CN108940385A - A kind of preparation method of efficient defluorinate modified resin - Google Patents
A kind of preparation method of efficient defluorinate modified resin Download PDFInfo
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- CN108940385A CN108940385A CN201810825249.4A CN201810825249A CN108940385A CN 108940385 A CN108940385 A CN 108940385A CN 201810825249 A CN201810825249 A CN 201810825249A CN 108940385 A CN108940385 A CN 108940385A
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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
- B01J47/00—Ion-exchange processes in general; Apparatus therefor
- B01J47/016—Modification or after-treatment of ion-exchangers
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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
- B01J47/00—Ion-exchange processes in general; Apparatus therefor
- B01J47/014—Ion-exchange processes in general; Apparatus therefor in which the adsorbent properties of the ion-exchanger are involved, e.g. recovery of proteins or other high-molecular compounds
Abstract
The present invention relates to defluorinate vector resin technical fields, disclose a kind of preparation method of efficient defluorinate modified resin, are to pass through vector resin pretreatment, Al using 201 × 7 resin anion (R.A.)s as vector resin3+The processes such as the preparation of solution, the modification of vector resin, are made modified resin, realize the efficient absorption to the fluorine ion in water；201 × 7 resin anion (R.A.)s have ion exchanging function in acid, neutral and alkaline environment simultaneously; and the regeneration of modified resin can be realized by simple technique; be conducive to the recycling of modified resin; the use cost of modified resin can be reduced, the inexpensive needs of small-scale or household water defluorinate processing are met.
Description
Technical field
The present invention relates to defluorinate vector resin technical field, in particular to a kind of preparation sides of efficient defluorinate modified resin
Method.
Background technique
Fluorine ion (F-) it is one of noxious pollutant present in water, Excess free enthalpy F-It will lead to calcium and the phosphorus metabolism of human body
It is abnormal, cause serious health problems.The World Health Organization (WHO) provides maximum allowable F in water-Content is 1.5mg/L.Manyly
The water head site such as Bangladesh of side and the Northwest F of China-Content is higher, and the low-income household in these places is not appropriate
Water processing establishment is to F-It is effectively removed.The fluorine removal method for treating water that early-stage study is announced mainly has coagulation sedimentation, chemistry
The precipitation method, electroosmose process, electrocoagulation, hyperfiltration etc..Wherein: chemical precipitation method and coagulation sedimentation can leave a large amount of calcium aluminium
Plasma is mainly used for Industrial Wastewater Treatment；High-fluorine water is mainly distributed on the ground of the few electricity of bad environments, with a varied topography or water shortage
Area, so the fluoride-removing equipment of electroosmose process, electrocoagulation, hyperfiltration is because of device complexity, equipment valuableness and use cost height etc.
Factor and be difficult to promote.Therefore, these low-income households are highly desirable to a kind of water treatment technology of low cost easy to operate.
Resin with adsorption function be usually have functional group insoluble granule shape macromolecular organic material it is netted
Object.It is a kind of insoluble support construction, and usually in the form of small microballon, microballon is usually porous, provides big surface
Product (including interstitial space).Resin is adsorbed as a kind of novel absorption material, with large specific surface area, contamination resistance is strong, changes
The convenient advantage of property, has preferable suction-operated to the fluorine ion in water body.
Existing absorption resin is adsorbed by itself functional group, and this resin could be under the conditions of specific pH value
Row absorption, after the pH value in solution changes, substantially reduces the adsorption capacity of fluorine ion；And most of absorption resin is inhaled
Attached amount is smaller, regenerability is poor, regenerative process is complex, needs often to replace absorption resin, causes use cost
It is high.
Summary of the invention
Based on problem above, the present invention provides a kind of preparation methods of efficient defluorinate modified resin, to solve existing tree
The rouge problem small to the adsorbance of the fluorine ion in water；201 × 7 resin anion (R.A.)s are equal in acid, neutrality and alkaline environment simultaneously
There is ion exchanging function, and the regeneration of modified resin can be realized by simple technique, is conducive to the repetition benefit of modified resin
With can reduce the use cost of modified resin, meet the inexpensive needs of small-scale or household water defluorinate processing.
The present invention is achieved through the following technical solutions:
A kind of preparation method of efficient defluorinate modified resin, includes the following steps,
(1) pretreatment of raw material: 1. using 201 × 7 resin anion (R.A.)s as vector resin, with deionized water to vector resin
It is rinsed, until rinsing to no fouling product；2. vector resin is immersed in turn mass percent be 5% NaOH solution and
2h is impregnated in 5% HCl solution respectively, vector resin makes in described 5% NaOH solution and 5% HCl solution alternating gap
It is rinsed, the above process is repeated 3~4 times, for the last time with deionized water flush vehicle resin until after rinsing with deionized water
Aqueous solution pH near neutral；3. with excessive 4~5% NaOH solution impregnate vector resin 2h after filter, spend from
Sub- water elutes filtered vector resin and is in neutrality to rear solution is rinsed, and is then dried with baking oven；
(2)Al3+The preparation of solution: by AlCl3Dissolution in deionized water, is configured to Al3+Concentration is the Al of 4g/L3+It is molten
Liquid；
(3) Al in step (2) modification of vector resin: is added in flask3+Solution, by the load after pretreatment and drying
Body resin is added in flask, Al in the flask3+Mass ratio with vector resin is 1:20；PH value of solution in flask is adjusted to acid
Property, after shaking 3h in constant temperature oscillation box with fixed revolving speed, carry out solid and liquid separation, extract solid matter therein, spend from
Sub- water repeated flushing 4~5 times, until the pH of the aqueous solution after rinsing is in neutrality；Finally the solid matter after flushing is dried, is obtained
Obtain modified resin.
As a preferred mode, deionized water is the cation-exchange membrane and yin that water is successively passed through to 0.2 μm of aperture
Amberplex and obtain.
As a preferred mode, the thermostat temperature of constant temperature oscillation box is 60 ± 2 DEG C in step (3).
As a preferred mode, it is 2.5~3.5 that pH value range is adjusted in step (3) flask.
As a preferred mode, soda acid tune is carried out by the buffer that dilute hydrochloric acid and ammonium hydroxide are configured in step (3)
Section.
As a preferred mode, to the drying temperature of pretreatment and modified solid matter in step (1) and (3)
It is 50 ± 5 DEG C.
Compared with prior art, the present invention have the following advantages that and the utility model has the advantages that
1, the present invention is by using 201 × 7 resin anion (R.A.)s as vector resin, in acid condition with Al3+Solution mixing,
Al3+It can be chelated on vector resin skeleton in strongly acidic solution, realize the modification of vector resin.Because aluminium ion is to fluorine ion
Aluminium ion and fluorine ion is set to form a system by aluminium ion immobilized on 201 × 7 resin anion (R.A.)s with stronger affinity
Stable compound is arranged, to realize the efficient absorption to the fluorine ion in water；Simultaneously 201 × 7 resin anion (R.A.)s it is acid, in
Property and alkaline environment have ion exchanging function, and the regeneration of modified resin can be realized by simple technique, are conducive to change
Property resin recycling, can reduce the use cost of modified resin, meet small-scale or household water defluorinate processing it is low at
This needs.
2, the deionized water in the present invention is that water is successively passed through to cation-exchange membrane and the anion exchange in 0.2 μm of aperture
Film, when water passes through cation-exchange membrane, the cation in water is adsorbed, while the hydrogen ion released；By anion exchange
When film, the anion in water is adsorbed, and the hydroxide ion released, hydrogen ion generates pure after combining with hydroxide ion
Water, thus by the ion remaval in water.
3, the thermostat temperature of constant temperature oscillation box is 60 ± 2 DEG C, when other conditions are identical, 201 in step of the invention (3)
× 7 resin anion (R.A.)s are in 60 ± 2 DEG C of temperature ranges and Al3+Supported quantity when chelating is maximum, effectively increases defluorinate resin pair
The treating capacity of fluorine ions in water body.
4, it is 2.5~3.5, when other conditions are identical, acid item that pH value range is adjusted in step of the invention (3) flask
Under part, 201 × 7 resin anion (R.A.)s are to Al3+Immobilized Optimal pH condition be 2.5~3.5.
5, acid-base accommodation is carried out by the buffer that dilute hydrochloric acid and ammonium hydroxide are configured in step of the invention (3), by dilute
Hydrochloric acid and ammonium hydroxide form NH in the solution4Cl-NH3It buffers to come the pH value that maintains chelating process, minimum impurity can introduced
Under the conditions of element, pH value is in optimum range during guaranteeing chelating.
It 6, is 50 ± 5 to the drying temperature of pretreatment and modified solid matter in the step (1) in the present invention and (3)
DEG C, drying temperature is excessively high to cause modified resin to be denaturalized, while drying temperature is too low causes drying time longer, influences production effect
Rate.
Detailed description of the invention
Fig. 1 is Al on vector resin under condition of different temperatures3+The curve of supported quantity；
Al on vector resin when Fig. 2 is different pH3+The curve of supported quantity.
Specific embodiment
It is further described in detail below with reference to embodiment, embodiments of the present invention are not limited thereto:
Embodiment 1:
A kind of preparation method of efficient defluorinate modified resin, the method the following steps are included:
(1) pretreatment of raw material: 1. using 201 × 7 resin anion (R.A.)s as vector resin, with deionized water to vector resin
It is rinsed, until rinsing to no fouling product；2. vector resin is immersed in turn mass percent be 5% NaOH solution and
2h is impregnated in 5% HCl solution respectively, vector resin makes in described 5% NaOH solution and 5% HCl solution alternating gap
It is rinsed, the above process is repeated 3~4 times, for the last time with deionized water flush vehicle resin until after rinsing with deionized water
Aqueous solution pH near neutral；3. with excessive 4~5% NaOH solution impregnate vector resin 2h after filter, spend from
Sub- water elutes filtered vector resin and is in neutrality to rear solution is rinsed, and is then dried with baking oven；
(2)Al3+The preparation of solution: by AlCl3Dissolution in deionized water, is configured to Al3+Concentration is the Al of 4g/L3+It is molten
Liquid.
(3) Al in step (2) modification of vector resin: is added in flask3+Solution, by the load after pretreatment and drying
Body resin is added in flask, Al in the flask3+Mass ratio with vector resin is 1:20；PH value of solution in flask is adjusted to acid
Property, after shaking 3h in constant temperature oscillation box with fixed revolving speed, carry out solid and liquid separation, extract solid matter therein, spend from
Sub- water repeated flushing 4~5 times, until the pH of the aqueous solution after rinsing is in neutrality；Finally the solid matter after flushing is dried, is obtained
Obtain modified resin.
The present invention by using 201 × 7 resin anion (R.A.)s as vector resin, in acid condition with Al3+Solution mixing, Al3+
It can be chelated on vector resin skeleton in strongly acidic solution, realize the modification of vector resin.Because aluminium ion has fluorine ion
There is stronger affinity, by aluminium ion immobilized on 201 × 7 resin anion (R.A.)s, forms aluminium ion with fluorine ion a series of
Stable compound, to realize the efficient absorption to the fluorine ion in water；201 × 7 resin anion (R.A.)s are acid, neutral simultaneously
And alkaline environment has ion exchanging function, and the regeneration of modified resin can be realized by simple technique, is conducive to be modified
The recycling of resin can reduce the use cost of modified resin, meet the low cost of small-scale or household water defluorinate processing
It needs.
Embodiment 2:
A kind of preparation method of efficient defluorinate modified resin, the method the following steps are included:
(1) pretreatment of raw material: 1. using 201 × 7 resin anion (R.A.)s as vector resin, with deionized water to vector resin
It is rinsed, until rinsing to no fouling product；2. vector resin is immersed in turn mass percent be 5% NaOH solution and
2h is impregnated in 5% HCl solution respectively, vector resin makes in described 5% NaOH solution and 5% HCl solution alternating gap
It is rinsed, the above process is repeated 3~4 times, for the last time with deionized water flush vehicle resin until after rinsing with deionized water
Aqueous solution pH near neutral；3. with excessive 4~5% NaOH solution impregnate vector resin 2h after filter, spend from
Sub- water elutes filtered vector resin and is in neutrality to rear solution is rinsed, and is then dried with baking oven；
(2)Al3+The preparation of solution: by AlCl3Dissolution in deionized water, is configured to Al3+Concentration is the Al of 4g/L3+It is molten
Liquid.
(3) Al in step (2) modification of vector resin: is added in flask3+Solution, by the load after pretreatment and drying
Body resin is added in flask, Al in the flask3+Mass ratio with vector resin is 1:20；PH value of solution in flask is adjusted to acid
Property, after shaking 3h in constant temperature oscillation box with fixed revolving speed, carry out solid and liquid separation, extract solid matter therein, spend from
Sub- water repeated flushing 4~5 times, until the pH of the aqueous solution after rinsing is in neutrality；Finally the solid matter after flushing is dried, is obtained
Obtain modified resin.
Deionized water in the present invention is that water is successively passed through to cation-exchange membrane and the anion exchange in 0.2 μm of aperture
Film, when water passes through cation-exchange membrane, the cation in water is adsorbed, while the hydrogen ion released；By anion exchange
When film, the anion in water is adsorbed, and the hydroxide ion released, hydrogen ion generates pure after combining with hydroxide ion
Water, thus by the ion remaval in water.
Embodiment 3:
Resin after taking 1g to remove impurity using assay balance, is put into 50mL Al3+Content is to use in the solution of 1g/L
Solution ph is adjusted to 2 by pH meter and dilute hydrochloric acid or ammonium hydroxide.It adjusts the temperature under the conditions of 30 DEG C, 40 DEG C, 50 DEG C, 60 DEG C and 70 DEG C
Oscillation 3 hours using residue Al3+ content in water after spectrophotometry measurement experiment, and passes through residue Al3+ in water after experiment
Content calculates resin-carried Al3+Amount, experimental result is as shown in Figure 1.
As shown in Figure 1,201x7 resin is at 60 DEG C or less, resin-carried Al3+Amount with temperature parameter raising without
It is disconnected to improve.After 60 DEG C, 201x7 resin supported quantity is reduced, this is primarily due to Al3+Chelating resin kinetic energy companion during this
Increase with the raising of temperature parameter.Decline is primarily due to temperature and keeps raising after more than 60 DEG C, Al3+Hydrolysis rate
Accelerate, so as to cause resin-carried Al3+Amount declined.Therefore the best immobilized Al of the resin3+Temperature be 60 DEG C.
Embodiment 4:
Resin after taking 1g to remove impurity using assay balance, is put into 50mL Al3+Content is in the solution of 1g/L.It uses
PH meter and dilute hydrochloric acid or ammonium hydroxide change the pH in solution, and pH is adjusted to 2,2.5,3,3.5,4, when temperature is 60 DEG C, in machine
3h is vibrated on tool shaking table to be reacted.Other conditions remain unchanged, and use residue Al in water after spectrophotometry measurement experiment3+Contain
Amount, and resin-carried Al is obtained by formula3+Amount, experimental result is as shown in Figure 2.
It is readily appreciated that by Fig. 2, when pH value is in 2~3.5, the amount of modified resin load Al3+ increases with PH and increased
Add, and supported quantity reduces as pH increases when pH is under the conditions of 3.5~4.And experiment discovery, once pH is more than 4, solution meeting
The cotton-shaped particle that suspends is generated, solution becomes cloudy, and the amount of modified resin load Al3+.It follows that under acid condition, pH pairs
The immobilized influential effect of 201x7 resin is simultaneously little, and 201x7 resin Optimal pH condition is 2.5~3.5.
Acid-base accommodation is carried out by the buffer that dilute hydrochloric acid and ammonium hydroxide are configured to, passes through dilute hydrochloric acid and ammonium hydroxide shape in the solution
At NH4Cl-NH3It buffers to come the pH value that maintains chelating process, can guarantee to chelate under the conditions of introducing minimum impurity element
PH value is in optimum range in the process.
Embodiment 5:
A kind of preparation method of efficient defluorinate modified resin, the method the following steps are included:
(1) pretreatment of raw material: 1. using 201 × 7 resin anion (R.A.)s as vector resin, with deionized water to vector resin
It is rinsed, until rinsing to no fouling product；2. vector resin is immersed in turn mass percent be 5% NaOH solution and
2h is impregnated in 5% HCl solution respectively, vector resin makes in described 5% NaOH solution and 5% HCl solution alternating gap
It is rinsed, the above process is repeated 3~4 times, for the last time with deionized water flush vehicle resin until after rinsing with deionized water
Aqueous solution pH near neutral；3. with excessive 4~5% NaOH solution impregnate vector resin 2h after filter, spend from
Sub- water elutes filtered vector resin and is in neutrality to rear solution is rinsed, and is then dried with baking oven；
(2)Al3+The preparation of solution: by AlCl3Dissolution in deionized water, is configured to Al3+Concentration is the Al of 4g/L3+It is molten
Liquid.
(3) Al in step (2) modification of vector resin: is added in flask3+Solution, by the load after pretreatment and drying
Body resin is added in flask, Al in the flask3+Mass ratio with vector resin is 1:20；PH value of solution in flask is adjusted to acid
Property, after shaking 3h in constant temperature oscillation box with fixed revolving speed, carry out solid and liquid separation, extract solid matter therein, spend from
Sub- water repeated flushing 4~5 times, until the pH of the aqueous solution after rinsing is in neutrality；Finally the solid matter after flushing is dried, is obtained
Obtain modified resin.
It is 50 ± 5 to the drying temperature of pretreatment and modified solid matter in step (1) and (3) in the present invention
DEG C, drying temperature is excessively high to cause modified resin to be denaturalized, while drying temperature is too low causes drying time longer, influences production effect
Rate.
It is as described above the embodiment of the present invention.Design parameter in above-described embodiment and embodiment is merely to clear
The invention verification process of inventor, the scope of patent protection being not intended to limit the invention, patent protection of the invention are stated by Chu
Range is still subject to the claims, all with equivalent variations made by description of the invention, similarly should all
It is included within the scope of the present invention.
Claims (6)
1. a kind of preparation method of efficient defluorinate modified resin, which comprises the following steps:
(1) pretreatment of raw material:
1. being rinsed with deionized water to vector resin using 201 × 7 resin anion (R.A.)s as vector resin, until rinsing
To no fouling product；
2. it is to impregnate 2h respectively in 5% NaOH solution and 5% HCl solution that vector resin is successively immersed to mass percent,
After the completion of vector resin impregnates in described 5% NaOH solution, 5% HCl solution respectively, using going during transfer
Ionized water rinses；The above process is repeated 3~4 times, uses water of the deionized water flush vehicle resin after rinsing for the last time
The pH of solution is in neutrality；
3. being filtered after being completely soaked the vector resin 2h being in neutrality in 2. with 4~5% NaOH solution, filtered carrier tree
Rouge is rinsed with deionized water, until the aqueous solution for flushing is in neutrality, is then dried with baking oven；
(2)Al3+The preparation of solution: by AlCl3Dissolution in deionized water, is configured to Al3+Concentration is the Al of 4g/L3+Solution；
(3) Al in step (2) modification of vector resin: is added in flask3+Solution, by the carrier tree after pretreatment and drying
Rouge is added in flask, Al in the flask3+Mass ratio with vector resin is 1:20；PH value of solution in flask is adjusted to buffer
Acidity carries out solid and liquid separation after flask is shaken 3h in constant temperature oscillation box with fixed revolving speed, extracts solids therein
Matter, with deionized water repeated flushing 4~5 times, until the pH of the aqueous solution after rinsing is in neutrality；Finally by the solids after flushing
Matter drying, obtains modified resin.
2. a kind of preparation method of efficient defluorinate modified resin according to claim 1, it is characterised in that: the deionization
Water is by water successively by the cation-exchange membrane in 0.2 μm of aperture and anion-exchange membrane.
3. a kind of preparation method of efficient defluorinate modified resin according to claim 1, it is characterised in that: the step
(3) thermostat temperature of constant temperature oscillation box is 60 ± 2 DEG C in.
4. a kind of preparation method of efficient defluorinate modified resin according to claim 3, it is characterised in that: the step
(3) it is 2.5~3.5 that pH value range is adjusted in flask.
5. a kind of preparation method of efficient defluorinate modified resin according to claim 4, it is characterised in that: the step
(3) acid-base accommodation is carried out by the buffer that dilute hydrochloric acid and ammonium hydroxide are configured in.
6. a kind of preparation method of efficient defluorinate modified resin according to claim 1, it is characterised in that: the step
It (1) and in (3) is 50 ± 5 DEG C to the drying temperature of pretreatment and modified solid matter.
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Cited By (2)
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| CN114700065A (en) * | 2022-05-11 | 2022-07-05 | 南京工业大学 | Waste resin carbon sphere composite ozone catalyst and preparation method and application thereof |
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| CN114700065A (en) * | 2022-05-11 | 2022-07-05 | 南京工业大学 | Waste resin carbon sphere composite ozone catalyst and preparation method and application thereof |
| CN114700065B (en) * | 2022-05-11 | 2023-08-08 | 南京工业大学 | Waste resin carbon sphere composite ozone catalyst and preparation method and application thereof |
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Application publication date: 20181207 |
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