CN110437839A - A kind of graphene quantum dot soil-solidified-agent preparation method - Google Patents
A kind of graphene quantum dot soil-solidified-agent preparation method Download PDFInfo
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Abstract
The invention discloses a kind of graphene quantum dot soil-solidified-agent preparation methods, it is different with domestic and international soil-solidified-agent, first by polymer graphite alkene quantum dot solution, polymer graphite alkene quantum dot inflation fluid, polymer graphite alkene quantum dot surface activity liquid, pass through thermal response, centrifugal treating, ultrasonic treatment, dialysis treatment, after being freeze-dried milled processed, a kind of solidification intensity obtained is high, it is few to solidify dosage, quick construction, environmentally protective new polymers graphene quantum dot curing agent, addition suitable for various concrete materials solidifies and the solidification of subgrade soil, and for tailing backfill solidification, building waste secondary curing, lake silt solidification, oil field sludge solidification, road construction solidification, building construction solidification, port construction solidification, the new soil polymer graphite alkene quantum solid point that airport construction solidifies etc. Agent added material.
Description
Technical field
The present invention relates to technical field of nano material, more particularly, are related to a kind of graphene quantum dot soil-solidified-agent
Preparation method.
Background technique
In the Large scale construction of city, fried mountain rubble, Wa He adopt sand, not only break up natural environment, sandstone material is remote
Far from meeting growing infrastructure needs, as can soil cheap, from a wealth of sources is made effective use of, as
Engineering construction material reduces the destruction to natural resources, and engineering test proves, can effectively improve using soil-solidified-agent solid
Change the intensity and items physical and mechanical property of the soil body, and gather materials on the spot, can economize on resources, protect environment, facilitate construction, save
Construction investment is saved, construction quality is improved, extends engineering service life etc..Domestic enterprise is from different raw material and engine request
The soil-solidified-agent product of oneself is had developed, and is applied in some geotechnical engineerings, soil-solidified-agent is after concrete
After additive application, the another success measure of engineering technology problem is solved using chemistry, physical chemistry and biochemical method, is opened
Application of the chemicals in Geotechnical Engineering has been opened up, has been a very promising geotechnological new technology.
In order to economize on resources, protection environment conducts in-depth research exploitation to soil stabilization, novel for developed country
Soil-solidified-agent can substitute rubble, river sand, lime, flyash etc., and be widely used in highway, hydraulic engineering, airfield runway,
The fields such as backroad, building construction, Hu Ba solidification are gathered materials on the spot since soil-solidified-agent has, construction technology is simple, engineering
Low cost etc. advantage increases substantially the compression strength of soil, economic benefit and obvious environment benefit, once by the U.S.
" Engineering News Record " is known as the invention of 20th century greatness.
Existing soil-solidified-agent is divided into inorganic solidification agent and organic liquid curing agent and biological enzyme solidification three classes,
Curing mechanism is as follows:
(1) inorganic solidification agent: inorganic curing agent focuses mostly on to be changed in the conventional curing material such as cement, lime, slag
Type, modification make the curing materials with comprehensive stability performance.Various chemical reactions are generated under water effect, are generated solidifying
Gelatinous hyrate surrounds soil particle, and this hyrate can voluntarily continue hardening and form skeleton, and generation is reacted with soil particle
Complex compound is finally interconnected to form stable reticular structure, to enhance adhesion strength, the Ca 2+ that is generated in use, 2 Mg
+ or Al 3+ can be swapped with Na+, K+ ion in native micelle adsorption layer, to reduce native micelle zeta potential, reduce native micelle
The thickness of electric double layer makes soil mutually generate cohesion.
(2) organic curing agent: organic curing agent includes the classes curing agent such as various kinds of resin, fiber, surfactant, benefit
Change grogs surface hydrophilic property with surfactant, or forms stereochemical structure package and binder soil using crosslinked polymer
Grain, on the basis of soil compression, the soil-solidified-agent of available preferable compression strength.Utilize the electric double layer of soil micelle
Principle generates the counter ion of high concentration, with the electrical property between soil micelle surface negative charge after the addition of macromolecular liquid curing agent
Power overcomes " energy barrier " between soil micelle, increases the attraction between micelle, reduces zeta potential, electric double layer thickness is effectively thinned,
The coalescence of soil colloid particle is improved, bond strength and water stability between soil particle are improved.
(3) biological enzyme curing agent: by the way that solidification enzyme is added to soil, soil is made quickly to generate closely knit, hard knot
Structure layer, to prevent from reducing density because absorbing moisture expansion.The main component of biological soil curing agent is enzyme, and this kind of soil is solid
The intensity for solidifying the soil body of agent is not high enough, and cementing material additional amount is larger, and soil porosity and permeability effects are poor, is difficult
The roadbed of high quality is obtained, service life is not long etc..
Solidification effect according to above-mentioned soil-solidified-agent is not ideal enough, and application range is relatively narrow, selects the soil being cured
Property it is high, it is big etc. to blend cement, sandstone amount in use, is unable to reach the performance requirement to soil-solidified-agent, is unfavorable for soil solidification
The application of agent, therefore, it is wide to research and develop a kind of P in soil H value range that is suitable for, and is not influenced by Geological and soil environment, can be just
Ground materials solidification, environmentally protective soil curing agent thing must go.
Summary of the invention
In order to overcome the drawbacks of the prior art, the present invention provides a kind of system of new polymers graphene quantum dot curing agent
Preparation Method.Therefore, it is an object of the present invention to provide a kind of new polymers graphene quantum dot curing agent.
The purpose of the invention is achieved by the following technical solution:
A kind of graphene quantum dot soil-solidified-agent preparation method, present invention is characterized in that by polymer graphite alkene quantum
Point solution, polymer graphite alkene quantum dot inflation fluid, polymer graphite alkene quantum dot surface activity liquid composition, above-mentioned three kinds of liquid
It is in parts by weight；Wherein:
The polymer graphite alkene quantum dot solution, by 150-550 parts of phytic acid powder, 150-350 parts of waterglass,
150-350 parts of sodium tripolyphosphate, multiple water 550-800 parts of compositions；Preparation method and step are as follows:
Polymer graphite alkene quantum dot solution preparation method and steps are as follows:
(1) by phytic acid powder, be placed in first vacuum reaction furnace, sequentially add multiple water dilution, waterglass,
Sodium tripolyphosphate, setting revolving speed are not less than 450/rps, and setting temperature is 35-95 DEG C, until shut down after reaction time 2-8/hour,
Room temperature cooling obtains polymer graphite alkene quantum dot mother liquor；
(2) by 0.1-0.25 μm of filtering with microporous membrane of polymer graphite alkene quantum dot mother liquor obtained in (1), subnatant
Body 3500Da bag filter, dialyse 24-72/hour, removes sundries extra in reactant, obtains polymer graphite alkene quantum dot
Aqueous solution；
(3) it by polymer graphite alkene quantum dot aqueous solution liquid nitrogen quenching obtained in (2), is lyophilized in freeze drier
After grind, obtain polymer graphite alkene quantum dot powder；
The polymer graphite alkene quantum dot inflation fluid, by 150-400 parts of phytic acid powder, 120-350 parts of first
Sour calcium, 100-300 part magnesia, 200-500 parts of sodium chloride, 200-500 parts of sodium sulphate, 300-800 parts of calcium chloride, 500-800
Repeatedly water forms part；
Polymer graphite alkene quantum dot inflation fluid is by the following method and prepared by step:
(1) it by phytic acid powder, is placed in second vacuum reaction furnace, sequentially adds multiple water, calcium formate, oxidation
Magnesium, sodium chloride, sodium sulphate, calcium chloride, setting revolving speed are not less than 450/rps, are arranged 35-60 DEG C of temperature, reaction time 2-8/
It is shut down after hour, room temperature cooling obtains polymer graphite alkene quantum dot expansion mother liquor；
(2) polymer graphite alkene quantum dot obtained in (1) is expanded into mother liquor, moved in centrifuge, revolving speed is set
11000/rps after being centrifuged 15-30/min, removes unreacted sundries, obtains polymer graphite alkene quantum dot expansion aqueous solution；
(3) it by the liquid nitrogen quenching of graphene quantum dot aqueous solution obtained in (2), is ground after being lyophilized in freeze drier
Mill obtains polymer graphite alkene quantum dot expansion powder；
The polymer graphite alkene quantum dot surface activity liquid is gathered by 120-250 parts of phytic acids, 120-250 parts
Ethylene glycol 400,150-300 part sodium lignin sulfonate, 200-500 parts of sulfonated oils, 500-800 parts of acidified sodium silicate solution compositions；
Described phytic acid 120-250 parts；Content >=50% of six phosphoric acid of preferably myo-inositol, molecular formula are as follows:
C6H18O24P6；
Polymer graphite alkene quantum dot surface activity liquid and preparation method thereof and step are as follows:
(1) by phytic acid, sodium lignin sulfonate, sulfonated oil, acidified sodium silicate solution, it is placed in third vacuum reaction
In furnace, revolving speed 550-750/rps is set, is arranged 30-45 DEG C of temperature, after reaction time 2-8/hour, obtains polymer graphite alkene
Quantum dot surface activity mother liquor；
(2) by 0.1-0.3 μm of miillpore filter mistake of polymer graphite alkene quantum dot surface activity mother liquor obtained in (1)
Filter, lower liquid 4500Da bag filter, dialyse 24-72/hour, and it is water-soluble to obtain polymer graphite alkene quantum dot surface activity
Liquid.
(3) it by polymer graphite alkene quantum dot surface activity aqueous solution liquid nitrogen quenching obtained in (2), is being freeze-dried
It is ground after being lyophilized in machine, obtains polymer graphite alkene quantum dot surface active powder；
The wherein liquid nitrogen quenching time 1-5/hour；80-200 nanometers are ground after the freeze-drying；
The polymer graphite alkene quantum dot aqueous solution of acquisition, polymer graphite alkene quantum dot are expanded into aqueous solution, polymer
Graphene quantum dot surface-active aqueous solution, by weight percentage 20-30:50-60:20 are transferred in ultrasonic cleaning machine, control temperature
45-75 DEG C of degree, ultrasonic cleaning machine processing power are 600-1000W, and sonication treatment time is that it is anti-to be placed in V-type mixing after 3-8 hours
It answers in machine, setting revolving speed is not less than 400/rps, heats up 60 DEG C -75 DEG C, after keeping 30-60/min, after natural cooling, is gathered
Close object graphene quantum dot soil-solidified-agent.
The polymer graphite alkene quantum dot aqueous solution of acquisition, polymer graphite alkene quantum dot are expanded into aqueous solution, polymer
Graphene quantum dot surface-active aqueous solution, by weight percentage 30:50:20 are transferred in ultrasonic cleaning machine, control temperature 55-
60 DEG C, ultrasonic cleaning machine processing power is 600-1000W, and sonication treatment time is to be placed in V-type mixing reactor after 5-6 hours
Interior, setting revolving speed is not less than 400/rps, heats up 60 DEG C -75 DEG C, after keeping 40-50/min, after natural cooling, obtains polymer
Graphene quantum dot soil-solidified-agent.
The polymer graphite alkene quantum dot powder of acquisition, polymer graphite alkene quantum dot are expanded into powder, polymer graphite
Alkene quantum dot surface active powder, by weight percentage 20:60:20 are placed in vacuum mixer, control 65 DEG C of temperature, ultrasound
Washer power 800W, sonication treatment time are 6 hours, and mixing machine revolving speed 650/rps is arranged, and keep vacuum after 60/min dry
It is dry, obtain polymer graphite alkene quantum dot soil-solidified-agent powder.
The present invention in polymer graphite alkene quantum dot solution preparation method and step, be selected as by the phytic acid powder
150 parts；The waterglass is preferably 150 parts；It is preferred that modulus of water glass 2.8-3.5, Baume degrees 2.4~32.4；The trimerization phosphorus
Sour sodium is preferably 150 parts；The multiple water is preferably 600 parts of multiple water.
For the present invention in polymer graphite alkene quantum dot inflation fluid by the following method and in step, the polyethylene glycol is preferred
It is 150 parts；The sodium lignin sulfonate is preferably 180 parts；The sulfonated oil is preferably 250 parts；The acidified sodium silicate solution
Preferably 600 parts；Wherein the acidified sodium silicate solution is in parts by weight: 150 parts of dilute sulfuric acid, concentration 15% and waterglass 150
Part, modulus 2.8-3.5, Baume degrees 2.4~32.4 forms.
The present invention is in polymer graphite alkene quantum dot surface activity liquid and preparation method thereof and step, the phytic acid powder
Preferably 150 parts of end；Content >=50% of six phosphoric acid of preferably myo-inositol, molecular formula are as follows: C6H18O24P6；
Calcium formate of the present invention is preferably 120 parts；The magnesia is preferably 200 parts；The sodium chloride is preferably 250
Part；The sodium sulphate is preferably 250 parts；The calcium chloride is preferably 400 parts；The multiple water is preferably 800 parts.
The present invention adds the polymer graphite alkene amount of 2%-8% according to the total weight percent of civil engineering inorganic material
Son point soil-solidified-agent, or the polymer graphite of the total weight percent addition 5%-10% according to civil engineering inorganic material
Alkene quantum dot soil-solidified-agent powder.
In conclusion the invention has the following advantages:
1, polymer graphite alkene quantum dot soil-solidified-agent has ion exchange effect, reduces dipole moment, changes soil parent
Aqueous is hydrophobicity, and electromotive force effect enhances soil quantum dot particle cohesion, and irreducible water is changed into Free water and is full of soil
Intergranular pore be further compressed soil can to enhance bearing capacity of soil；
2, polymer graphite alkene quantum dot soil-solidified-agent has quantum point effect, and the unique property of quantum dot is based on it certainly
The quantum effect of body, when particle size enters nanometer scale, size confinement will cause dimensional effect, quantum confined effect, macro
Quantum tunneling effect and skin effect are seen, to derive the nanometer system low-dimensional object different with microsystem with normal sight system
Property, many physicochemical properties for being different from macroscopic body material are shown, are had in civil engineering material application aspect extremely wide
Wealthy application prospect can generate H+, further reinforced soil ion-exchange effect in the soil；
3, polymer graphite alkene quantum dot soil-solidified-agent has quantum dot ionisation effect, the quantum dot between clay particle
Contact, increases soil strength, and generate Ca 2+, Mg2+ or Al3+, can carry out with Na+, K+ ion in native micelle adsorption layer
Exchange is thinned the thickness of soil micelle electric double layer, makes soil particle generation soil close to each other to reduce soil micelle zeta potential
Cohesiveness；
4, there is polymer graphite alkene quantum dot soil-solidified-agent quantum dot crystal form to recombinate effect, the crystalline substance of clay microstructure
Shape rearranges under the action of quantum dot curing agent, forms more stable soil quantum crystalline form web frame；
5, polymer graphite alkene quantum dot soil-solidified-agent has quanta point biological sterilizing effect, and quantum dot has unique raw
Object sterilizing function, use will not be destroyed solidification plate by soil miscellaneous bacteria institute's attack in the soil, thus stable soil base plate
Service life.
6, polymer graphite alkene quantum dot soil-solidified-agent, dosage is few at low cost in actual use, and dosage is mixing material
It is used after the 2%-8% for expecting total weight ratio, with the water dilution of 100%-200%；Polymer graphite alkene quantum dot soil-solidified-agent
Powder hardener dose is to use after the 5%-10% of admixture total weight is stirred；
7, polymer graphite alkene quantum dot soil-solidified-agent has relatively strongization to adapt to effect in various soft base soil and concrete
Fruit improves compaction strength, the modulus of resilience, deflection value, CBR (load-carrying as added material into concrete and in soft base soil property
Than), shear strength etc., can be used for road infrastructure, the backfill of tailing hole, building waste, lake silt, oil field sludge it is secondary
Using solidification, so that integrated application range of the invention be greatly improved.
Specific embodiment
Further detailed description is done to the present invention combined with specific embodiments below, the following examples are merely to illustrate this
It invents rather than limits the scope of the invention.
Embodiment 1:
One, the polymer graphite alkene quantum dot solution, the polymer graphite alkene quantum dot solution, in parts by weight by
150 parts of phytic acid powder, 350 parts of waterglass, 150 parts of sodium tripolyphosphate, 700 parts of multiple water compositions；
(1) it by phytic acid powder, is placed in first vacuum reaction furnace, sequentially adds and multiple water dilution, water is added
Glass, sodium tripolyphosphate, setting revolving speed are not less than 450/rps, are arranged 95 DEG C of temperature, shut down after reaction time 8/hour, room temperature
Cooling polymer graphite alkene quantum dot mother liquor；With 0.1 μm of filtering with microporous membrane, lower liquid 3500Da bag filter, dialysis
24/hour removes sundries extra in reactant, obtains polymer graphite alkene quantum dot water solution A -1；With liquid nitrogen quenching, In
It is ground after being lyophilized in freeze drier, obtains polymer graphite alkene quantum dot powder B-1.
Two, the polymer graphite alkene quantum dot inflation fluid, in parts by weight by 150 parts of phytic acid powder, 350
Part calcium formate, 100 parts of magnesia, 200 parts of sodium chloride, 200 parts of sodium sulphate, 300 parts of calcium chloride, 500 parts of multiple water compositions；
(1) it by phytic acid powder, is placed in second vacuum reaction furnace, sequentially adds multiple water, calcium formate, oxidation
Magnesium, sodium chloride, sodium sulphate, calcium chloride, setting revolving speed are not less than 450/rps, are arranged 40 DEG C of temperature, stop after reaction time 2/hour
Machine, room temperature cooling obtain polymer graphite alkene quantum dot expansion mother liquor；It moves in centrifuge, revolving speed 11000/rps, centrifugation is set
After 15/min, unreacted sundries is removed, obtains polymer graphite alkene quantum dot expansion water solution A -2；With liquid nitrogen quenching polymer
Graphene quantum dot expands aqueous solution, grinds after being lyophilized in freeze drier, obtains polymer graphite alkene quantum dot expanding powder
Body B-2；
Three, the polymer graphite alkene quantum dot surface activity liquid, in parts by weight by 120 parts of phytic acids, 120
Part polyethylene glycol 400,150 parts of sodium lignin sulfonates, 200 parts of sulfonated oils, 500 parts of acidified sodium silicate solution compositions；
(1) by phytic acid, sodium lignin sulfonate, sulfonated oil, acidified sodium silicate solution, it is placed in third vacuum reaction
In furnace, revolving speed 560/rps is set, is arranged 30 DEG C of temperature, after reaction time 2/hour, obtains polymer graphite alkene quantum dot surface
Active mother liquor；With 0.1 μm of filtering with microporous membrane, lower liquid 4500Da bag filter, dialyse 24/hour, obtains polymer stone
Black alkene quantum dot surface activity water solution A -3.With liquid nitrogen quenching polymer graphite alkene quantum dot surface activity aqueous solution, freezing
It is ground after being lyophilized in drying machine, obtains polymer graphite alkene quantum dot surface active powder B-3；
Four, it by above-mentioned A-1, A-2, A-3 30:50:20 by weight percentage, is transferred in ultrasonic cleaning machine, controls temperature 45
DEG C, ultrasonic cleaning machine processing power is 600W, and sonication treatment time is to be placed in V-type mixing reactor after 3 hours, and setting turns
Speed is not less than 400/rps, and 60 DEG C -75 DEG C of control heating after keeping 30/min, after natural cooling, obtains polymer graphite alkene amount
Son point soil-solidified-agent.
Five, it by above-mentioned B-1, B-2, B-3 20:60:20 by weight percentage, is placed in vacuum mixer, controls temperature 60
DEG C, mixing machine revolving speed 650/rps is set, is dried in vacuo after keeping 60/min, polymer graphite alkene quantum dot soil solidification is obtained
Agent powder.
The above embodiment of the present invention is a kind of first public new polymers graphene quantum dot soil-solidified-agent, in material
Material using and the mechanism of action on at present soil-solidified-agent both domestic and external be it is distinguishing, the principle of solidification be utilize polymer stone
Black alkene quantum dot compositions form depth vertical body package to particle in soil property, under the interaction of inorganic material, form soil property
Three-dimensional high-density network structure further consolidates the every comprehensive strength for improving soil property, can be widely applied to civil engineering etc..
Embodiment 2
One, the polymer graphite alkene quantum dot solution, the polymer graphite alkene quantum dot solution, in parts by weight by
550 parts of phytic acid powder, 350 parts of waterglass, 350 parts of sodium tripolyphosphate, 800 parts of multiple water compositions；
(2) it by phytic acid powder, is placed in first vacuum reaction furnace, sequentially adds and multiple water dilution, water is added
Glass, sodium tripolyphosphate, setting revolving speed are not less than 450/rps, are arranged 95 DEG C of temperature, shut down after reaction time 8/hour, room temperature
Cooling polymer graphite alkene quantum dot mother liquor；With 0.25 μm of filtering with microporous membrane, lower liquid 3500Da bag filter, dialysis
72/hour removes sundries extra in reactant, obtains polymer graphite alkene quantum dot water solution A -1；With liquid nitrogen quenching, In
It is ground after being lyophilized in freeze drier, obtains polymer graphite alkene quantum dot powder B-1.
Two, the polymer graphite alkene quantum dot inflation fluid, in parts by weight by 400 parts of phytic acid powder, 350
Part calcium formate, 300 parts of magnesia, 500 parts of sodium chloride, 500 parts of sodium sulphate, 800 parts of calcium chloride, 800 parts of multiple water compositions；
(1) it by phytic acid powder, is placed in second vacuum reaction furnace, sequentially adds multiple water, calcium formate, oxidation
Revolving speed 650/rps is arranged in magnesium, sodium chloride, sodium sulphate, calcium chloride, and temperature 60 C is arranged, shuts down after reaction time 8/hour, often
Temperature is cooling that polymer graphite alkene quantum dot expands mother liquor；It moves in centrifuge, revolving speed 11000/rps is set, be centrifuged 30/min
Afterwards, unreacted sundries is removed, polymer graphite alkene quantum dot expansion water solution A -2 is obtained；With liquid nitrogen quenching polymer graphite alkene
Quantum dot expands aqueous solution, grinds after being lyophilized in freeze drier, obtains polymer graphite alkene quantum dot expansion powder B-2；
Three, the polymer graphite alkene quantum dot surface activity liquid, in parts by weight by 250 parts of phytic acids, 250
Part polyethylene glycol 400,300 parts of sodium lignin sulfonates, 500 parts of sulfonated oils, 800 parts of acidified sodium silicate solution compositions；
(1) by phytic acid, sodium lignin sulfonate, sulfonated oil, acidified sodium silicate solution, it is placed in third vacuum reaction
In furnace, revolving speed 750/rps is set, temperature 45 C is set, after reaction time 8/hour, obtains polymer graphite alkene quantum dot surface
Active mother liquor；With 0.3 μm of filtering with microporous membrane, lower liquid 4500Da bag filter, dialyse 72/hour, obtains polymer stone
Black alkene quantum dot surface activity water solution A -3.With liquid nitrogen quenching polymer graphite alkene quantum dot surface activity aqueous solution, freezing
It is ground after being lyophilized in drying machine, obtains polymer graphite alkene quantum dot surface active powder B-3；
Four, it by above-mentioned A-1, A-2, A-3 30:50:20 by weight percentage, is transferred in ultrasonic cleaning machine, controls temperature 65
DEG C, ultrasonic cleaning machine processing power is 1000W, and sonication treatment time is to be placed in V-type mixing reactor after 8 hours, and setting turns
Fast 600/rps, 75 DEG C of control heating after keeping 60/min, after natural cooling, obtain polymer graphite alkene quantum dot soil solidification
Agent.Five, it by above-mentioned B-1, B-2, B-3 20:60:20 by weight percentage, is placed in vacuum mixer, controls 75 DEG C of temperature, if
Mixing machine revolving speed 650/rps is set, is dried in vacuo after keeping 60/min, polymer graphite alkene quantum dot soil-solidified-agent powder is obtained
Body.
Embodiment 3
One, the polymer graphite alkene quantum dot solution, the polymer graphite alkene quantum dot solution, in parts by weight by
350 parts of phytic acid powder, 200 parts of waterglass, 200 parts of sodium tripolyphosphate, 650 parts of multiple water compositions；
(3) it by phytic acid powder, is placed in first vacuum reaction furnace, sequentially adds and multiple water dilution, water is added
Revolving speed 450/rps is arranged in glass, sodium tripolyphosphate, is arranged 65 DEG C of temperature, shuts down after reaction time 5/hour, room temperature cooling obtains
Polymer graphite alkene quantum dot mother liquor；With 0.15 μm of filtering with microporous membrane, lower liquid 3500Da bag filter, dialysis 45/
Hour removes sundries extra in reactant, obtains polymer graphite alkene quantum dot water solution A -1；With liquid nitrogen quenching, freezing
It is ground after being lyophilized in drying machine, obtains polymer graphite alkene quantum dot powder B-1.
Two, the polymer graphite alkene quantum dot inflation fluid, in parts by weight by 200 parts of phytic acid powder, 200
Part calcium formate, 200 parts of magnesia, 350 parts of sodium chloride, 350 parts of sodium sulphate, 450 parts of calcium chloride, 650 parts of multiple water compositions；
(1) it by phytic acid powder, is placed in second vacuum reaction furnace, sequentially adds multiple water, calcium formate, oxidation
Revolving speed 850/rps is arranged in magnesium, sodium chloride, sodium sulphate, calcium chloride, and temperature 50 C is arranged, shuts down after reaction time 5/hour, often
Temperature is cooling that polymer graphite alkene quantum dot expands mother liquor；It moves in centrifuge, revolving speed 11000/rps is set, be centrifuged 20/min
Afterwards, unreacted sundries is removed, polymer graphite alkene quantum dot expansion water solution A -2 is obtained；With liquid nitrogen quenching polymer graphite alkene
Quantum dot expands aqueous solution, grinds after being lyophilized in freeze drier, obtains polymer graphite alkene quantum dot expansion powder B-2；
Three, the polymer graphite alkene quantum dot surface activity liquid, in parts by weight by 180 parts of phytic acids, 180
Part polyethylene glycol 400,200 parts of sodium lignin sulfonates, 300 parts of sulfonated oils, 650 parts of acidified sodium silicate solution compositions；
(1) by phytic acid, sodium lignin sulfonate, sulfonated oil, acidified sodium silicate solution, it is placed in third vacuum reaction
In furnace, setting revolving speed is not less than 650/rps, is arranged 40- DEG C of temperature, after reaction time 5/hour, obtains polymer graphite alkene amount
Son point surface-active mother liquor；With 0.2 μm of filtering with microporous membrane, lower liquid 4500Da bag filter, dialyse 55/hour, obtains
Polymer graphite alkene quantum dot surface activity water solution A -3.It is water-soluble with liquid nitrogen quenching polymer graphite alkene quantum dot surface activity
Liquid grinds after being lyophilized in freeze drier, obtains polymer graphite alkene quantum dot surface active powder B-3；
Four, it by above-mentioned A-1, A-2, A-3 30:50:20 by weight percentage, is transferred in ultrasonic cleaning machine, controls temperature 55
DEG C, ultrasonic cleaning machine processing power is 850W, and sonication treatment time is to be placed in V-type mixing reactor after 6 hours, and setting turns
Fast 650/rps, 70 DEG C of control heating after keeping 50/min, after natural cooling, obtain polymer graphite alkene quantum dot soil solidification
Agent.Five, it by above-mentioned B-1, B-2, B-3 20:60:20 by weight percentage, is placed in vacuum mixer, controls temperature 70 C, if
Mixing machine revolving speed 650/rps is set, is dried in vacuo after keeping 60/min, polymer graphite alkene quantum dot soil-solidified-agent powder is obtained
Body.
Embodiment 4
A kind of graphene quantum dot soil-solidified-agent preparation method, by polymer graphite alkene quantum dot solution, polymer stone
Black alkene quantum dot inflation fluid, polymer graphite alkene quantum dot surface activity liquid composition, above-mentioned three kinds of liquid are in parts by weight；Its
In:
The polymer graphite alkene quantum dot solution, by 400 parts of phytic acid powder, 180 parts of waterglass, tripolyphosphate
220 parts of sodium, 750 parts of multiple water compositions；Preparation method and step are as follows:
Polymer graphite alkene quantum dot solution preparation method and steps are as follows:
(3) by phytic acid powder, be placed in first vacuum reaction furnace, sequentially add multiple water dilution, waterglass,
Revolving speed 850/rps is arranged in sodium tripolyphosphate, and setting temperature is 75 DEG C, until shutting down after reaction time 5/hour, room temperature cooling must gather
Close object graphene quantum dot mother liquor；
(4) by 0.2 μm of filtering with microporous membrane of polymer graphite alkene quantum dot mother liquor obtained in (1), lower liquid is used
3500Da bag filter, dialyse 30/hour, removes sundries extra in reactant, obtains polymer graphite alkene quantum dot aqueous solution；
(3) it by polymer graphite alkene quantum dot aqueous solution liquid nitrogen quenching obtained in (2), is lyophilized in freeze drier
After grind, obtain polymer graphite alkene quantum dot powder；
The polymer graphite alkene quantum dot inflation fluid, by 250 parts of phytic acid powder, 180 parts of calcium formates, 180
Part magnesia, 350 parts of sodium chloride, 300 parts of sodium sulphate, 500 parts of calcium chloride, 6500 parts of multiple water compositions；
Polymer graphite alkene quantum dot inflation fluid is by the following method and prepared by step:
(1) it by phytic acid powder, is placed in second vacuum reaction furnace, sequentially adds multiple water, calcium formate, oxidation
Revolving speed 650/rps is arranged in magnesium, sodium chloride, sodium sulphate, calcium chloride, and temperature 45 C is arranged, shuts down after reaction time 4/hour, often
Temperature is cooling that polymer graphite alkene quantum dot expands mother liquor；
(2) polymer graphite alkene quantum dot obtained in (1) is expanded into mother liquor, moved in centrifuge, revolving speed is set
11000/rps after being centrifuged 18/min, removes unreacted sundries, obtains polymer graphite alkene quantum dot expansion aqueous solution；
(3) it by the liquid nitrogen quenching of graphene quantum dot aqueous solution obtained in (2), is ground after being lyophilized in freeze drier
Mill obtains polymer graphite alkene quantum dot expansion powder；
The polymer graphite alkene quantum dot surface activity liquid, by 165 parts of phytic acids, 180 parts of polyethylene glycol
400,200 parts of sodium lignin sulfonates, 350 parts of sulfonated oils, 700 parts of acidified sodium silicate solution compositions；
170 parts of the phytic acid；Content >=50% of six phosphoric acid of preferably myo-inositol, molecular formula are as follows: C6H18O24P6；
Polymer graphite alkene quantum dot surface activity liquid and preparation method thereof and step are as follows:
(1) by phytic acid, sodium lignin sulfonate, sulfonated oil, acidified sodium silicate solution, it is placed in third vacuum reaction
In furnace, revolving speed 650/rps is set, is arranged 40 DEG C of temperature, after reaction time 5/hour, obtains polymer graphite alkene quantum dot surface
Active mother liquor；
(2) by 0.25 μm of filtering with microporous membrane of polymer graphite alkene quantum dot surface activity mother liquor obtained in (1), under
Layer liquid 4500Da bag filter, dialyse 30/hour, obtains polymer graphite alkene quantum dot surface activity aqueous solution.
(3) it by polymer graphite alkene quantum dot surface activity aqueous solution liquid nitrogen quenching obtained in (2), is being freeze-dried
It is ground after being lyophilized in machine, obtains polymer graphite alkene quantum dot surface active powder；
The wherein liquid nitrogen quenching time 3/hour；100 nanometers are ground after the freeze-drying；
The polymer graphite alkene quantum dot aqueous solution of acquisition, polymer graphite alkene quantum dot are expanded into aqueous solution, polymer
Graphene quantum dot surface-active aqueous solution, by weight percentage 25:55:20 are transferred in ultrasonic cleaning machine, control temperature 55
DEG C, ultrasonic cleaning machine processing power is 800W, and sonication treatment time is to be placed in V-type mixing reactor after 6 hours, and setting turns
Fast 550/rps is warming up to 65 DEG C, after keeping 55/min, after natural cooling, obtains polymer graphite alkene quantum dot soil solidification
Agent.
The polymer graphite alkene quantum dot aqueous solution of acquisition, polymer graphite alkene quantum dot are expanded into aqueous solution, polymer
Graphene quantum dot surface-active aqueous solution, by weight percentage 30:50:20 are transferred in ultrasonic cleaning machine, control temperature 58
DEG C, ultrasonic cleaning machine processing power is 800W, and sonication treatment time is to be placed in V-type mixing reactor after 5 hours, and setting turns
Fast 450/rps heats up 60 DEG C, after keeping 45/min, after natural cooling, obtains polymer graphite alkene quantum dot soil-solidified-agent.
The polymer graphite alkene quantum dot powder of acquisition, polymer graphite alkene quantum dot are expanded into powder, polymer graphite
Alkene quantum dot surface active powder, by weight percentage 20:60:20 are placed in vacuum mixer, control 65 DEG C of temperature, ultrasound
Washer power 800W, sonication treatment time are 6 hours, and mixing machine revolving speed 650/rps is arranged, and keep vacuum after 60/min dry
It is dry, obtain polymer graphite alkene quantum dot soil-solidified-agent powder.
The present invention in polymer graphite alkene quantum dot solution preparation method and step, be selected as by the phytic acid powder
150 parts；The waterglass is preferably 150 parts；It is preferred that modulus of water glass 2.8-3.5, Baume degrees 2.4~32.4；The trimerization phosphorus
Sour sodium is preferably 150 parts；The multiple water is preferably 600 parts of multiple water.
For the present invention in polymer graphite alkene quantum dot inflation fluid by the following method and in step, the polyethylene glycol is preferred
It is 150 parts；The sodium lignin sulfonate is preferably 180 parts；The sulfonated oil is preferably 250 parts；The acidified sodium silicate solution
Preferably 600 parts；Wherein the acidified sodium silicate solution is in parts by weight: 150 parts of dilute sulfuric acid, concentration 15% and waterglass 150
Part, modulus 2.8, Baume degrees 20 forms.
The present invention is in polymer graphite alkene quantum dot surface activity liquid and preparation method thereof and step, the phytic acid powder
Preferably 150 parts of end；Content >=50% of six phosphoric acid of preferably myo-inositol, molecular formula are as follows: C6H18O24P6；
Calcium formate of the present invention is preferably 120 parts；The magnesia is preferably 200 parts；The sodium chloride is preferably 250
Part；The sodium sulphate is preferably 250 parts；The calcium chloride is preferably 400 parts；The multiple water is preferably 800 parts.
Claims (6)
1. a kind of graphene quantum dot soil-solidified-agent preparation method, it is characterised in that: by polymer graphite alkene quantum dot solution,
Polymer graphite alkene quantum dot inflation fluid, polymer graphite alkene quantum dot surface activity liquid composition, above-mentioned three kinds of liquid is with weight
Measure part meter；Wherein:
The polymer graphite alkene quantum dot solution, by 150-550 parts of phytic acid powder, 150-350 parts of waterglass, trimerization
150-350 parts of sodium phosphate, multiple water 550-800 parts of compositions；Preparation method and step are as follows:
Polymer graphite alkene quantum dot solution preparation method and steps are as follows:
(1) it by phytic acid powder, is placed in first vacuum reaction furnace, sequentially adds multiple water dilution, waterglass, trimerization
Sodium phosphate, setting revolving speed are not less than 450/rps, and setting temperature is 35-95 DEG C, until shutting down after reaction time 2-8/hour, room temperature
Cooling polymer graphite alkene quantum dot mother liquor；
(2) by 0.1-0.25 μm of filtering with microporous membrane of polymer graphite alkene quantum dot mother liquor obtained in (1), lower liquid is used
3500Da bag filter, dialyse 24-72/hour, removes sundries extra in reactant, it is water-soluble to obtain polymer graphite alkene quantum dot
Liquid；
(3) it by polymer graphite alkene quantum dot aqueous solution liquid nitrogen quenching obtained in (2), is ground after being lyophilized in freeze drier
Mill, obtains polymer graphite alkene quantum dot powder；
The polymer graphite alkene quantum dot inflation fluid, by 150-400 parts of phytic acid powder, 120-350 parts of calcium formates,
100-300 parts of magnesia, 200-500 parts of sodium chloride, 200-500 parts of sodium sulphate, 300-800 parts of calcium chloride, 500-800 parts repeatedly
Water composition；
Polymer graphite alkene quantum dot inflation fluid is by the following method and prepared by step:
(1) by phytic acid powder, be placed in second vacuum reaction furnace, sequentially add multiple water, calcium formate, magnesia,
Sodium chloride, sodium sulphate, calcium chloride, setting revolving speed are not less than 450/rps, are arranged 35-60 DEG C of temperature, after reaction time 2-8/hour
It shuts down, room temperature cooling obtains polymer graphite alkene quantum dot expansion mother liquor；
(2) polymer graphite alkene quantum dot obtained in (1) is expanded into mother liquor, moved in centrifuge, revolving speed 11000/ is set
Rps after being centrifuged 15-30/min, removes unreacted sundries, obtains polymer graphite alkene quantum dot expansion aqueous solution；
(3) it by the liquid nitrogen quenching of graphene quantum dot aqueous solution obtained in (2), grinds, obtains after being lyophilized in freeze drier
Powder is expanded to polymer graphite alkene quantum dot；
The polymer graphite alkene quantum dot surface activity liquid, by 120-250 parts of phytic acids, 120-250 parts of poly- second two
Alcohol 400,150-300 part sodium lignin sulfonate, 200-500 parts of sulfonated oils, 500-800 parts of acidified sodium silicate solution compositions；
Described phytic acid 120-250 parts；Content >=50% of six phosphoric acid of preferably myo-inositol, molecular formula are as follows: C6H18O24P6；
Polymer graphite alkene quantum dot surface activity liquid and preparation method thereof and step are as follows:
(1) by phytic acid, sodium lignin sulfonate, sulfonated oil, acidified sodium silicate solution, it is placed in third vacuum reaction furnace
In, revolving speed 550-750/rps is set, is arranged 30-45 DEG C of temperature, after reaction time 2-8/hour, obtains polymer graphite alkene amount
Son point surface-active mother liquor；
(2) by 0.1-0.3 μm of filtering with microporous membrane of polymer graphite alkene quantum dot surface activity mother liquor obtained in (1), under
Layer liquid 4500Da bag filter, dialyse 24-72/hour, obtains polymer graphite alkene quantum dot surface activity aqueous solution；
(3) by polymer graphite alkene quantum dot surface activity aqueous solution liquid nitrogen quenching obtained in (2), in freeze drier
It is ground after freeze-drying, obtains polymer graphite alkene quantum dot surface active powder；
The wherein liquid nitrogen quenching time 1-5/hour；80-200 nanometers are ground after the freeze-drying；
The polymer graphite alkene quantum dot aqueous solution of acquisition, polymer graphite alkene quantum dot are expanded into aqueous solution, polymer graphite
Alkene quantum dot surface activity aqueous solution, by weight percentage 20-30:50-60:20 are transferred in ultrasonic cleaning machine, control temperature
45-75 DEG C, ultrasonic cleaning machine processing power is 600-1000W, and sonication treatment time is to be placed in V-type hybrid reaction after 3-8 hours
In machine, setting revolving speed is not less than 400/rps, heats up 60 DEG C -75 DEG C, after keeping 30-60/min, after natural cooling, is polymerize
Object graphene quantum dot soil-solidified-agent.
2. a kind of graphene quantum dot soil-solidified-agent preparation method according to claim 1, which is characterized in that will obtain
Polymer graphite alkene quantum dot aqueous solution, polymer graphite alkene quantum dot expand aqueous solution, polymer graphite alkene quantum dot table
Face activity aqueous solution, by weight percentage 30:50:20 are transferred in ultrasonic cleaning machine, control 55-60 DEG C of temperature, ultrasonic cleaning machine
Processing power is 600-1000W, and sonication treatment time is to be placed in V-type mixing reactor after 5-6 hours, and setting revolving speed is not low
It in 400/rps, heats up 60 DEG C -75 DEG C, after keeping 40-50/min, after natural cooling, obtains polymer graphite alkene quantum dot soil
Curing agent.
3. a kind of graphene quantum dot soil-solidified-agent preparation method according to claim 1, which is characterized in that will obtain
Polymer graphite alkene quantum dot powder, polymer graphite alkene quantum dot expansion powder, polymer graphite alkene quantum dot surface it is living
Property powder, by weight percentage 20:60:20, be placed in vacuum mixer, control 65 DEG C of temperature, ultrasonic cleaning machine power 800W,
Sonication treatment time is 6 hours, and mixing machine revolving speed 650/rps is arranged, and is dried in vacuo after keeping 60/min, and polymer graphite is obtained
Alkene quantum dot soil-solidified-agent powder.
4. a kind of graphene quantum dot soil-solidified-agent preparation method according to claim 1, which is characterized in that polymerizeing
In object graphene quantum dot solution preparation method and step, the phytic acid powder is selected as 150 parts；The waterglass is preferred
It is 150 parts；It is preferred that modulus of water glass 2.8-3.5, Baume degrees 2.4~32.4；The sodium tripolyphosphate is preferably 150 parts；It is described
Multiple water is preferably 600 parts of multiple water.
5. a kind of graphene quantum dot soil-solidified-agent preparation method according to claim 1, which is characterized in that polymerizeing
For object graphene quantum dot inflation fluid by the following method and in step, the polyethylene glycol is preferably 150 parts；The sulfomethylated lignin
Sour sodium is preferably 180 parts；The sulfonated oil is preferably 250 parts；The acidified sodium silicate solution is preferably 600 parts；It is wherein described
Acidified sodium silicate solution is in parts by weight: 150 parts of dilute sulfuric acid, concentration 15% with 150 parts of waterglass, modulus 2.8-3.5, Baume degrees
2.4~32.4 compositions.
6. a kind of graphene quantum dot soil-solidified-agent preparation method according to claim 1, which is characterized in that polymerizeing
In object graphene quantum dot surface-active liquid and preparation method thereof and step, the phytic acid powder is preferably 150 parts；It is preferred that flesh
Content >=50% of six phosphoric acid of alcohol, molecular formula are as follows: C6H18O24P6；
The calcium formate is preferably 120 parts；The magnesia is preferably 200 parts；The sodium chloride is preferably 250 parts；The sulphur
Sour sodium is preferably 250 parts；The calcium chloride is preferably 400 parts；The multiple water is preferably 800 parts.
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| Title |
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| 朱安伟 等: "《基于无机-有机功能纳米材料检测金属离子及其生物成像》", 31 August 2017, 同济大学出版社 * |
| 胡超凡: "《光学功能化石墨烯基纳米材料的制备及其生物医学中的应用》", 30 June 2016, 山西科学技术出版社 * |
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Application publication date: 20191112 |