CN110075789A - A kind of cyanobacteria magnetic based on the modified preparation of attapulgite catches the preparation method of agent - Google Patents
A kind of cyanobacteria magnetic based on the modified preparation of attapulgite catches the preparation method of agent Download PDFInfo
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- CN110075789A CN110075789A CN201910432880.2A CN201910432880A CN110075789A CN 110075789 A CN110075789 A CN 110075789A CN 201910432880 A CN201910432880 A CN 201910432880A CN 110075789 A CN110075789 A CN 110075789A
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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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- 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
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28002—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 physical properties
- B01J20/28009—Magnetic properties
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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
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
Abstract
A kind of cyanobacteria magnetic based on the modified preparation of attapulgite catches the preparation method of agent, first, attapulgite clay mineral is mixed with inorganic acid, it stands, product is centrifuged, washing, it is dry to obtain solid 1, secondly, soluble trivalent iron salt and soluble divalent iron salt are dissolved in ethylene glycol and form solution A, by sodium hydroxide formation B solution soluble in water, again, solid 1 is sufficiently stirred with solution A, obtain solution C, finally, B solution and C solution are mixed, mixed solution cooling for reflux under certain microwave power reacts, after reacting cooling, sample is centrifuged, ethanol washing, it is dry, obtain product, the present invention is by using acidification to Concave-convex clay rod, a kind of cyanobacteria magnetic based on the modified preparation of attapulgite is synthesized by microwave-assisted mode with magnetic iron ore and catches agent, material therefor is environmental-friendly, it compares Catching agent in other magnetic, cost is relatively low, suitable for mass production, has the characteristics that simple process, fast energy-saving, Product environment are friendly.
Description
Technical field
It is the present invention relates to nanocomposite preparation technical field, in particular to a kind of that preparation is modified based on attapulgite
Cyanobacteria magnetic catches the preparation method of agent.
Background technique
With the development of science and technology, the freshwater resources utilized by the mankind increase, due to China's industrial or agricultural and urbanization
The discharge amount of the rapid development of process, sanitary sewage and industrial wastewater also increasingly increases, but carried out due to associated emission measure
It is not in place, cause a large amount of waste water unprocessed or processing is below standard is just discharged into natural water body, and contain a large amount of battalion in waste water
Substance such as nitrogen, phosphorus etc. is supported, these substances accelerate the eutrophication of water body, and water body oxygen content is reduced, cyanobacteria raised growth,
Cause water quality deterioration, exhaust water oxygen when serious and causes the death of fish.More seriously, some types in cyanobacteria
(such as Microcystis aeruginosa) can also generate Microcystin, and MCs is other than directly generating murder by poisoning to fish, people and animals and the weight of liver cancer
Want inducement.In addition, the Anabaena in cyanobacteria can quickly generate lethal factor, the gill tissue of cultivation object is destroyed, interferes it new old
Metabolism is normally carried out, and paralysis nerve makes its death.Individual kinds of not only living body band poison, and dead individuals decomposition meeting in cyanobacteria
Generate biotoxin --- cyanophycean toxin (such as Microcystin).Cyanophycean toxin amount can directly contribute cultivation object death by poisoning when more
It dies；Even if quantity is few, cultivation object can also be endangered by food chain build-up effect, until harmful to human.
The predominantly artificial fishing of the technology of the cyanobacteria of China's processing at present, mechanical algae removement, chemical algae removing, physics removes, magnetic catches ship
Except algae removal technologies such as algaes.It is artificial fishing collect means backwardness, low efficiency, costly；Mechanical algae removement can cause dirt to dirty waters
Dye, maintenance cost are high；Chemical algae removing method is palliative, easily causes secondary pollution to water body；Physics algae-removing method is also all deposited
In low efficiency, the drawbacks such as algae cannot be removed on a large scale, and apart from practical application, there are certain gaps.Since magnetic catches ship technology to large area
Except algae has the advantages such as quick, efficient, to be widely used.The core that magnetic catches ship technology is research and development that high-performance magnetism catches agent,
Currently, efficient magnetic is caught agent and is substantially more expensive, therefore the cyanobacteria processing magnetic developed efficiently, inexpensive catches agent with extensive city
Field demand and good application prospect.
Attapulgite be it is a kind of have chain layer structure aqueous rich magnesium aluminosilicate clays mineral, have bigger serface,
It the features such as light weight, porous, adsorptivity, has a wide range of applications.Acid processing is frequently used to increase the surface area of clay, to obtain
With porous and active site solid material.During attapulgite acidification, it can be removed and be distributed in by acidification
Impurity in Concave-convex clay rod duct, dredges duct, increases pore volume.Attapulgite and magnetic iron ore knot after enabling acidification
It closes, forms cyanobacteria magnetic and catch agent, be adsorbed in cyanobacteria surface, so that cyanobacteria conglomerate, point of cyanobacteria and water body is realized by magnetic force
From.
Summary of the invention
In order to overcome the disadvantages of the above prior art, the purpose of the present invention is to provide one kind based on the modified system of attapulgite
Standby cyanobacteria magnetic catches the preparation method of agent, can quickly prepare and catch agent based on the modified cyanobacteria magnetic of attapulgite, is suitable for extensive
Production has the characteristics that raw material economics, simple process, fast energy-saving, Product environment are friendly.
In order to achieve the above object, the technical scheme adopted by the invention is as follows:
A kind of cyanobacteria magnetic based on the modified preparation of attapulgite catches the preparation method of agent, and steps are as follows:
Step 1: being the inorganic acid of 5mol/L according to solid-to-liquid ratio (g/mL) 1:4 by attapulgite clay mineral and molar concentration
Mixing, stands for 24 hours, and product centrifugation, washing, drying are obtained solid 1；
Step 2: soluble trivalent iron salt and soluble divalent iron salt example (1.5-2.5): 1 are dissolved in ethylene glycol in molar ratio
Middle formation solution A, solid-to-liquid ratio 0.1-0.5g/mL；By sodium hydroxide formation B solution soluble in water, solid-to-liquid ratio 0.1-0.5g/
The molar ratio of mL, sodium hydroxide and trivalent iron salt is (4-6): 1；
Step 3: step 1 obtained solid 1 is sufficiently stirred according to solid than 0.3-5 (g/g) with gained solution A in step 2
15-30min obtains solution C；
Step 4: step 2 gained B solution and step 3 gained C solution being mixed, mixed solution is cold under certain microwave power
But back flow reaction；
Step 5: after reacting cooling, by sample centrifugation, ethanol washing, drying, obtaining product.
The content of scpiolitc is greater than 90% in the attapulgite clay mineral.
The attapulgite clay mineral is mechanically pulverized to less than 200 mesh powders.
The inorganic acid is one of hydrochloric acid, nitric acid or sulfuric acid.
The solubility trivalent iron salt is one of iron chloride, ferric nitrate, ferric sulfate.
The solubility divalent iron salt is one of frerrous chloride or ferrous sulfate.
The water is deionized water.
The inorganic acid, trivalent iron salt, divalent iron salt, ethylene glycol, sodium hydroxide, ethyl alcohol are the pure rank of analysis.
Example 2:1 is dissolved in ethylene glycol in molar ratio for the solubility trivalent iron salt and soluble divalent iron salt.
After the solution mixing of the step 4 is transferred in round-bottomed flask, it is placed in microwave chemical reactor, in 50%-
Cooling for reflux reacts under 100% microwave power, and the microwave chemical reactor frequency is 50Hz, and the microwave reaction time is
15-60 minutes.
The step 5 is dried using vacuum oven.
The present invention having the beneficial effect that compared with prior art
The present invention synthesizes one by microwave-assisted mode with magnetic iron ore by using acidification to Concave-convex clay rod
Kind catches agent based on the cyanobacteria magnetic of the modified preparation of attapulgite.It is a kind of green syt that this method, which prepares used microwave assisting method,
Method, product material therefor are environment-friendly material, and raw material is simple and easy to get, because attapulgite has biggish specific surface area, because
This product adsorption efficiency is high, and catching agent compared to other magnetic, cost is relatively low, while prepared modified based on attapulgite using method
It is suitable for mass production that preparation cyanobacteria magnetic catches agent, has the characteristics that simple process, fast energy-saving, Product environment close friend.
Specific embodiment
The present invention is described in further details below with reference to embodiment.
Embodiment 1
Step 1: the mixed in hydrochloric acid for being 5mol/L by 2.5g sepiolite clay mineral and 10ml molar concentration is stood for 24 hours, institute
The content for stating scpiolitc in attapulgite clay mineral is greater than 90%, sepiolite clay mineral mechanical crushing to less than 100
Mesh powder.By product centrifugation, washing, dry acquisition solid 1；
Step 2: by 0.27g FeCl3·6H2O (Iron(III) chloride hexahydrate) and 0.10g FeCl2·4H2O (four hydrations two
Frerrous chloride) it is dissolved in formation solution A in 10mL EG (ethylene glycol)；0.16g NaOH (sodium hydroxide) is dissolved in 1.5mL deionization
B solution is formed in water.
Step 3: 15min is sufficiently stirred in gained solution A in 0.1g step 1 obtained solid 1 and step 2, obtains solution C；
Step 4: step 2 gained B solution and step 3 gained C solution being mixed, mixed solution is transferred to 250mL round bottom
In flask, it is placed in microwave chemical reactor the cooling for reflux under 50% microwave power and reacts 15min, the microwave chemical reaction
Device frequency is 50Hz.
Step 5: after reacting cooling, sample centrifugation, ethanol wash being produced until drying in a vacuum drying oven
Product.
Embodiment 2
Step 1: the mixed in hydrochloric acid for being 5mol/L by 2.5g sepiolite clay mineral and 10ml molar concentration is stood for 24 hours, institute
The content for stating scpiolitc in attapulgite clay mineral is greater than 90%, sepiolite clay mineral mechanical crushing to less than 100
Mesh powder.By product centrifugation, washing, dry acquisition solid 1；
Step 2: by 0.27g FeCl3·6H2O (Iron(III) chloride hexahydrate) and 0.10g FeCl2·4H2O (four hydrations two
Frerrous chloride) it is dissolved in formation solution A in 10mL EG (ethylene glycol)；0.16g NaOH (sodium hydroxide) is dissolved in 1.5mL water (to go
Ionized water) in formed B solution.
Step 3: 30min is sufficiently stirred in gained solution A in 0.2g step 1 obtained solid 1 and step 2, obtains solution C；
Step 4: step 2 gained B solution and step 3 gained C solution being mixed, mixed solution is transferred to 250mL round bottom
In flask, it is placed in microwave chemical reactor the cooling for reflux under 60% microwave power and reacts 20min, the microwave chemical reaction
Device frequency is 50Hz.
Step 5: after reacting cooling, sample centrifugation, ethanol wash being produced until drying in a vacuum drying oven
Product.
Embodiment 3
Step 1: the mixed in hydrochloric acid for being 5mol/L by 2.5g sepiolite clay mineral and 10ml molar concentration is stood for 24 hours, institute
The content for stating scpiolitc in attapulgite clay mineral is greater than 90%, sepiolite clay mineral mechanical crushing to less than 100
Mesh powder.By product centrifugation, washing, dry acquisition solid 1；
Step 2: by 0.27g FeCl3·6H2O (Iron(III) chloride hexahydrate) and 0.10g FeCl2·4H2O (four hydrations two
Frerrous chloride) it is dissolved in formation solution A in 10mL EG (ethylene glycol)；0.16g NaOH (sodium hydroxide) is dissolved in 1.5mL water (to go
Ionized water) in formed B solution.
Step 3: 30min is sufficiently stirred in gained solution A in 0.3g step 1 obtained solid 1 and step 2, obtains solution C；
Step 4: step 2 gained B solution and step 3 gained C solution being mixed, mixed solution is transferred to 250mL round bottom
In flask, it is placed in microwave chemical reactor the cooling for reflux under 70% microwave power and reacts 30min, the microwave chemical reaction
Device frequency is 50Hz.
Step 5: after reacting cooling, sample centrifugation, ethanol wash being produced until drying in a vacuum drying oven
Product.
Embodiment 4
Step 1: 2.5g sepiolite clay mineral being mixed with the sulfuric acid that 10ml molar concentration is 5mol/L, are stood for 24 hours, institute
The content for stating scpiolitc in attapulgite clay mineral is greater than 90%, sepiolite clay mineral mechanical crushing to less than 100
Mesh powder.By product centrifugation, washing, dry acquisition solid 1；
Step 2: by 0.27g FeCl3·6H2O (Iron(III) chloride hexahydrate) and 0.10g FeCl2·4H2O (four hydrations two
Frerrous chloride) it is dissolved in formation solution A in 10mL EG (ethylene glycol)；0.16g NaOH (sodium hydroxide) is dissolved in 1.5mL water (to go
Ionized water) in formed B solution.
Step 3: 30min is sufficiently stirred in gained solution A in 0.2g step 1 obtained solid 1 and step 2, obtains solution C；
Step 4: step 2 gained B solution and step 3 gained C solution being mixed, mixed solution is transferred to 250mL round bottom
In flask, it is placed in microwave chemical reactor the cooling for reflux under 90% microwave power and reacts 40min, the microwave chemical reaction
Device frequency is 50Hz.
Step 5: after reacting cooling, sample centrifugation, ethanol wash being produced until drying in a vacuum drying oven
Product.
Embodiment 5
Step 1: 2.5g sepiolite clay mineral being mixed with the nitric acid that 10ml molar concentration is 5mol/L, are stood for 24 hours, institute
The content for stating scpiolitc in attapulgite clay mineral is greater than 90%, sepiolite clay mineral mechanical crushing to less than 100
Mesh powder.By product centrifugation, washing, dry acquisition solid 1；
Step 2: by 0.27g FeCl3·6H2O (Iron(III) chloride hexahydrate) and 0.10g FeCl2·4H2O (four hydrations two
Frerrous chloride) it is dissolved in formation solution A in 10mL EG (ethylene glycol)；0.16g NaOH (sodium hydroxide) is dissolved in 1.5mL water (to go
Ionized water) in formed B solution.
Step 3: 30min is sufficiently stirred in gained solution A in 0.2g step 1 obtained solid 1 and step 2, obtains solution C；
Step 4: step 2 gained B solution and step 3 gained C solution being mixed, mixed solution is transferred to 250mL round bottom
In flask, it is placed in microwave chemical reactor the cooling for reflux under 80% microwave power and reacts 50min, the microwave chemical reaction
Device frequency is 50Hz.
Step 5: after reacting cooling, sample centrifugation, ethanol wash being produced until drying in a vacuum drying oven
Product.
Embodiment 6
Step 1: the mixed in hydrochloric acid for being 5mol/L by 2.5g sepiolite clay mineral and 10ml molar concentration is stood for 24 hours, institute
The content for stating scpiolitc in attapulgite clay mineral is greater than 90%, sepiolite clay mineral mechanical crushing to less than 100
Mesh powder.By product centrifugation, washing, dry acquisition solid 1；
Step 2: by 0.27g FeCl3·6H2O (Iron(III) chloride hexahydrate) and 0.10g FeCl2·4H2O (four hydrations two
Frerrous chloride) it is dissolved in formation solution A in 10mL EG (ethylene glycol)；0.16g NaOH (sodium hydroxide) is dissolved in 1.5mL water (to go
Ionized water) in formed B solution.
Step 3: 30min is sufficiently stirred in gained solution A in 0.2g step 1 obtained solid 1 and step 2, obtains solution C；
Step 4: step 2 gained B solution and step 3 gained C solution being mixed, mixed solution is transferred to 250mL round bottom
In flask, it is placed in microwave chemical reactor the cooling for reflux under 100% microwave power and reacts 60min, the microwave chemical is anti-
Answering device frequency is 50Hz.
Step 5: after reacting cooling, sample centrifugation, ethanol wash being produced until drying in a vacuum drying oven
Product.
Claims (10)
1. the preparation method that a kind of cyanobacteria magnetic based on the modified preparation of attapulgite catches agent, which comprises the steps of:
Step 1: the inorganic acid for being 5mol/L by attapulgite clay mineral and molar concentration is mixed according to solid-to-liquid ratio (g/mL) 1:4
It closes, stands for 24 hours, product centrifugation, washing, drying are obtained into solid 1；
Step 2: soluble trivalent iron salt and soluble divalent iron salt example (1.5-2.5): 1 are dissolved in shape in ethylene glycol in molar ratio
At solution A, solid-to-liquid ratio 0.1-0.5g/mL；By sodium hydroxide formation B solution soluble in water, solid-to-liquid ratio 0.1-0.5g/mL,
The molar ratio of sodium hydroxide and trivalent iron salt is (4-6): 1；
Step 3: 15- is sufficiently stirred than 0.3-5 (g/g) according to solid in gained solution A in step 1 obtained solid 1 and step 2
30min obtains solution C；
Step 4: step 2 gained B solution and step 3 gained C solution being mixed, mixed solution cools back under certain microwave power
Stream reaction；
Step 5: after reacting cooling, by sample centrifugation, ethanol washing, drying, obtaining product.
2. a kind of cyanobacteria magnetic based on the modified preparation of attapulgite according to claim 1 catches the preparation method of agent, special
Sign is that the content of scpiolitc is greater than 90% in the sepiolite clay mineral.
3. a kind of cyanobacteria magnetic based on the modified preparation of attapulgite according to claim 1 catches the preparation method of agent, special
Sign is that the sepiolite clay mineral are mechanically pulverized to less than 100 mesh powders.
4. a kind of cyanobacteria magnetic based on the modified preparation of attapulgite according to claim 1 catches the preparation method of agent, special
Sign is that the inorganic acid is one of hydrochloric acid, nitric acid or sulfuric acid.
5. a kind of cyanobacteria magnetic based on the modified preparation of attapulgite according to claim 1 catches the preparation method of agent, special
Sign is that the solubility trivalent iron salt is one of iron chloride, ferric nitrate or ferric sulfate.
6. a kind of cyanobacteria magnetic based on the modified preparation of attapulgite according to claim 1 catches the preparation method of agent, special
Sign is that the solubility divalent iron salt is one of frerrous chloride or ferrous sulfate.
7. a kind of cyanobacteria magnetic based on the modified preparation of attapulgite according to claim 1 catches the preparation method of agent, special
Sign is that the water is deionized water.
8. a kind of cyanobacteria magnetic based on the modified preparation of attapulgite according to claim 1 catches the preparation method of agent, special
Sign is that the inorganic acid, trivalent iron salt, divalent iron salt, ethylene glycol, sodium hydroxide, ethyl alcohol are the pure rank of analysis.
9. a kind of cyanobacteria magnetic based on the modified preparation of attapulgite according to claim 1 catches the preparation method of agent, special
Sign is, after the solution mixing of the step 4 is transferred in round-bottomed flask, is placed in microwave chemical reactor, in 50%-
Cooling for reflux reacts under 100% microwave power, and the microwave chemical reactor frequency is 50Hz, and the microwave reaction time is
15-60 minutes.
10. a kind of cyanobacteria magnetic based on the modified preparation of attapulgite according to claim 1 catches the preparation method of agent, special
Sign is that the step 5 is dried using vacuum oven.
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| CN109019622A (en) * | 2018-08-09 | 2018-12-18 | 陕西科技大学 | A method of preparing clay loaded nano magnetite |
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| US20090162919A1 (en) * | 2007-12-21 | 2009-06-25 | Aurora Biofuels, Inc. | Methods for concentrating microalgae |
| CN102886252A (en) * | 2012-11-07 | 2013-01-23 | 西北师范大学 | Preparation of magnetic palygorskite clay adsorbent and application thereof in dye wastewater treating |
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