CN107362776A - The composite modified clay of a kind of sulfobetaines and inorganic salts, preparation method and applications - Google Patents
The composite modified clay of a kind of sulfobetaines and inorganic salts, preparation method and applications Download PDFInfo
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- CN107362776A CN107362776A CN201710678969.8A CN201710678969A CN107362776A CN 107362776 A CN107362776 A CN 107362776A CN 201710678969 A CN201710678969 A CN 201710678969A CN 107362776 A CN107362776 A CN 107362776A
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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
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
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- 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
- B01J20/12—Naturally occurring clays or bleaching earth
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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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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/10—Inorganic compounds
- C02F2101/105—Phosphorus compounds
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Abstract
The invention provides a kind of sulfobetaines and the composite modified clay of inorganic salts, preparation method and applications, compared with prior art, the present invention carries out organic-pillared modification using sulfobetaines to clay mineral, clay specific surface area can be obviously improved and improve subsequent metal ion decentralization on the surface and utilization rate, again with inorganic metal salt modification, a large amount of Phosphateadsorption sites can be provided in clay surface, so that the adsorbent has higher adsorption capacity.For clearance up to more than 99%, the phosphorus concentration after processing can be reduced to below 0.02mg/L, reach national surface water I class water bodys standard requirement in the water sample that phosphorus concentration is 2mg/L.Moreover, water body pH significant change will not be caused in use, water ecology will not be damaged, be particularly advantageous to use in natural water body.Preparation method is easy, and three wastes produce, and is advantageous to industrialization large-scale production.
Description
Technical field
The invention belongs to water-treatment technology field, and in particular to the composite modified clay of a kind of sulfobetaines and inorganic salts,
Preparation method and applications.
Background technology
With the increase of population, the growth of industrial and agricultural production, a large amount of uses of phosphorous agricultural chemicals box agricultural fertilizer, make the phosphorus of water body dirty
Contaminate getting worse.Body eutrophication caused by phosphorus content is too high has turned into the environmental problem of whole world facing.
At present, conventional chemical precipitation method, ion-exchange, bioanalysis dephosphorization both at home and abroad, or can caused by mud amount it is big,
Secondary pollution is easily caused, either price is higher or removal effect is unstable, is not suitable for the removal of low phosphorus.Phase
Compared with above method, absorption method is due to floor space is small, technique is simple and convenient to operate, especially suitable for handling low concentration
The features such as sewage and as one of focus of Recent study.
Clay mineral has the characteristics that the absorption that specific surface area is big, good and ion-exchange performance, rich reserves, inexpensive,
It is one of ideal material of phosphorus adsorbent.By being modified to clay mineral, its phosphor-removing effect can be increased substantially.China
It is raw material that patent CN104923151A disclosed one kind on the 23rd with attapulgite in September in 2015, through potassium hydroxide high-temperature process
The phosphorus adsorbent obtained afterwards using the secondary remodeling of aluminium polychloride, to phosphatic clearance in 30mg/L solution up to 96%.
But this method produces a large amount of strong basicity waste liquids during preparing, while the material handled through highly basic can cause pH bright in use
Aobvious rise, changes water body environment.Chinese patent CN101264955 September in 2008 disclose within 17th it is a kind of using bentonite as
Raw material, first the whip modified in lanthanum salt solution, adds inorganic polymer flocculant mixing, filtered.Drying, crush system
Dephosphorization water purification agent, to the clearance of phosphate radical up to 98% in 2mg/L solution containing phosphates.But during prepared by this method
A large amount of waste water, which can be produced, to be needed to handle, and adds cost.
The content of the invention
It is an object of the invention to provide a kind of sulfobetaines and the composite modified clay of inorganic salts and preparation method thereof, with
Clay mineral is matrix, preprocessed, sulfobetaines is organically-modified, metal salt is inorganic modified is prepared, and product compares surface
Accumulate up to 200~550m2/g。
Present invention also offers the application of a kind of sulfobetaines and the composite modified clay of inorganic salts, for total phosphorus concentration compared with
The advanced treating of low waste water.
A kind of preparation method of the composite modified clay of sulfobetaines and inorganic salts provided by the invention, including following step
Suddenly：
1) pre-process:Clay mineral grinding sieving, is preserved after roasting in dry environment；
2) sulfobetaines is organically-modified：Clay mineral regulation pH to 5-6 after step 1) processing, adds sulfobetaines
Alkali modification；
3) inorganic metal salt is modified：The modified clay mineral of step 2) and inorganic metal salt are mixed and modified, you can.
Further, step 1) the ground sieve is specially：200-400 mesh sieves are crossed after grinding.
Step 1) the clay mineral is the mixing of one or both of attapulgite, bentonite or sepiolite；Pretreatment
The specific surface area of clay mineral afterwards is 150-450m2/g。
Roasting described in step 1) refers to 250-600 DEG C of roasting 3-5h.
Step 2) is specially：
Add water to the clay mineral after step 1) processing, stir, adjust pH to 5-6, add sulfobetaines, stir
Dried after mixing, you can.
Further, the mass ratio of the clay mineral in step 2) after step 1) processing used, water and sulfobetaines is
100：80-100：3-15.
Sulfobetaines described in step 2) is dodecyl sulfobetaine, cocamidopropyl propyl amide hydroxyl sulfobetaines
One kind in alkali, dodecanamide propyl hydroxy sulfo lycine or octadecyldimethyl azochlorosulfonate propyl lycine；It is preferred that octadecyl
Dimethyl sulfopropyl betaine.
Further, regulation pH agents useful for same is 0.5-2mol/L dilute sulfuric acids in step 2)；
Stirred specially described in step 2)：0.5-2h is stirred in 30-80 DEG C of water bath with thermostatic control.
Drying refers to 80-105 DEG C of dry 6-8h described in step 2).
Step 3) is specially：
By weight, 2-10 parts inorganic metal salt clay modified with step 2) is stirred, adds 80-100
Part water, heating stirring is uniform, re-dry, grinding sieving, finished product.
The metal cation of inorganic metal salt described in step 3) is selected from Fe2+、Al3+、Ca2+Or Mg2+Any one；It is described
The anion of inorganic metal salt is selected from SO4 2-、NO3 -Or Cl-In one kind；The inorganic metal salt is selected from above-mentioned inorganic metal salt
It is any one or several.
Heating stirring described in step 3) uniformly refers to stir 0.5-2h in 30-80 DEG C of water bath with thermostatic control.
Dried described in step 3) and refer to dry 6-8h in 80-105 DEG C of baking oven；
After step 3) the grinding sieving refers to grinding, 200-400 mesh sieves, finished product are crossed.
A kind of composite modified clay of sulfobetaines and inorganic salts of the offer of the present invention, is prepared into using the above method
Arrive, the composite modified clay specific surface area of sulfobetaines and inorganic salts of preparation is 200-550m2/g。
A kind of composite modified clay of sulfobetaines and inorganic salts provided by the invention is used for adsorbed water body as adsorbent
The application of middle low phosphorus.Described low phosphorus refers to that phosphorus concentration is less than 5mg/L.
Compared with prior art, the present invention carries out organic-pillared modification using sulfobetaines to clay mineral, can be notable
Lifting clay specific surface area simultaneously improves subsequent metal ion decentralization on the surface and utilization rate, then is modified with inorganic metal salt
Processing, a large amount of Phosphateadsorption sites can be provided in clay surface, so that the adsorbent has higher adsorption capacity.
In modifying process, pH to 5-6 is adjusted, glycine betaine is amphoteric surfactant, in acid condition, positively charged, is advantageous to and sticks
Cation in soil swaps.Using sulphur acid for adjusting pH, on the one hand because in common acid, HCl use can cause to use
Chlorine ion concentration increases in Shi Shuiti and many hardwares of Cl ion pairs have corrosiveness, HNO3Use then can be in the later stage
Brown fume pollution environment is produced in drying process, another aspect sulfuric acid is cheap, reduces cost.
The product of preparation is in 2mg/L phosphorus solutions, and adsorption capacity is up to 19.7mg/g.Sulfobetaines prepared by the present invention
And the composite modified clay dephosphorization agent of inorganic salts to the waste water containing total phosphorus concentration relatively low (being less than 5mg/L) especially suitable for carrying out depth
Processing.Up to more than 99%, the phosphorus concentration after processing can be reduced to clearance in the water sample that phosphorus concentration is 2mg/L
Below 0.02mg/L, reach national surface water I class water bodys standard requirement.Moreover, it will not cause water body pH's in use
Significant change, water ecology will not be damaged, be particularly advantageous to use in natural water body.Preparation method is easy, without three
It is useless to produce, be advantageous to industrialization large-scale production.
Embodiment
With reference to embodiment, the embodiment of the present invention is described in further detail.
Embodiment 1
A kind of preparation method of the composite modified clay of sulfobetaines and inorganic salts, comprises the following steps：
(1) pre-process:Attapulgite grinds and crosses 200 mesh sieves, in 600 DEG C of kiln kiln roasting 2h, in feed bin kept dry
It is standby；
(2) sulfobetaines is organically-modified：100 parts of pretreated attapulgites are weighed by weight, are added 80 parts of water, are stirred
Mix uniformly, add 1mol/L dilute sulfuric acids regulation pH to 5-6,3 parts of dodecyl sulfobetaines are added, in 30 DEG C of waters bath with thermostatic control
Middle stirring 2h, then 8h is dried in 80 DEG C of baking ovens；
(3) inorganic salt modification：2 parts of calcium chloride are weighed by weight, are stirred with the organically-modified attapulgite after being dried in (2)
Mixing is mixed, adds 80 parts of water, 1h is stirred in 30 DEG C of waters bath with thermostatic control, then 8h, ground 200 mesh are dried in 80 DEG C of baking ovens
Sieve, finished product.
A kind of composite modified clay of sulfobetaines and inorganic salts is used for low phosphorus in adsorbed water body as adsorbent
Using：
Absorption effect of the composite modified clay dephosphorization agent of prepared sulfobetaines and inorganic salts in 2mg/L solution containing phosphates
Fruit is detected by Staticadsorption experiment, is specially：Weigh appropriate dried potassium dihydrogen phosphate and prepare the water that phosphorus concentration is 5mg/L
Sample, adjusted with 1mol/L NaOH solutions to pH=6.5.The organic-inorganic for weighing the water depth dephosphorization of 0.5g preparations respectively changes
Property clay mineral adsorbent add in 1L 2mg/L phosphorous water sample, the concussion absorption 4h in 25 DEG C of waters bath with thermostatic control, take after standing
Sample, filtering, pH meter measure solution ph, and using the phosphorus concentration in even magnificent water quality fast detector detection water sample, and calculate phosphorus
Clearance.Filtering retains solid, is added into the 1L 2mg/L newly configured phosphorous water sample, is shaken in 25 DEG C of waters bath with thermostatic control
Adsorb 4h, sampling and testing.Above step is repeated, until material adsorption saturation, so as to which material be calculated in 2mg/L phosphorus solutions
Adsorption capacity.
After testing, the specific surface area of the attapulgite after roasting is 178m2/ g, and it is modified through organic-inorganic, material
Specific surface area increases to 226m2/g.After the phosphorous water samples of material process 2mg/L, the pH of solution is 6.2, tp removal rate 99.2%,
Adsorption capacity is 10.1mg/g.
Embodiment 2
A kind of preparation method of the composite modified clay of sulfobetaines and inorganic salts, comprises the following steps：
(1) pre-process:Attapulgite grinds and crosses 200 mesh sieves, is calcined 2h in 600 DEG C of kilns, is preserved in drying in feed bin
It is standby；Bentonite grinds and crosses 200 mesh sieves, is calcined 3h in 450 DEG C of kilns, is saved backup in drying in feed bin.
(2) sulfobetaines is organically-modified：After weighing 60 parts of pretreated attapulgites and 40 parts of pretreatments by weight
Bentonite mixing, add 90 parts of water, stir, add 0.5mol/L dilute sulfuric acids regulation pH to 5-6, add 8 portions of cocounut oil
Amido propyl hydroxy sulfo lycine, 1h is stirred in 40 DEG C of waters bath with thermostatic control, then 8h is dried in 80 DEG C of baking ovens；
(3) inorganic salt modification：5 parts of magnesium nitrates are weighed by weight, are stirred with the organically-modified attapulgite of drying in (2)
Mixing, adds 90 parts of water, and 1h is stirred in 40 DEG C of waters bath with thermostatic control, then 8h is dried in 80 DEG C of baking ovens, ground 200 mesh sieve,
Finished product.
A kind of composite modified clay of sulfobetaines and inorganic salts is used for low phosphorus in adsorbed water body as adsorbent
Using：Specifically with embodiment 1.
After testing, the specific surface area of material is 152m after roasting mixing2/ g, and, the ratio of material modified through organic-inorganic
Surface area increases to 246m2/g.After the phosphorous water samples of material process 2mg/L, the pH of solution is 6.1, tp removal rate 99.5%, is inhaled
Attached capacity is 13.6mg/g.
Embodiment 3
A kind of preparation method of the composite modified clay of sulfobetaines and inorganic salts, comprises the following steps：
(1) pre-process:Attapulgite grinds and crosses 200 mesh sieves, is calcined 3h in 600 DEG C of kilns, is preserved in drying in feed bin
It is standby；Sepiolite grinds and crosses 200 mesh sieves, is calcined 3h in 250 DEG C of high temperature ovens, is saved backup in drying in feed bin.
(2) sulfobetaines is organically-modified：After weighing 50 parts of pretreated attapulgites and 50 parts of pretreatments by weight
Sepiolite mixing, add 100 parts of water, stir, add 1mol/L dilute sulfuric acids regulation pH to 5-6, add 12 portions of bays
Amido propyl hydroxy sulfo lycine, 0.5h is stirred in 60 DEG C of waters bath with thermostatic control, then 6h is dried in 105 DEG C of baking ovens；
(3) inorganic salt modification：4 parts of ferric sulfate and 2 parts of aluminum sulfate are weighed by weight, it is organically-modified with being dried in (2)
Attapulgite is stirred, and adds 100 parts of water, 0.5h is stirred in 60 DEG C of waters bath with thermostatic control, then dried in 105 DEG C of baking ovens
6h, ground 200 mesh sieve, finished product.
A kind of composite modified clay of sulfobetaines and inorganic salts is used for low phosphorus in adsorbed water body as adsorbent
Using：Specifically with embodiment 1.
After testing, the specific surface area of material is 326m after roasting mixing2/ g, and, the ratio of material modified through organic-inorganic
Surface area increases to 395m2/g.After the phosphorous water samples of material process 2mg/L, the pH of solution is 6.1, tp removal rate 99.8%, is inhaled
Attached capacity is 15.2mg/g.
Embodiment 4
A kind of preparation method of the composite modified clay of sulfobetaines and inorganic salts, comprises the following steps：
(1) pre-process:Bentonite is ground and crosses 200 mesh sieves, and 3h is calcined in 450 DEG C of kilns, is preserved in dry feed bin standby
With；Sepiolite grinds and crosses 200 mesh sieves, is calcined 3h in 250 DEG C of high temperature ovens, is saved backup in drying in feed bin.
(2) sulfobetaines is organically-modified：20 parts of pretreated bentonites are weighed by weight and 80 parts pretreated
Sepiolite mixes, and adds 100 parts of water, stirs, and adds 2mol/L dilute sulfuric acids regulation pH to 5-6, adds 15 parts of octadecanes
Base dimethyl sulfopropyl betaine, 0.5h is stirred in 80 DEG C of waters bath with thermostatic control, then 6h is dried in 105 DEG C of baking ovens；
(3) inorganic salt modification：5 parts of ferrous sulfate and 5 parts of alchlors are weighed by weight, it is organic with being dried in (2)
It is attapulgite modified to be stirred, 100 parts of water are added, 0.5h are stirred in 80 DEG C of waters bath with thermostatic control, then done in 105 DEG C of baking ovens
Dry 6h, ground 200 mesh sieve, finished product.
A kind of composite modified clay of sulfobetaines and inorganic salts is used for low phosphorus in adsorbed water body as adsorbent
Using：Specifically with embodiment 1.
After testing, the specific surface area of material is 448m after roasting mixing2/ g, and, the ratio of material modified through organic-inorganic
Surface area increases to 537m2/g.After the phosphorous water samples of material process 2mg/L, the pH of solution is 6.0, tp removal rate 99.9%, is inhaled
Attached capacity is 19.7mg/g.
The preferred embodiments of the present invention are the foregoing is only, are not intended to limit the invention, the present invention there can be various change
Become；Any modification for being made within the spirit and principles of the invention, improvement etc., equivalent substitution；As long as satisfaction uses needs,
It should be included in the scope of the protection.
Claims (10)
- A kind of 1. preparation method of sulfobetaines and the composite modified clay of inorganic salts, it is characterised in that the preparation method bag Include following steps：1) pre-process:Clay mineral grinding sieving, is preserved after roasting in dry environment；2) sulfobetaines is organically-modified：Clay mineral regulation pH to 5-6 after step 1) processing, adds sulfobetaines and changes Property；3) inorganic metal salt is modified：The modified clay mineral of step 2) and inorganic metal salt are mixed and modified, you can.
- 2. preparation method according to claim 1, it is characterised in that the step 1) clay mineral is attapulgite, swollen The mixing of one or both of profit soil or sepiolite；The specific surface area of pretreated clay mineral is 150-450m2/g。
- 3. preparation method according to claim 1 or 2, it is characterised in that roasting refers to 250-600 DEG C described in step 1) It is calcined 3-5h.
- 4. preparation method according to claim 1 or 2, it is characterised in that step 2) is specially：Add water to the clay mineral after step 1) processing, stir, adjust pH to 5-6, sulfobetaines is added, after stirring Dry, you can.
- 5. preparation method according to claim 4, it is characterised in that the clay ore deposit in step 2) after step 1) processing used The mass ratio of thing, water and sulfobetaines is 100：80-100：3-15.
- 6. according to the preparation method described in claim any one of 1-5, it is characterised in that the sulfobetaines described in step 2) For dodecyl sulfobetaine, cocamidopropyl propyl amide hydroxy sulfo lycine, dodecanamide propyl hydroxy sulfo lycine or 18 One kind in alkyl dimethyl azochlorosulfonate propyl lycine.
- 7. according to the preparation method described in claim any one of 1-6, it is characterised in that step 3) is specially：By weight, will 2-10 parts inorganic metal salt clay modified with step 2) is stirred, and adds 80-100 part water, and heating stirring is uniform, then Dry, grinding sieving, finished product.
- 8. according to the preparation method described in claim any one of 1-7, it is characterised in that inorganic metal salt described in step 3) Metal cation is selected from Fe2+、Al3+、Ca2+Or Mg2+Any one；The anion of the inorganic metal salt is selected from SO4 2-、NO3 -Or Cl-In one kind；It is any one or several that the inorganic metal salt is selected from above-mentioned inorganic metal salt.
- 9. sulfobetaines and the composite modified clay of inorganic salts prepared by a kind of any one of claim 1-8 methods described, it is special Sign is that sulfobetaines and the composite modified clay specific surface area of inorganic salts are 200-550m2/g。
- 10. the application of the composite modified clay of sulfobetaines and inorganic salts described in a kind of claim 9, it is characterised in that use The application of low phosphorus in adsorbed water body.
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| CN112044393A (en) * | 2019-06-06 | 2020-12-08 | 中南大学 | Two-dimensional clay-based composite phosphorus removal agent and preparation method and application thereof |
| CN115536118A (en) * | 2022-10-09 | 2022-12-30 | 陕西水研环境科技研究院有限公司 | Sewage treatment flocculant and preparation method and application thereof |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112044393A (en) * | 2019-06-06 | 2020-12-08 | 中南大学 | Two-dimensional clay-based composite phosphorus removal agent and preparation method and application thereof |
| CN112044393B (en) * | 2019-06-06 | 2021-05-04 | 中南大学 | Two-dimensional clay-based composite phosphorus removal agent and preparation method and application thereof |
| CN111468073A (en) * | 2020-04-03 | 2020-07-31 | 江南大学 | Dephosphorization reagent for air floatation and preparation method thereof |
| CN111468073B (en) * | 2020-04-03 | 2021-06-25 | 江南大学 | Dephosphorization reagent for air floatation and preparation method thereof |
| CN115536118A (en) * | 2022-10-09 | 2022-12-30 | 陕西水研环境科技研究院有限公司 | Sewage treatment flocculant and preparation method and application thereof |
| CN115536118B (en) * | 2022-10-09 | 2024-04-12 | 陕西水研环境科技研究院有限公司 | Sewage treatment flocculant and preparation method and application thereof |
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