CN108249532A - A kind of preparation method and application method of the novel sink depressant prescription based on Silica clusters - Google Patents
A kind of preparation method and application method of the novel sink depressant prescription based on Silica clusters Download PDFInfo
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- CN108249532A CN108249532A CN201810030200.XA CN201810030200A CN108249532A CN 108249532 A CN108249532 A CN 108249532A CN 201810030200 A CN201810030200 A CN 201810030200A CN 108249532 A CN108249532 A CN 108249532A
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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
- C02F1/52—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities
- C02F1/5236—Treatment of water, waste water, or sewage by flocculation or precipitation of suspended impurities using inorganic agents
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/18—Preparation of finely divided silica neither in sol nor in gel form; After-treatment thereof
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/20—Silicates
- C01B33/32—Alkali metal silicates
- C01B33/325—After-treatment, e.g. purification or stabilisation of solutions, granulation; Dissolution; Obtaining solid silicate, e.g. from a solution by spray-drying, flashing off water or adding a coagulant
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/007—Contaminated open waterways, rivers, lakes or ponds
Abstract
The invention discloses a kind of preparation method and application methods of the novel sink depressant prescription based on Silica clusters, using Silica clusters object as sedimentation agent main body, utilize the strong interaction between Silica clusters object and metal ion, metal ion is made to be combined with Silica clusters object, so as to obtain the sedimentation agent of Metal Ions Modification, the metal ion residual content in water body, especially aluminium ion after handling can be reduced；The sedimentation agent of the present invention selective can be combined with cyanobacteria, substantially reduce the influence to other aquatic organisms；The density of final settlement object can be adjusted in the present invention by adjusting the degree of polymerization of Silica clusters or granular size and tenor in sedimentation agent, prepared sediment can bubble through the water column and can also sink under water, and can meet different salvaging process demands；The sedimentation agent of the present invention is faintly acid, and the living environment of cyanobacteria by way of reducing water pH value, can be also destroyed while cyanobacteria is settled, and inhibits blue algae growth.
Description
Technical field
The present invention relates to field of environment protection, and in particular to a kind of preparation of the novel sink depressant prescription based on Silica clusters
Method and application process.
Background technology
With the fast development of China's economic, environmental problem is of increasing concern.However in recent years, the pollution of freshwater lake
Problem is increasingly sharpened.7.8 ten thousand square kilometres of Chinese Lakes area, wherein 92% large and medium-sized lake tends to eutrophication.In addition, I
8.1 ten thousand square kilometres of state's aquaculture area, the problem of being also frequently present of eutrophication.The eutrophication of water body is usually associated with
The outburst of cyanobacteria, referred to as cyanobacterial bloom.
Cyanobacterial bloom seriously destroys the ecological environment of water body, and the toxin that cyanobacteria releases brings people and animals serious prestige
The side of body.It is more effective at present and widely used method to remove cyanobacteria with flocculant.Organic polymer coargulator（Such as polyacrylamide
Amine）Though significant effect, not degradable, monomer has strong neurotoxicity, therefore should limit use.Inorganic salts flocculant
（Aluminum sulfate, iron chloride, polyaluminium chloride, polyiron sulfate etc.）Treatment effect is good, is now widely used flocculant.But this
A little inorganic salts flocculants also have the disadvantage that：1) metal ion residual content is high in water body after existing flocculant process, causes
Secondary pollution, especially aluminium ion can cause stomach trouble, nephrosis and the nervous system disease.2) flocculation that existing flocculant generates
Object density is low, often swims in the water surface, therefore, in not easily collecting and the processing of the more water surface of some barriers, while a large amount of drifts
Float meeting shielded from sunlight, influences aquatic organism growth, destroys the ecological balance.3) existing flocculate is usually cluster-shaped jelly,
Non-selectivity is sticked, to being also possible to damage beneficial to aquatic organism.
Invention content
A kind of preparation method and application method of the novel sink depressant prescription based on Silica clusters of the present invention, is effectively settling
While cyanobacteria, the residual quantity of metal ion can be greatly reduced, sediment is loose, and density is adjustable, and sedimentation agent can select
Selecting property sticks cyanobacteria.
In order to achieve the above objectives, the present invention uses following technical scheme：
A kind of preparation method of the novel sink depressant prescription based on Silica clusters, using Silica clusters object as sedimentation agent master
Body using the strong interaction between Silica clusters object and metal ion, makes metal ion and Silica clusters object knot
It closes, so as to obtain the sedimentation agent of Metal Ions Modification to get to a kind of novel sink depressant prescription；
The Silica clusters object refers to silicon dioxide microparticle aqueous solution, oligomeric silicic acid salting liquid or oligomeric silicic acid solution；
The degree of polymerization or granular size of the Silica clusters object can be by standing the method tune of aging at a certain temperature
Section.
Wherein, the silicon dioxide microparticle aqueous solution is prepared using simple substance silica flour for raw material, and specific method is：
10-50g simple substance silica flours are added in 50-100mL water, are heated to 60-150 DEG C, 5-30min are stirred, in addition by 0.1-
0.5g sodium hydroxides are dissolved in 50-200mL water, which is slowly added in above-mentioned silica flour suspension, is being protected
It holds and continues under conditions of temperature to stir 5-24h, room temperature is then cooled under conditions of stirring, and stand 5-12h, then depressurized
It filters, residual solid is detached with liquid, the silica containing 20-30% in gained liquid, liquid pH value is more than 8；Gained is molten
Liquid after carrying out ion exchange with acid cation exchange resin, obtains neutral or acid two with flow rate of liquid 5-20mL/min
Silicon oxide particle solution；
The burin-in process condition of the silicon dioxide microparticle solution is 50-90 DEG C of temperature, and heat preservation stands 0.5-24h.
Wherein, the silicon dioxide microparticle aqueous solution also sodium metasilicate can be used to be made for raw material, and specific method is：
The sodium silicate solution of 5-20% is flowed through into cation exchange resin with the speed of 5-20mL/min and carries out ion exchange, gained
Solution is mixed with a certain amount of sodium metasilicate to silica/sodium oxide molybdena（SiO2/Na2O）Ratio is 50-100；
Mixed liquor is subjected to burin-in process later, aging condition is 50-90 DEG C of temperature, and heat preservation stands 0.5-24h, is cooled to room temperature
Afterwards, its pH value can be adjusted by adding in sodium hydroxide or potassium hydroxide solution.
Wherein, the preparation method of the oligomeric silicic acid salting liquid is：
By dioxide-containing silica 5-30% sodium silicate solution, by acid-exchange resin carry out ion exchange, by changing
Become the dosage of ion exchange resin, obtain different SiO2/Na2O than solution, later by the solution quickly with a certain amount of alkali
Liquid mixes；
Wherein, the lye is sodium hydroxide, potassium hydroxide, sodium metasilicate or ammonium hydroxide.
The method of the Metal Ions Modification Silica clusters is specially：The pH of Silica clusters object is first passed through into drop
Add inorganic acid alkali or adjusted by the method for ion exchange column to 2-10, it is then that a certain amount of aqueous metallic ions are fast
Speed is added in the Silica clusters object solution regulated, and 5-90min is stirred at room temperature, and forms uniform solution, then pass through
Anion exchange resin is crossed by negative valency ion remaval；
Wherein, the molar ratio of silica and metal ion is in 20-300：1；
The metal ion is manganese salt, one or more combinations in nickel salt, aluminium salt, molysite, mantoquita, zinc salt, cobalt salt.
Wherein, by the sedimentation agent of Metal Ions Modification, the property of sedimentation agent can be adjusted by the method for temperature control aging,
Distillation and concentration and burin-in process are carried out to the Silica clusters for carrying metal ion；Aging condition is 10-90 DEG C of temperature,
Heat preservation stands 0.5-24h.
Application process of the novel sink depressant prescription prepared using the method for the present invention in cyanobacterial bloom is administered, the sedimentation agent can
The waters for being directly sprayed into blue algae growth with spray appliance or the semi-finished product by sedimentation agent, i.e. Silica clusters object and metal salt
Aqueous solution stores respectively, when in use, is sprayed after on-line mixing inside spray appliance.
Application process of the novel sink depressant prescription in cyanobacterial bloom is administered, 1 tonne of water body containing cyanobacteria of processing need 50-
New take-off agent solution prepared by 1000ml.
Compared with prior art, the present invention has the following advantages：
1st, the present invention develops one kind based on Silica clusters, sedimentation agent of a small amount of metal ion for dressing agent, this hair
Bright sedimentation agent utilizes Silica clusters object（Silicon dioxide microparticle or oligomerization silicate or oligomeric silicic acid）With metal ion it
Between have strong interaction, reduce diffusion of the metal ion in water body, the metal ion residual after reduction processing in water body contains
Amount, especially aluminium ion.
2nd, sedimentation agent of the invention selective can be combined with cyanobacteria, substantially reduce the influence to other aquatic organisms.
3rd, can be contained in the present invention by adjusting the degree of polymerization of Silica clusters or granular size and metal in sedimentation agent
Amount adjusts the density of final settlement object, and prepared sediment can bubble through the water column and can also sink under water, and can meet different beat
Process demand is dragged for, reaches the high-efficiency sedimentation of cyanobacteria.
4th, sedimentation agent of the invention is faintly acid, while cyanobacteria is settled also can by way of reducing water pH value,
The living environment of cyanobacteria is destroyed, inhibits blue algae growth, the cyanobacteria wrapped up by sedimentation agent, the degree of stick to each other is small, loose as husky
Sedimentation, other attached aquatic organisms will not be twined, reduce the influence to other aquatic organisms.
Description of the drawings
Fig. 1 implements water body aluminium content comparison diagram after 2 sedimentation agent of business flocculant and embodiment；Wherein, curve is to be tried with aluminium
After agent combines, the UV-vis absorbances of aluminium complex in water body；
Fig. 2（a）Business flocculant and sedimentation agent effect of settling comparison diagram of the present invention；It is followed successively by from left to right：Untreated cyanobacteria
Water body, with the water body after business flocculant process, water body after being handled with sedimentation agent of the present invention；
（b）By adjusting the property of sedimentation agent, sediment can be made, which to be sunken to the bottom, to bubble through the water column；
The sedimentation schematic diagram of Fig. 3 sedimentation agents of the present invention.
Specific embodiment
Elaborate below to embodiment provided by the invention, but these embodiments be only it is exemplary, it is not right
The scope of the present invention forms any restrictions.It will be understood by those skilled in the art that such as to the details of technical solution of the present invention
The reasonable modifications or substitutions carried out with form, each fall in protection scope of the present invention.
Embodiment 1
A kind of preparation method of the novel sink depressant prescription based on Silica clusters, using Silica clusters object as sedimentation agent master
Body, using the strong interaction between Silica clusters object and metal ion, by aqueous metal salt and Silica clusters
The aqueous solution of object is sufficiently mixed, and obtains the uniform solution of sedimentation agent of metal salt modification to get to a kind of novel sink depressant prescription；
The Silica clusters object uses silicon dioxide microparticle aqueous solution；
The density or size of the Silica clusters object are adjustable, can be adjusted by standing the method for aging at a certain temperature
Its degree of polymerization, so as to adjust its density or size.
It is as follows：
（1）The preparation of silicon dioxide microparticle aqueous solution：
50g simple substance silica flours are added in 100mL water, are heated to 98 DEG C, 30min is stirred, is in addition dissolved in 0.4g sodium hydroxides
In 200mL water, which is slowly added in above-mentioned silica flour suspension, continues to stir under conditions of temperature is kept
Then 20h is cooled to room temperature under conditions of stirring, and stands 12h, then decompression filters, and residual solid is detached with liquid,
Silica containing 20-30% in gained liquid, liquid pH value are more than 8；Acquired solution is with flow rate of liquid 10mL/min, with acid
Property cation exchange resin carry out ion exchange after, obtain weakly acidic silicon dioxide microparticle solution；
Later by obtained silicon dioxide microparticle solution in 80 DEG C of temperature, heat preservation is stood for 24 hours, carries out burin-in process.
（2）Silica clusters object is modified with iron ion：
By the method for ion exchange column or it is directly added into acid（Such as hydrochloric acid）Or alkali（Such as sodium hydroxide）Method, by dioxy
The pH of SiClx cluster object is adjusted to 7.5, then by iron chloride（FeCl3）Aqueous solution is rapidly added the Silica clusters regulated
In object solution, and 5-90min is stirred at room temperature, forms the solution of transparent and homogeneous.Wherein silica and iron chloride（SiO2/
FeCl3）Mass ratio between 10-80, finally using anion exchange resin by chlorion（Cl-）Removal；
Distillation and concentration and burin-in process will be carried out by the Silica clusters of iron ion modification；Aging condition is temperature 50 C,
Heat preservation stands 10h..Aluminium ion is free of in the iron content sedimentation agent.
Embodiment 2
A kind of preparation method of the novel sink depressant prescription based on Silica clusters, using Silica clusters object as sedimentation agent master
Body, using the strong interaction between Silica clusters object and metal ion, by aqueous metal salt and Silica clusters
The aqueous solution of object is sufficiently mixed, and obtains the uniform solution of sedimentation agent of metal salt modification to get to a kind of novel sink depressant prescription；
The Silica clusters object uses silicon dioxide microparticle aqueous solution；
The density of the Silica clusters object is adjustable, can adjust its polymerization by standing the method for aging at a certain temperature
Degree, so as to adjust its density size.
It is as follows：
（1）The preparation of silicon dioxide microparticle aqueous solution：
50g simple substance silica flours are added in 100mL water, are heated to 98 DEG C, 30min is stirred, is in addition dissolved in 0.4g sodium hydroxides
In 200mL water, which is slowly added in above-mentioned silica flour suspension, continues to stir under conditions of temperature is kept
Then 20h is cooled to room temperature under conditions of stirring, and stands 12h, then decompression filters, and residual solid is detached with liquid,
Silica containing 20-30% in gained liquid, liquid pH value are more than 8；Acquired solution is with flow rate of liquid 10mL/min, with acid
Property cation exchange resin carry out ion exchange after, obtain weakly acidic silicon dioxide microparticle solution；
Later by obtained silicon dioxide microparticle solution in temperature 50 C, heat preservation stands 5h, carries out burin-in process.
（2）Silica clusters object is modified with aluminium ion：
The pH of Silica clusters object is adjusted to 2-4, then by aluminium chloride by the method for ion exchange column（AlCl3）It is water-soluble
Liquid is rapidly added in the Silica clusters object solution regulated, and 5-90min is stirred at room temperature, and forms the molten of transparent and homogeneous
The suspension of liquid or stable homogeneous.Wherein silica and aluminium chloride（SiO2/ AlCl3）Mass ratio between 10-80, most
Afterwards using anion exchange resin by chlorion（Cl-）Removal；
Distillation and concentration and burin-in process will be carried out by the Silica clusters of aluminium ion modification；Aging condition is temperature 50 C,
Heat preservation stands 8h.
Embodiment 3
A kind of preparation method of the novel sink depressant prescription based on Silica clusters, using Silica clusters object as sedimentation agent master
Body, using the strong interaction between Silica clusters object and metal ion, by aqueous metal salt and Silica clusters
The aqueous solution of object is sufficiently mixed, and obtains the uniform solution of sedimentation agent of metal salt modification to get to a kind of novel sink depressant prescription；
The Silica clusters object uses silicon dioxide microparticle aqueous solution；
The density of the Silica clusters object is adjustable, can adjust its polymerization by standing the method for aging at a certain temperature
Degree, so as to adjust its density size.
It is as follows：
（1）The preparation of silicon dioxide microparticle aqueous solution：
50g simple substance silica flours are added in 100mL water, are heated to 98 DEG C, 30min is stirred, is in addition dissolved in 0.4g sodium hydroxides
In 200mL water, which is slowly added in above-mentioned silica flour suspension, continues to stir under conditions of temperature is kept
Then 20h is cooled to room temperature under conditions of stirring, and stands 12h, then decompression filters, and residual solid is detached with liquid,
Silica containing 20-30% in gained liquid, liquid pH value are more than 8；Acquired solution is with flow rate of liquid 10mL/min, with acid
Property cation exchange resin carry out ion exchange after, obtain weakly acidic silicon dioxide microparticle solution；
Later by obtained silicon dioxide microparticle solution in temperature 50 C, heat preservation stands 5h, carries out burin-in process.
（2）Silica clusters object is modified with iron ion：
The pH of Silica clusters object is adjusted to 7.5, then by iron chloride by the method for ion exchange column（FeCl3）It is water-soluble
Liquid is rapidly added in the Silica clusters object solution regulated, and 5-90min is stirred at room temperature, and forms the molten of transparent and homogeneous
Liquid.Wherein silica and iron chloride（SiO2/FeCl3）Mass ratio between 10-80, finally using anion exchange tree
Fat is by chlorion（Cl-）Removal；
Distillation and concentration and burin-in process will be carried out by the Silica clusters of iron ion modification；Aging condition is temperature 50 C,
Heat preservation stands 8h.
After handling cyanobacteria water body with the iron content sedimentation agent, other ions are free of in water body in addition to a small amount of iron ion.
After being implemented using business flocculant and 2 sedimentation agent containing aluminium of the embodiment of the present invention to containing cyanobacteria water body, to aluminium in water body
Content is measured comparison, the result is shown in Figure 1.
As seen from the figure due to aluminium content height in water body after the use of business flocculant, and absorbance is also high.Plasma
Emission spectrum（ICP）Test shows that the introduced aluminium composition of sedimentation agent of the present invention only has commercial 1/2.
Claims (8)
1. a kind of preparation method of the novel sink depressant prescription based on Silica clusters, which is characterized in that with Silica clusters object
As sedimentation agent main body, using the strong interaction between Silica clusters object and metal ion, make metal ion and dioxy
SiClx cluster object combines, so as to obtain the sedimentation agent of Metal Ions Modification to get to a kind of novel sink depressant prescription；
The Silica clusters object refers to silicon dioxide microparticle aqueous solution, oligomeric silicic acid salting liquid or oligomeric silicic acid solution；
The degree of polymerization or granular size of the Silica clusters object can be by standing the method tune of aging at a certain temperature
Section.
2. a kind of preparation method of novel sink depressant prescription based on Silica clusters according to claim 1, feature exist
In the silicon dioxide microparticle aqueous solution is prepared using simple substance silica flour for raw material, and specific method is：
10-50g simple substance silica flours are added in 50-100mL water, are heated to 60-150 DEG C, 5-30min are stirred, in addition by 0.1-
0.5g sodium hydroxides are dissolved in 50-200mL water, which is slowly added in above-mentioned silica flour suspension, is being protected
It holds and continues under conditions of temperature to stir 5-24h, room temperature is then cooled under conditions of stirring, and stand 5-12h, then depressurized
It filters, residual solid is detached with liquid, the silica containing 20-30% in gained liquid, liquid pH value is more than 8；Gained is molten
Liquid after carrying out ion exchange with acid cation exchange resin, obtains neutral or acid two with flow rate of liquid 5-20mL/min
Silicon oxide particle solution；
The burin-in process condition of the silicon dioxide microparticle solution is 50-90 DEG C of temperature, and heat preservation stands 0.5-24h.
3. a kind of preparation method of novel sink depressant prescription based on Silica clusters according to claim 1, feature exist
In the silicon dioxide microparticle aqueous solution also sodium metasilicate can be used to be made for raw material, and specific method is：
The sodium silicate solution of 5-20% is flowed through into cation exchange resin with the speed of 5-20mL/min and carries out ion exchange, gained
Solution is mixed with a certain amount of sodium metasilicate to silica/sodium oxide molybdena（SiO2/Na2O）Ratio is 50-100；
Mixed liquor is subjected to burin-in process later, aging condition is 50-90 DEG C of temperature, and heat preservation stands 0.5-24h, is cooled to room temperature
Afterwards, its pH value can be adjusted by adding in sodium hydroxide or potassium hydroxide solution.
4. a kind of preparation method of novel sink depressant prescription based on Silica clusters according to claim 1, feature exist
In the preparation method of the oligomeric silicic acid salting liquid is：
By dioxide-containing silica 5-30% sodium silicate solution, by acid-exchange resin carry out ion exchange, by changing
Become the dosage of ion exchange resin, obtain different SiO2/Na2O than solution, later by the solution quickly with a certain amount of alkali
Liquid mixes；
The lye is sodium hydroxide, potassium hydroxide, sodium metasilicate or ammonium hydroxide.
5. a kind of preparation method of novel sink depressant prescription based on Silica clusters according to claim 1, feature exist
In the method for the Metal Ions Modification Silica clusters is specially：First by the pH of Silica clusters object by the way that nothing is added dropwise
Machine soda acid is adjusted by the method for ion exchange column to 2-10, is then added a certain amount of aqueous metallic ions rapidly
Enter in the Silica clusters object solution regulated, and 5-90min is stirred at room temperature, uniform solution is formed, using the moon
Ion exchange resin is by negative valency ion remaval；
Wherein, the molar ratio of silica and metal ion is in 20-300：1；
The metal ion is manganese salt, one or more combinations in nickel salt, aluminium salt, molysite, mantoquita, zinc salt, cobalt salt.
6. a kind of preparation method of novel sink depressant prescription based on Silica clusters according to claim 5, feature exist
In by the sedimentation agent of Metal Ions Modification, the property of sedimentation agent being adjusted by the method for temperature control aging, i.e., to carrying gold
The Silica clusters for belonging to ion carry out distillation and concentration and burin-in process；Aging condition is 10-90 DEG C of temperature, and heat preservation is stood
0.5-24h。
7. application side of the novel sink depressant prescription that the preparation method as described in claim 1-5 is any obtains in cyanobacterial bloom is administered
Method, which is characterized in that the sedimentation agent can directly with spray appliance be sprayed into blue algae growth waters or by the half of sedimentation agent into
Product, i.e. Silica clusters object and metal ion, store respectively, when in use, are sprayed after on-line mixing inside spray appliance.
8. the application process of a kind of novel sink depressant prescription according to claim 7, which is characterized in that 1 tonne of processing contains cyanobacteria
Water body need 50-1000ml prepare new take-off agent solution.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113304507A (en) * | 2021-06-03 | 2021-08-27 | 黄铭 | The separation of the molecular clusters in the solution realizes the enrichment and separation of different substances |
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| CN113304507A (en) * | 2021-06-03 | 2021-08-27 | 黄铭 | The separation of the molecular clusters in the solution realizes the enrichment and separation of different substances |
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