CN106669598A - Novel zeolite adsorbent for removing anionic pollutant in water and preparation method - Google Patents
Novel zeolite adsorbent for removing anionic pollutant in water and preparation method Download PDFInfo
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- CN106669598A CN106669598A CN201611191512.6A CN201611191512A CN106669598A CN 106669598 A CN106669598 A CN 106669598A CN 201611191512 A CN201611191512 A CN 201611191512A CN 106669598 A CN106669598 A CN 106669598A
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/16—Alumino-silicates
- B01J20/18—Synthetic zeolitic molecular sieves
- B01J20/186—Chemical treatments in view of modifying the properties of the sieve, e.g. increasing the stability or the activity, also decreasing the activity
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/0203—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of metals not provided for in B01J20/04
- B01J20/0207—Compounds of Sc, Y or Lanthanides
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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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/288—Treatment of water, waste water, or sewage by sorption using composite sorbents, e.g. coated, impregnated, multi-layered
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Abstract
The invention discloses a novel zeolite adsorbent for removing an anionic pollutant in water and a preparation method thereof, and relates to the field of materials and the technical field of water quality purification and sewage treatment. The novel zeolite adsorbent is characterized in that a cationic surfactant is loaded on the outer surface of zeolite; rare-earth-metal lanthanum capable of forming a complex compound with an anion is loaded in an internal super-cage; the more-efficient utilization of the inner and outer surfaces of a zeolite molecular sieve is achieved; thus, the capacity removal, on the anionic pollutant in the water, of the novel zeolite adsorbent is greatly improved. The novel adsorbent provided by the invention is convenient to prepare, excellent in effect, low in cost and high in utilization rate, and has a quite wide application prospect in the treatment of anionic polluted wastewater.
Description
Technical field
The present invention relates to it is a kind of for going eliminating water in anionic pollutant new zeolite adsorbent and preparation method, belong to
Material Field, purification of water quality and Pollutant Treatment technical field.
Background technology
For some micropollutant waters in nature, the aniones such as nitrate, phosphate, arsenate are widely present dirty
Dye thing.Pollutant load is small present in these water bodys, and general processing method is difficult under the conditions of Low investment that its is up to standard
Process.
Additionally, the various waste water that mankind's daily life and industry are produced, Jing after Sewage Plant process, it is still one that TN hardly possiblies are up to standard
It is individual to compare distinct issues, and N is mainly with the presence of nitrate nitrogen form in TN.Because carbon source is not enough and nitrate nitrogen content is relative
It is relatively low, biological denitrification apparatus are again introduced into, have that cost of investment is high, time-consuming and micro nitrate nitrogen is difficult to by microorganism for technique
The problem for utilizing very well, thus not economical and feasibility.
Absorption method has many advantages, such as that easy to operate, operating cost is low, more and more be used to process micro-polluted water
Trace contaminant in body and Sewage Plant bio-chemical effluent, and obtained good effect.
Some adsorbents have the strong limitation of unicity in adsorption treatment water pollutant, it is impossible to most of or
The pollutant of a certain type have good removal effect.And the modified of zeolite is concentrated on to its outer surface load difference in the past
Cationic surfactant improving the removal ability to anionic pollutant in water.But cationic surfactant point
Son is larger, it is impossible to into inside zeolite supercage, cause adsorbent prepared by previous methods to the absorbability of nitrate nitrogen relatively
It is low.In view of this, the invention provides it is a kind of for going eliminating water in anionic pollutant new zeolite adsorbent preparation side
Method so that most of anion state pollutant that may be present have preferable removal effect to adsorbent of the present invention in water.
The content of the invention
It is an object of the invention to overcome the shortcomings of that existing adsorbent absorption unicity and adsorbance are low, there is provided one kind can
Go the preparation method of the new zeolite adsorbent of various anionic pollutants in eliminating water.The adsorbent of the present invention is by outer surface sun
The electrostatic attraction of ionic surface active agent and ligand exchange are acted on, and the complexing of zeolite inside supercage lanthanum, greatly
The absorption to anionic pollutant in water is improved, so as to reach the purpose of micropollutant water purification.
The present invention is achieved through the following technical solutions：
The preparation method of the new zeolite adsorbent of anionic pollutant, comprises the following steps in for going eliminating water：
1) zeolite for taking 2~20 mass parts through remove impurity and performance activating pretreatment is in container, plus deionized water and stirs
Mix to form suspension；The hydrated lanthanum chloride of 0.5~5 mass parts is added, after stirring, pH is adjusted between 8-10 with NaOH solution,
Continue to stir after at least 2h, filter and deionized water is cleaned to without Cl-Exist；After drying, high-temperature activation promotes La in zeolite
Supercage inside bonding；
2) by step 1) zeolite of acquisition after high temperature activation is placed in cationic surfactant solution, vibration 5~
72h, obtains zeolite adsorbents after filtering drying.
In above-mentioned technical proposal, each step can be using following concrete optimal way：
Step 1) in, described zeolite adopts natural clinoptilolite, NaY zeolite molecular sieve or 13X zeolite molecular sieves.
Described preprocess method is：After zeolite is sieved, 0.5~2h is boiled with 1+3 hydrochloric acid, after washing filtering, in Muffle
400 DEG C of calcining 2-5h of stove, realize that the Impurity removal to zeolite surface and performance are activated.
Step 1) in, described sized zeolite particles are between 200~80 mesh.
Step 1) in, the mass ratio of zeolite and added lanthanum chloride is 10：1~2：Between 1.
Step 1) in, the concentration range of NaOH solution is 0.1~3mol/L.
Step 2) in, described cationic surfactant is cetyl trimethylammonium bromide, cation surface activating
Agent solution concentration range is between 10~50mM.
Step 2) in, hunting speed is 150~300rpm, and vibration temperature is 20~60 DEG C.
The present invention has an advantageous effect in that compared with prior art：
1. by loading different materials in outer surface of zeolite and supercage, improving zeolite molecular sieve surface adsorption and utilizing
Rate, strengthens its removal effect to most of anionic pollutant in water, purifies in Sewage Plant bio-chemical effluent and micropollutant water
In all have boundless application prospect.
2. zeolite materials are cheap, greatly reduce the cost of adsorbent.
3. adsorption process is easy to operate, less demanding to conditions such as temperature, pH, more energy-conserving and environment-protective.
Description of the drawings
Fig. 1 is the structural representation of adsorbent of the present invention.
Specific embodiment
Below in conjunction with the accompanying drawings the present invention is further elaborated with specific embodiment.
The new zeolite adsorbent preparation of the present invention is main negative with outer surface HDTMA including the La loads of zeolite supercage inside
Carry modified two parts.
Steady loads of the La inside zeolite supercage is realized by adjusting pH and high-temperature activation：Take 2~20 mass parts process
The zeolite of remove impurity and performance activating pretreatment in container, plus deionized water and stirring form suspension；Add 0.5~5 mass
The hydrated lanthanum chloride of part, after stirring, pH is adjusted between 8-10, continuing to stir after at least 2h with NaOH solution, is filtered and is spent
Ionized water is cleaned to without Cl-Exist.In the step, La is made with La (OH) by the regulation to pH2+、[La(OH2)La]4+[La
(OH)2La]4+Form be bonded to zeolite inner surface, promote it to move to the inside of zeolite supercage and stably bear by high-temperature activation
Carry.
The loaded modified of outer surface HDTMA is carried out in conical flask with cover.The zeolite of a certain amount of Jing high temperature drying activation is taken,
In being placed in the cationic surfactant solution of concentration excess (such as HDTMA solution), by constant temperature oscillation, major part can be made
HDTMA is carried on zeolite surface in the form of bilayer molecules.
By analysis, the new zeolite sorbent structure for ultimately forming is as shown in figure 1, inside molecular sieve outer surface and supercage
The different materials of load, realize the more efficient utilization to molecular sieve surface product, make adsorbent of the present invention to present in water it is cloudy from
Sub- pollutant this particular type pollutant have preferable adsorption effect.Specifically, zeolite molecular sieve outer surface is loaded
By anionic pollutant in the effect absorption water such as electrostatic attraction and ligand exchange, molecular sieve supercage inside passes through lanthanum to HDTMA
The effect such as the complexation Adsorption that completes to anionic pollutant in water.
In order to verify the adsorbent effect of present invention preparation, also adsorption test is carried out to it.Adsorption experiment is in tool plug cone
Carry out in shape bottle, finite concentration nitrate solution and the zeolite adsorbents of preparation are added, in being placed in constant temperature oscillation case, reaction one
After fixing time, using Suction filtration device sharp separation adsorbent and adsorbate solution, and it is used to adsorb with filter filtration fraction solution
The measure of nitrate concentration afterwards.
Further detailed complete the specific practice for illustrating and adsorption effect are done to the present invention with reference to embodiment.
Embodiment 1
1. it is standby that the mesh sieve zeolite pretreatment post-drying of a certain amount of mistake 80~200 is taken.Preprocess method is：By NaY zeolite mistake
Sieve, after washing filtering, in 400 DEG C of calcining 3h of Muffle furnace, realizes that the performance to zeolite surface is activated.
2. the NaY zeolite of 10g and the hydrated lanthanum chloride of 5g are weighed respectively, and first 10gNaY zeolites are placed in container, plus
Deionized water and stirring form suspension；Then under 25 DEG C of magnetic agitation, hydrated lanthanum chloride is added in zeolite suspension, is made
Both are sufficiently mixed and in suspended state, stir 1h.Then to the sodium hydroxide that Deca concentration in reactant liquor is 1.0mol/L
Solution, pH is adjusted to 9, continues to be separated by filtration after stirring 2h, and deionized water rinses solid to without chloride ion presence repeatedly.Dry
High-temperature activation after dry, is obtained zeolite-lanthanum.
3. 10mM cetyl trimethylammonium bromide solutions 100ml are taken in 250ml conical flask with cover, add 10g zeolites-lanthanum
Adsorbent, at 45 DEG C 24h is vibrated.After filtration washing drying, cationic surfactant modified zeolite-lanthanum composite adsorption is obtained
Agent.
4. the cationic surfactant modified zeolite-lanthanum compound adsorbent of 0.5g said methods preparation is weighed, is placed in
During 50ml concentration is for the phosphate solution of 10mg/L, solution is placed in thermostatic control oscillator vibration and vibrates 12h, concussion speed is
150rpm.Phosphate free detection (being less than test limit), i.e. experiment after experiment draws, is the phosphatic suctions of 10mg/L to initial concentration
Attached clearance nearly 100%.
Embodiment 2
1. it is standby that the mesh sieve zeolite pretreatment post-drying of a certain amount of mistake 80~200 is taken.Preprocess method is：By NaY zeolite mistake
Sieve, after washing filtering, in 400 DEG C of calcining 3h of Muffle furnace, realizes that the performance to zeolite surface is activated.
2. the NaY zeolite of 10g and the hydrated lanthanum chloride of 5g are weighed respectively, and first 10gNaY zeolites are placed in container, plus
Deionized water and stirring form suspension；Then under 25 DEG C of magnetic agitation, hydrated lanthanum chloride is added in zeolite suspension, is made
Both are sufficiently mixed and in suspended state, stir 1h.Then to the sodium hydroxide that Deca concentration in reactant liquor is 1.0mol/L
Solution, by pH 9 are adjusted to, and continue to be separated by filtration after stirring 2h, and deionized water rinses solid to without chloride ion presence repeatedly.Drying
Afterwards high-temperature activation, is obtained zeolite-lanthanum.
3. 30mM cetyl trimethylammonium bromide solutions 100ml are taken in 250ml conical flask with cover, add 10g zeolites-lanthanum
Adsorbent, at 45 DEG C 36h is vibrated.After filtration washing drying, cationic surfactant modified zeolite-lanthanum composite adsorption is obtained
Agent.
4. the cationic surfactant modified zeolite-lanthanum compound adsorbent of 0.1g said methods preparation is weighed, is placed in
During 50ml concentration is for the phosphate solution of 50mg/L, solution is placed in thermostatic control oscillator vibration and vibrates 12h, concussion speed is
150rpm.Experiment draws, be to initial concentration the phosphatic adsorbances of 50mg/L be 23.98mg/g, clearance is up to 91.25%.
Embodiment 3
1. it is standby that the mesh sieve natural clinoptilolite pretreatment post-drying of a certain amount of mistake 80~150 is taken.Preprocess method is：By day
After so clinoptilolite sieves, 1h is boiled with 1+3 hydrochloric acid, after washing filtering, in 400 DEG C of calcining 3h of Muffle furnace, realized to zeolite surface
Impurity removal and performance activation.
2. the hydrated lanthanum chloride of the pretreated natural clinoptilolite of 5g and 1g is weighed respectively, first by 5g natural clinoptilolite
Be placed in container, plus deionized water and stirring form suspension；Then under 25 DEG C of magnetic agitation, hydrated lanthanum chloride is added
In zeolite suspension, it is sufficiently mixed both and in suspended state, stirs 1h.It is then to Deca concentration in reactant liquor
The sodium hydroxide solution of 1.0mol/L, by pH 9 are adjusted to, and continue to be separated by filtration after stirring 2h, and deionized water rinses solid repeatedly
To without chloride ion presence.High-temperature activation after drying, is obtained zeolite-lanthanum.
3. 30mM cetyl trimethylammonium bromide solutions 100ml are taken in 250ml conical flask with cover, add zeolite-lanthanum to inhale
Attached dose, at 45 DEG C 24h is vibrated.After filtration washing drying, cationic surfactant modified zeolite-lanthanum compound adsorbent is obtained.
4. the cationic surfactant modified zeolite-lanthanum compound adsorbent of 0.1g said methods preparation is weighed, is placed in
During 50ml concentration is for the nitrate nitrogen solution of 50mg/L, solution is placed in thermostatic control oscillator vibration and vibrates 12h, concussion speed is
150rpm.Experiment draws, is 14.12mg/g to the adsorbance that initial concentration is 50mg/L nitrate nitrogens, and clearance reaches
56.50%.
As can be seen from the above-described embodiment, the zeolite adsorbents that the present invention is prepared are that may be present big in water
Anionic part state pollutant have preferable removal effect, extremely project especially for phosphatic eliminating rate of absorption, up near
100%.
Claims (9)
1. it is a kind of for going eliminating water in anionic pollutant new zeolite adsorbent preparation method, it is characterised in that include
Following steps：
1) zeolite for taking 2~20 mass parts through remove impurity and performance activating pretreatment is in container, plus deionized water and stirs shape
Into suspension；The hydrated lanthanum chloride of 0.5~5 mass parts is added, after stirring, pH is adjusted between 8-10 with NaOH solution, continued
After stirring at least 2h, filter and deionized water is cleaned to without Cl-Exist；After drying, high-temperature activation promotes La in zeolite supercage
Internal bonding；
2) by step 1) zeolite of acquisition after high temperature activation is placed in cationic surfactant solution, vibrates 5~72h,
Zeolite adsorbents are obtained after filtering drying.
2. preparation method as claimed in claim 1, it is characterised in that step 1) in, described zeolite is using natural oblique boiling
Stone, NaY zeolite molecular sieve or 13X zeolite molecular sieves.
3. preparation method as claimed in claim 1, it is characterised in that step 1) in, described preprocess method is：By zeolite
After sieving, 0.5~2h is boiled with 1+3 hydrochloric acid, after washing filtering, in 400 DEG C of calcining 2-5h of Muffle furnace, realized to the miscellaneous of zeolite surface
Matter is removed and performance activation.
4. preparation method as claimed in claim 1, it is characterised in that step 1) in, described sized zeolite particles are in 200~80 mesh
Between.
5. preparation method as claimed in claim 1, it is characterised in that step 1) in, the mass ratio of zeolite and added lanthanum chloride
10：1~2：Between 1.
6. preparation method as claimed in claim 1, it is characterised in that step 1) in, the concentration range of NaOH solution is 0.1~
3mol/L。
7. preparation method as claimed in claim 1, it is characterised in that step 2) in, described cationic surfactant is
Cetyl trimethylammonium bromide, cationic surfactant solution concentration range is between 10~50mM.
8. preparation method as claimed in claim 1, it is characterised in that step 2) in, hunting speed is 150~300rpm, is shaken
Temperature is swung for 20~60 DEG C.
9. a kind of zeolite adsorbents prepared such as the arbitrary methods described of claim 1~8.
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Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107213866A (en) * | 2017-06-26 | 2017-09-29 | 泉州师范学院 | A kind of preparation method and application for being used to go the zinc oxide modified zeolite adsorbing material of anionic pollutant in water removal |
| CN108905960A (en) * | 2018-07-23 | 2018-11-30 | 山东建筑大学 | A method of Cu-W ore deposit river is repaired using modified particles zeolite |
| CN110170312A (en) * | 2019-05-30 | 2019-08-27 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of ammonia nitrogen adsorbent based on Chitosan-coated SBA-15 mesopore molecular sieve and products thereof and application |
| CN111530412A (en) * | 2020-04-28 | 2020-08-14 | 北京工业大学 | Method for synthesizing synchronous denitrification and dephosphorization adsorbent based on natural zeolite |
| CN111530410A (en) * | 2020-04-28 | 2020-08-14 | 北京工业大学 | Method for preparing phosphorus removal adsorbent based on natural zeolite synthesized molecular sieve waste |
| CN112023873A (en) * | 2020-08-25 | 2020-12-04 | 广西桂林新大桂工环境科技中心(有限合伙) | Preparation method of heavy metal scavenging agent for sewage treatment |
| CN112495340A (en) * | 2020-10-20 | 2021-03-16 | 广州振清环保技术有限公司 | Preparation method of modified clinoptilolite and water body purifying agent |
| CN113185671A (en) * | 2021-05-27 | 2021-07-30 | 复旦大学 | Impurity removal and purification method for epoxy resin |
| CN114749143A (en) * | 2022-04-01 | 2022-07-15 | 北京工业大学 | Preparation method and application of natural clinoptilolite-based synchronous denitrification and dephosphorization adsorbent material |
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Cited By (12)
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| CN107213866A (en) * | 2017-06-26 | 2017-09-29 | 泉州师范学院 | A kind of preparation method and application for being used to go the zinc oxide modified zeolite adsorbing material of anionic pollutant in water removal |
| CN108905960A (en) * | 2018-07-23 | 2018-11-30 | 山东建筑大学 | A method of Cu-W ore deposit river is repaired using modified particles zeolite |
| CN108905960B (en) * | 2018-07-23 | 2021-05-18 | 山东建筑大学 | Method for repairing copper-polluted river channel by using modified granular zeolite |
| CN110170312A (en) * | 2019-05-30 | 2019-08-27 | 上海纳米技术及应用国家工程研究中心有限公司 | Preparation method of ammonia nitrogen adsorbent based on Chitosan-coated SBA-15 mesopore molecular sieve and products thereof and application |
| CN111530412A (en) * | 2020-04-28 | 2020-08-14 | 北京工业大学 | Method for synthesizing synchronous denitrification and dephosphorization adsorbent based on natural zeolite |
| CN111530410A (en) * | 2020-04-28 | 2020-08-14 | 北京工业大学 | Method for preparing phosphorus removal adsorbent based on natural zeolite synthesized molecular sieve waste |
| CN112023873A (en) * | 2020-08-25 | 2020-12-04 | 广西桂林新大桂工环境科技中心(有限合伙) | Preparation method of heavy metal scavenging agent for sewage treatment |
| CN112495340A (en) * | 2020-10-20 | 2021-03-16 | 广州振清环保技术有限公司 | Preparation method of modified clinoptilolite and water body purifying agent |
| CN113185671A (en) * | 2021-05-27 | 2021-07-30 | 复旦大学 | Impurity removal and purification method for epoxy resin |
| CN113185671B (en) * | 2021-05-27 | 2022-09-16 | 复旦大学 | Impurity removal and purification method for epoxy resin |
| CN114749143A (en) * | 2022-04-01 | 2022-07-15 | 北京工业大学 | Preparation method and application of natural clinoptilolite-based synchronous denitrification and dephosphorization adsorbent material |
| CN114749143B (en) * | 2022-04-01 | 2024-03-01 | 北京工业大学 | Preparation method and application of synchronous denitrification and dephosphorization adsorbent material based on natural clinoptilolite |
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