1)；Reaction time is 11~13h.
Preferably, reaction temperature is 5~90 DEG C in step (2)；Continue mixing time after dripping off and is greater than 10min.
Preferably, reaction temperature is 10~40 DEG C in step (2)；Continuing mixing time after dripping off is 18~22min.
Preferably, dry for vacuum drying or vacuum freeze drying in step (2).
Preferably, dry in step (2) is vacuum freeze drying, and the condition of vacuum freeze drying is：First -14~-16
3.5~4.5h is freezed at a temperature of DEG C, is dried in vacuo 11~13h afterwards.
The beneficial effects of the present invention are：
(1) the cadmium sorption agent category macroscopic material is easy to be separated by solid-liquid separation and recycle, and physics with higher and chemistry
Stability；
(2) the cadmium sorption agent is high to the adsorption rate and adsorption capacity of cadmium ion；
(3) the cadmium sorption agent is i.e. renewable after acid solution wash, can be recycled, and absorption property is stablized, tool
There is wide industrial applications prospect.
Detailed description of the invention
Fig. 1 is the synthetic route chart of cadmium sorption agent in embodiment 1；
Fig. 2 is (a) digital photograph and (b, c) scanning electron microscope diagram piece of cadmium sorption agent prepared by embodiment 1.
Specific embodiment
Embodiment 1：Synthesize cadmium sorption agent
Fig. 1 is the synthetic route chart that the present embodiment prepares cadmium sorption agent, as shown in Figure 1, specific step is as follows：
(1) 1.5g sodium alginate (viscosity is weighed：200 ± 20mPas) it is dissolved in the 2-morpholine ethane sulfonic acid-of 98.5g pH5.5
In sodium hydroxide (MES) buffer solution, under stirring condition, it is sub- that 0.15g 1- (3- dimethylamino-propyl) -3- ethyl carbon two is added
Amine hydrochlorate (EDC) and 0.5g melamine under the conditions of 25 DEG C, continue to be stirred to react 12h, afterwards will using 10mL injector for medical purpose
The mixed liquor is instilled dropwise in 500mL 0.2mol/L calcium nitrate solution, continues to stir 20min, through filtering, distilled water after dripping off
Calcium alginate-melamine composite hydrogel is made in washing；
(2) calcium alginate made from step (1)-melamine composite hydrogel is soaked in distilled water, is placed in vacuum
It freezes, be dried in vacuo in freeze drier, (condition of vacuum freeze drying is：4h, rear vacuum are first freezed at a temperature of -15 DEG C
Dry 12h.) calcium alginate-melamine composite aerogel (cadmium sorption agent) is made.
Embodiment 2：Synthesize cadmium sorption agent
(1) it weighs 1.5g potassium alginate to be dissolved in 2-morpholine ethane sulfonic acid (MES) buffer solution of 98.5g pH 5.5, stir
Under the conditions of, 0.15g 1- (3- dimethylamino-propyl) -3- ethyl-carbodiimide hydrochloride (EDC) and 0.5g melamine is added,
Under the conditions of 25 DEG C, continue to be stirred to react 12h, the mixed liquor is instilled by 500mL0.2mol/ using 10mL injector for medical purpose dropwise afterwards
In L calcium nitrate solution, continues to stir 20min after dripping off, be filtered, distill water washing, it is compound that calcium alginate-melamine is made
Hydrogel；
(2) calcium alginate made from step (1)-melamine composite hydrogel is soaked in distilled water, is placed in vacuum
It freezes, be dried in vacuo in freeze drier, be made calcium alginate-melamine composite aerogel (cadmium sorption agent).
Embodiment 2 is relative to the difference of embodiment 1：Sodium alginate is replaced with into potassium alginate.
Embodiment 3：Synthesize cadmium sorption agent
(1) 2-morpholine ethane sulfonic acid-sodium hydroxide (MES) buffer solution that 1.5g alginic acid is dissolved in 98.5gpH 5.5 is weighed
In, under stirring condition, 0.15g 1- (3- dimethylamino-propyl) -3- ethyl-carbodiimide hydrochloride (EDC) and 0.5g tri- is added
Poly cyanamid under the conditions of 25 DEG C, continues to be stirred to react 12h, and the mixed liquor is instilled 500mL dropwise using 10mL injector for medical purpose afterwards
In 0.2mol/L calcium nitrate solution, continues to stir 20min after dripping off, be filtered, distill water washing, calcium alginate-trimerization is made
Cyanamide composite hydrogel；
(2) calcium alginate made from step (1)-melamine composite hydrogel is soaked in distilled water, is placed in vacuum
It freezes, be dried in vacuo in freeze drier, be made calcium alginate-melamine composite aerogel (cadmium sorption agent).
Embodiment 3 is relative to the difference of embodiment 1：Sodium alginate is replaced with into alginic acid.
Embodiment 4：Synthesize cadmium sorption agent
(1) 1.5g sodium alginate (viscosity is weighed：200 ± 20mPas) it is dissolved in the 2-morpholine ethane sulfonic acid-of 98.5g pH5.5
In sodium hydroxide (MES) buffer solution, under stirring condition, 0.15g n-hydroxysuccinimide and 0.5g melamine is added,
Under the conditions of 25 DEG C, continue to be stirred to react 12h, the mixed liquor is instilled by 500mL0.2mol/ using 10mL injector for medical purpose dropwise afterwards
In L calcium nitrate solution, continues to stir 20min after dripping off, be filtered, distill water washing, it is compound that calcium alginate-melamine is made
Hydrogel；
(2) calcium alginate made from step (1)-melamine composite hydrogel is soaked in distilled water, is placed in vacuum
It freezes, be dried in vacuo in freeze drier, be made calcium alginate-melamine composite aerogel (cadmium sorption agent).
Embodiment 4 is relative to the difference of embodiment 1：By 1- (3- dimethylamino-propyl) -3- ethyl carbodiimide salt
Hydrochlorate replaces with n-hydroxysuccinimide.
Embodiment 5：Synthesize cadmium sorption agent
(1) 1.5g sodium alginate (viscosity is weighed：200 ± 20mPas) it is dissolved in the 2-morpholine ethane sulfonic acid-of 98.5g pH5.5
In sodium hydroxide (MES) buffer solution, under stirring condition, 0.15g 2- (7- aoxidizes benzotriazole)-N, N, N', N'- is added
Tetramethylurea hexafluorophosphoric acid ester and 0.5g melamine under the conditions of 25 DEG C, continue to be stirred to react 12h, use 10mL medical injection afterwards
Emitter instills the mixed liquor in 500mL 0.2mol/L calcium nitrate solution dropwise, continues to stir 20min after dripping off, through filtering,
Water washing is distilled, calcium alginate-melamine composite hydrogel is made；
(2) calcium alginate made from step (1)-melamine composite hydrogel is soaked in distilled water, is placed in vacuum
It freezes, be dried in vacuo in freeze drier, be made calcium alginate-melamine composite aerogel (cadmium sorption agent).
Embodiment 5 is relative to the difference of embodiment 1：By condensing agent 1- ethyl-(3- dimethylaminopropyl) carbon two
Inferior amine salt hydrochlorate replaces with 2- (7- aoxidizes benzotriazole)-N, N, N', N'- tetramethylurea hexafluorophosphoric acid ester.
Embodiment 6：Synthesize cadmium sorption agent
(1) 1.5g sodium alginate (viscosity is weighed：200 ± 20mPas) it is dissolved in the 2-morpholine ethane sulfonic acid-of 98.5g pH5.5
In sodium hydroxide (MES) buffer solution, under stirring condition, it is sub- that 0.15g 1- (3- dimethylamino-propyl) -3- ethyl carbon two is added
Amine hydrochlorate (EDC) and 0.5g melamine under the conditions of 60 DEG C, continue to be stirred to react 12h, afterwards will using 10mL injector for medical purpose
The mixed liquor is instilled dropwise in 500mL 0.2mol/L calcium nitrate solution, continues to stir 20min, through filtering, distilled water after dripping off
Calcium alginate-melamine composite hydrogel is made in washing；
(2) calcium alginate made from step (1)-melamine composite hydrogel is soaked in distilled water, is placed in vacuum
It freezes, be dried in vacuo in freeze drier, be made calcium alginate-melamine composite aerogel (cadmium sorption agent).
Embodiment 6 is relative to the difference of embodiment 1：Step (1) reaction temperature is replaced with 60 DEG C by 25 DEG C.
Embodiment 7：Synthesize cadmium sorption agent
(1) 1.5g sodium alginate (viscosity is weighed：200 ± 20mPas) it is dissolved in the 2-morpholine ethane sulfonic acid-of 98.5g pH5.5
In sodium hydroxide (MES) buffer solution, under stirring condition, it is sub- that 0.15g 1- (3- dimethylamino-propyl) -3- ethyl carbon two is added
Amine hydrochlorate (EDC) and 0.5g melamine under the conditions of 5 DEG C, continue to be stirred to react 12h, afterwards will using 10mL injector for medical purpose
The mixed liquor is instilled dropwise in 500mL 0.2mol/L calcium nitrate solution, continues to stir 20min, through filtering, distilled water after dripping off
Calcium alginate-melamine composite hydrogel is made in washing；
(2) calcium alginate made from step (1)-melamine composite hydrogel is soaked in distilled water, is placed in vacuum
It freezes, be dried in vacuo in freeze drier, be made calcium alginate-melamine composite aerogel (cadmium sorption agent).
Embodiment 7 is relative to the difference of embodiment 1：Step (1) reaction temperature is replaced with 5 DEG C by 25 DEG C.
Embodiment 8：Synthesize cadmium sorption agent
(1) 1.5g sodium alginate (viscosity is weighed：200 ± 20mPas) it is dissolved in the 2-morpholine ethane sulfonic acid-of 98.5g pH5.5
In sodium hydroxide (MES) buffer solution, under stirring condition, it is sub- that 0.15g 1- (3- dimethylamino-propyl) -3- ethyl carbon two is added
Amine hydrochlorate (EDC) and 0.5g melamine under the conditions of 25 DEG C, continue to be stirred to react for 24 hours, afterwards will using 10mL injector for medical purpose
The mixed liquor is instilled dropwise in 500mL 0.2mol/L calcium nitrate solution, continues to stir 20min, through filtering, distilled water after dripping off
Calcium alginate-melamine composite hydrogel is made in washing；
(2) calcium alginate made from step (1)-melamine composite hydrogel is soaked in distilled water, is placed in vacuum
It freezes, be dried in vacuo in freeze drier, be made calcium alginate-melamine composite aerogel (cadmium sorption agent).
Embodiment 8 is relative to the difference of embodiment 1：Step (1) reaction time is replaced with for 24 hours by 12h.
Embodiment 9：Synthesize cadmium sorption agent
(1) 1.5g sodium alginate (viscosity is weighed：200 ± 20mPas) it is dissolved in the 2-morpholine ethane sulfonic acid-of 98.5g pH5.5
In sodium hydroxide (MES) buffer solution, under stirring condition, it is sub- that 0.15g 1- (3- dimethylamino-propyl) -3- ethyl carbon two is added
Amine hydrochlorate (EDC) and 0.5g melamine under the conditions of 25 DEG C, continue to be stirred to react 4h, afterwards will using 10mL injector for medical purpose
The mixed liquor is instilled dropwise in 500mL 0.2mol/L calcium nitrate solution, continues to stir 20min, through filtering, distilled water after dripping off
Calcium alginate-melamine composite hydrogel is made in washing；
(2) calcium alginate made from step (1)-melamine composite hydrogel is soaked in distilled water, is placed in vacuum
It freezes, be dried in vacuo in freeze drier, be made calcium alginate-melamine composite aerogel (cadmium sorption agent).
Embodiment 9 is relative to the difference of embodiment 1：Step (1) reaction time is replaced with into 4h by 12h.
Embodiment 10：Synthesize cadmium sorption agent
(1) 1.5g sodium alginate (viscosity is weighed：200 ± 20mPas) it is dissolved in the 2-morpholine ethane sulfonic acid-of 98.5g pH5.5
In sodium hydroxide (MES) buffer solution, under stirring condition, it is sub- that 0.15g 1- (3- dimethylamino-propyl) -3- ethyl carbon two is added
Amine hydrochlorate (EDC) and 1.0g melamine under the conditions of 25 DEG C, continue to be stirred to react 12h, afterwards will using 10mL injector for medical purpose
The mixed liquor is instilled dropwise in 500mL 0.2mol/L calcium nitrate solution, continues to stir 20min, through filtering, distilled water after dripping off
Calcium alginate-melamine composite hydrogel is made in washing；
(2) calcium alginate made from step (1)-melamine composite hydrogel is soaked in distilled water, is placed in vacuum
It freezes, be dried in vacuo in freeze drier, be made calcium alginate-melamine composite aerogel (cadmium sorption agent).
Embodiment 10 is relative to the difference of embodiment 1：The quality of melamine in step (1) is replaced with by 0.5g
1.0g。
Embodiment 11：Synthesize cadmium sorption agent
(1) 1.5g sodium alginate (viscosity is weighed：200 ± 20mPas) it is dissolved in the 2-morpholine ethane sulfonic acid-of 98.5g pH5.5
In sodium hydroxide (MES) buffer solution, under stirring condition, it is sub- that 0.15g 1- (3- dimethylamino-propyl) -3- ethyl carbon two is added
Amine hydrochlorate (EDC) and 0.2g melamine under the conditions of 25 DEG C, continue to be stirred to react 12h, afterwards will using 10mL injector for medical purpose
The mixed liquor is instilled dropwise in 500mL 0.2mol/L calcium nitrate solution, continues to stir 20min, through filtering, distilled water after dripping off
Calcium alginate-melamine composite hydrogel is made in washing；
(2) calcium alginate made from step (1)-melamine composite hydrogel is soaked in distilled water, is placed in vacuum
It freezes, be dried in vacuo in freeze drier, be made calcium alginate-melamine composite aerogel (cadmium sorption agent).
Embodiment 11 is relative to the difference of embodiment 1：The quality of melamine in step (1) is replaced with by 0.5g
0.2g。
Embodiment 12
The cadmium sorption agent made from embodiment 1 handles the water sample containing cadmium ion, to Cd in water sample2+Adsorption rate and
Maximum adsorption capacity is as shown in table 1：
Specific step is as follows for adsorption test：
(a) Cd of 1000mg/L is drawn respectively2+Standard reserving solution 5,10,20,50,80mL to 100mL volumetric flask, add distillation
Water is settled to scale, shakes up, and stands, the Cd of preparation2+Concentration of standard solution is respectively 50mg/L, 100mg/L, 200mg/L, 500mg/
L, 800mg/L；
(b) with Cd in the solution of inductive coupling plasma emission spectrograph (ICP-OES) measurement preparation2+Actual concentrations
Value；
(c) weigh~100mg embodiment 1 made from cadmium sorption agent be scattered in 40mL step (a) preparation Cd2+Standard
It in liquid, is filtered after 6h, with remaining Cd in ICP-OES measurement filtrate2+Concentration；
(d) by following formula, cadmium sorption agent is calculated to Cd2+Adsorption rate and adsorption capacity.
Wherein C0For Cd2+Initial concentration (mg/L), CfFor residue Cd in filtrate after absorption2+Concentration (mg/L), W are cadmium ion
Adsorbent mass.
The cadmium sorption agent of 1 embodiment 1 of table is to Cd2+Adsorption rate and maximum adsorption capacity
Embodiment 13
The absorption property of the cadmium sorption agent of embodiment 1-11 preparation is tested, obtained data such as the following table 2, table
Shown in 3：
Maximum adsorption capacity, performance data are recycled in the adsorption rate of 2 embodiment 1-5 of table
Adsorption capacity, performance experimental data is recycled in the adsorption rate of 3 embodiment 6-11 of table
Embodiment 14
Acquisition contains Cd2+Plant chimney stalk water sample or contain Cd2+Environmental water sample, then inhaled with cadmium ion made from embodiment 1
Attached dose adsorbs it, and the data obtained is as shown in table 4 below：
Specific step is as follows for adsorption experiment：
(a) water sampling to be adsorbed：Certain depth (10 with water sampler in three different locations in waste water from plating plant pond
~50cm) at acquire water sample；With water sampler Xue Hu (Anhui Province's Qianshan County) three different locations certain depth (10~
50cm) place acquires water sample；
(b) Cd in water sample to be adsorbed is measured with ICP-OES2+Concentration value；
(c) weigh~100mg embodiment 1 made from cadmium sorption agent be scattered in 40mL step (1) water sample to be adsorbed,
It is filtered after 6h, with residue Cd in ICP-OES measurement filtrate2+Concentration, to calculate cadmium sorption agent to Cd2+Adsorption rate.
4 cadmium sorption agent of table absorption contains Cd2+The adsorpting data of water sample
| Waste water from plating plant 1 | Waste water from plating plant 2 | Waste water from plating plant 3 | |
| Cd in raw water sample2+Concentration value | 57.29mg/L | 58.71mg/L | 57.33mg/L |
| Residue Cd in filtrate2+Concentration value | 0.21mg/L | 0.28mg/L | 0.19mg/L |
| Adsorption rate | 99.63% | 99.52% | 99.66% |
| Avenge lake water 1 | Avenge lake water 2 | Avenge lake water 3 | |
| Cd in raw water sample2+Concentration value | 17.16mg/L | 15.24mg/L | 16.53mg/L |
| Residue Cd in filtrate2+Concentration value | 0.04mg/L | 0.03mg/L | 0.04mg/L |
| Adsorption rate | 99.78% | 99.80% | 99.75% |
Embodiment 15
The cadmium sorption agent prepared to embodiment 1 is recycled, and obtained adsorpting data is as shown in table 5 below：
Experiment is recycled, and specific step is as follows：
(a) Cd will be adsorbed with2+Cadmium sorption agent be added acid solution in, by acid protonation, make Cd2+From
It is separated in cadmium sorption agent；
(b) it filters, successively uses distilled water, Ca (OH)2Solution (0.01mol/L), distillation water washing have sloughed Cd2+Suction
Attached dose, the regeneration of cadmium sorption agent can be realized after dry.
Wherein, acid solution be selected from acetic acid, nitric acid, hydrochloric acid, phosphoric acid, oxalic acid, or combinations thereof, preferably acetic acid.When the acid
It when being applied in combination, can successively be handled using acid, or be handled after acid-mixed is closed.
The performance parameter that 5 cadmium sorption agent of table is recycled
Technical solution of the present invention is described in detail in embodiment described above, it should be understood that the above is only
It for specific embodiments of the present invention, is not intended to restrict the invention, all any modifications made in spirit of the invention
With improve etc., should all be included in the protection scope of the present invention.
Claims (9)
1. a kind of cadmium sorption agent, it is characterised in that：Containing amino, carboxyl and hydroxyl and alkaline-earth metal ions, can pass through
Chemical coordination mode and ion-exchange method combination cadmium ion.
2. a kind of preparation method of cadmium sorption agent, it is characterised in that：Include the following steps：
(1) functional reagent I is dissolved in acidic buffer solution, under stirring condition, condensing agent is added and functional reagent II is carried out instead
It answers；
(2) under stirring condition, mixed liquor made from step (1) is instilled in the solution of alkaline including earth metal ion, after fully reacting,
Through separation of solid and liquid, washing, drying, the cadmium sorption agent is made；
Wherein, functional reagent I is at least one of potassium alginate, sodium alginate or alginic acid；Acidic buffer solution is 2-
Quinoline ethanesulfonic acid-sodium hydroxide buffer solution, disodium hydrogen phosphate-citric acid solution, citric acid-sodium citrate buffer,
One of acetic acid-sodium acetate buffer solution, disodium hydrogen phosphate-potassium dihydrogen phosphate buffer solution；Condensing agent is 1- ethyl-(3-
Dimethylaminopropyl) carbodiimide hydrochloride, 2- (7- aoxidizes benzotriazole)-N, N, N', N'- tetramethylurea hexafluorophosphoric acid
At least one of ester, n-hydroxysuccinimide and I-hydroxybenzotriazole；Functional reagent II is melamine, 2,4- diamino
At least one of base -6- phenyl -1,3,5- triazine, N- cyclopropyl -1,3,5- triazine -2,4,6- triamine；Alkaline including earth metal from
The solution of son is the solution of one of calcium ions, strontium ion, barium ions or different kinds of ions.
3. a kind of preparation method of cadmium sorption agent according to claim 2, it is characterised in that：The functional reagent
I is sodium alginate；Acidic buffer solution is 2-morpholine ethane sulfonic acid-sodium hydroxide buffer solution；Condensing agent is 1- ethyl-(3- bis-
Dimethylaminopropyl) carbodiimide hydrochloride；Functional reagent II is melamine；The solution of alkaline including earth metal ion be calcic from
The aqueous solution of son.
4. a kind of preparation method of cadmium sorption agent according to claim 2, it is characterised in that：Reaction in step (1)
Temperature is 5~80 DEG C；Reaction time is greater than 6h.
5. a kind of preparation method of cadmium sorption agent according to claim 4, it is characterised in that：Reaction in step (1)
Temperature is 10~40 DEG C；Reaction time is 11~13h.
6. a kind of preparation method of cadmium sorption agent according to claim 2, it is characterised in that：Reaction in step (2)
Temperature is 5~90 DEG C；Continue mixing time after dripping off and is greater than 10min.
7. a kind of preparation method of cadmium sorption agent according to claim 6, it is characterised in that：Reaction in step (2)
Temperature is 10~40 DEG C；Continuing mixing time after dripping off is 18~22min.
8. a kind of preparation method of cadmium sorption agent according to claim 2, it is characterised in that：It is dry in step (2)
For vacuum drying or vacuum freeze drying.
9. a kind of preparation method of cadmium sorption agent according to claim 8, it is characterised in that：It is dry in step (2)
Condition for vacuum freeze drying, vacuum freeze drying is：3.5~4.5h, rear vacuum are first freezed at a temperature of -14~-16 DEG C
Dry 11~13h.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104258817A (en) * | 2014-07-30 | 2015-01-07 | 青岛科技大学 | Melamine-modified magnetic chitosan, preparation method and application thereof |
| CN104684850A (en) * | 2011-11-29 | 2015-06-03 | 新加坡科技研究局 | Melamine aldehyde polymers |
| CN106861643A (en) * | 2017-03-10 | 2017-06-20 | 安庆师范大学 | Bifunctional material and its synthetic method and application for detecting and adsorbing copper ion |
| CN107245135A (en) * | 2017-06-22 | 2017-10-13 | 蚌埠学院 | Organic porous polymer and its preparation method and application |
| CN107262073A (en) * | 2017-08-24 | 2017-10-20 | 安庆师范大学 | A kind of cadmium sorption agent and its preparation method and application |
-
2018
- 2018-07-11 CN CN201810759025.8A patent/CN108816198A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104684850A (en) * | 2011-11-29 | 2015-06-03 | 新加坡科技研究局 | Melamine aldehyde polymers |
| CN104258817A (en) * | 2014-07-30 | 2015-01-07 | 青岛科技大学 | Melamine-modified magnetic chitosan, preparation method and application thereof |
| CN106861643A (en) * | 2017-03-10 | 2017-06-20 | 安庆师范大学 | Bifunctional material and its synthetic method and application for detecting and adsorbing copper ion |
| CN107245135A (en) * | 2017-06-22 | 2017-10-13 | 蚌埠学院 | Organic porous polymer and its preparation method and application |
| CN107262073A (en) * | 2017-08-24 | 2017-10-20 | 安庆师范大学 | A kind of cadmium sorption agent and its preparation method and application |
Non-Patent Citations (1)
| Title |
|---|
| 王敏等: "改性海藻酸钙气凝胶的制备及吸附铅离子性能研究", 《化工新型材料》 * |
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Application publication date: 20181116 |