CN109735161A - A kind of graphene dispersion agent and its preparation method and application - Google Patents

A kind of graphene dispersion agent and its preparation method and application Download PDF

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Publication number
CN109735161A
CN109735161A CN201811485544.6A CN201811485544A CN109735161A CN 109735161 A CN109735161 A CN 109735161A CN 201811485544 A CN201811485544 A CN 201811485544A CN 109735161 A CN109735161 A CN 109735161A
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dispersion agent
trimethylolpropane
graphene dispersion
solution
preparation
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胡玥
范新传
陈奠宇
卢佳晨
张懿俊
牛俊
陈孝峰
李宁燕
赵世健
陈子寅
陆建军
安孟可
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Changshu Institute of Technology
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Changshu Institute of Technology
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Abstract

The invention discloses a kind of graphene dispersion agent and its preparation method and application, which is prepared by following raw material: trimethylolpropane-three (3- aziridinyl propionic ester), polyacrylic resin, organic amine, acidic catalyst, water and ethyl alcohol;Trimethylolpropane-three (3- aziridinyl propionic ester) is made the preparation method comprises the following steps: first being reacted by trimethylolpropane trimethacrylate and aziridine, trimethylolpropane-three (3- aziridinyl propionic ester) and organic amine are reacted in acidic catalyst agent solution and form star-like surfactant again, finally the surfactant is connected on the polyacrylic resin with carboxyl, obtains a kind of dispersing agent of structure novel.Graphene dispersion agent prepared by the present invention is applied in the epoxy zinc rich primer of containing graphene, the dispersibility of graphene can be significantly improved, to reduce the dosage of zinc powder in priming paint, improve the utilization rate of zinc powder.

Description

A kind of graphene dispersion agent and its preparation method and application
Technical field
The present invention relates to technical field of organic synthesis, more particularly to a kind of graphene dispersion agent and its preparation side Method and application.
Background technique
Since human society enters the steel epoch, the harm of corrosion is just like the shadow following the person-and it is just as a kind of slow poison, development Process is extremely slow, is easily ignored by people.China every year because corrosion caused by economic loss account for about annual GDP 3.34%, more than 2,000,000,000,000 yuans, corrosion results in high-cost loss, and global researcher has been promoted to constantly look for subtracting The measure corroded less.
Currently, researcher explored many effective methods will corrosion minimize, organic coating (mono-/multi- at Point, composite material and blend etc.) it is one of most widely used corrosion control strategy, epoxy zinc rich primer is as organic anti-corrosive One kind of coating is used widely with excellent physical mechanical property and antiseptic property, high but there is also hardness of paint films, Flexibility and the poor disadvantage of impact resistance.Moreover, it in the corrosive environment of some harshnesses, needs by increasing epoxy The mode of zinc rich primer coating thickness improves antiseptic property, this just increases painting cost and later maintenance cost.
Graphene be one kind by carbon atom with sp2Hybridized orbit forms the flat film that hexagon is in honeycomb lattice, only There is the two-dimensional material of a carbon atom thickness.Graphene is most thin, the most tough nano material being currently known, breaking strength 200 times more taller than best steel;Its thermal coefficient is up to 5300W/mK, its electron mobility is more than under room temperature 15000cm2/ Vs, and resistivity about 10-6Ω·cm;In addition to this, graphene also has the specific surface area, excellent of super large Permeability resistance, high thermal stability and the advantages that chemical stability, these characteristics make it in the mechanical property for promoting coating and There is huge application potential in terms of Corrosion Protection.Graphene is added in epoxy zinc rich primer, one side graphene can To replace part zinc powder therein to reduce the dosage of zinc powder and reduce cost, the shielding of paint film on the other hand can also be improved Energy.
But powerful Van der Waals force and high-specific surface area is easily clumped together graphene, limit it makes extensively With.It is modified and dispersed graphite alkene studies have shown that a variety of methods can be used, such as oxidation-reduction method is to graphene table Face is modified the purpose that can reach dispersion.However, during being modified using oxidation-reduction method to graphene aqueous solution, it is past The application effect of graphene is influenced toward because graphene dispersion is ineffective or the anti-settling time is too short.Existing graphene dispersion Agent includes: neopelex (SDBS), 1- pyrene formic acid, 1- pyrene sulfonic acid etc., Arabic gum, polyvinylpyrrolidone (PVP) etc., there are also the complicated organic molecule of synthesis, but these graphene dispersion agent dispersed graphite alkene in aqueous solution Ability it is very limited, dispersion performance is bad.
Therefore, how to provide a kind of graphene dispersion agent of good dispersion property is those skilled in the art's urgent need to resolve Problem.
Summary of the invention
In view of this, the purpose of the present invention is to provide a kind of graphene dispersion agent and its preparation method and application, this point Powder can rapidly dispersed graphite alkene and for a long time do not reunite, for improving the mechanical property and anticorrosive property of epoxy zinc rich primer Energy.
To achieve the goals above, the present invention provides a kind of graphene dispersion agent, are prepared by the raw material of following parts by weight It obtains: 40-50 parts of trimethylolpropane-three (3- aziridinyl propionic ester), 20-25 parts of polyacrylic resin, organic amine 8-12 Part, 1-3 parts of acidic catalyst, 25-30 parts of water and 5-10 parts of ethyl alcohol.
The beneficial effects of the present invention are:
(1) present invention with aziridine crosslinker-trimethylolpropane-three (3- aziridinyl propionic ester) of high activity and lives Bold and vigorous amido reacts the star-like surfactant to be formed and carry active secondary amine, then reacts with the polyacrylic resin with carboxyl, by table Face activating agent is connected on the polyacrylic resin with carboxyl, obtains a kind of dispersing agent of structure novel;
(2) present invention introduces quaternary ammonium salt cationic on dispersant molecule chain, increases the hydration capability and heat of dispersing agent Stability;
(3) present invention introduces a large amount of carboxylic acid ions on dispersant molecule chain, can make dispersant molecule and graphene Combination can it is fully dispersed in water, enhance graphene particle between repulsive interaction, increase its dispersion effect.
Further, above-mentioned organic amine be methylamine or ethamine,
Further, above-mentioned acidic catalyst is any one in phosphoric acid, sulfuric acid or hydrofluoric acid,
Further, above-mentioned ethyl alcohol is dehydrated alcohol.
It is using above-mentioned further beneficial effect, methylamine or ethamine belong to the relatively simple organic amine object of structure Matter, convenient for the ring-opening reaction of aziridine;Phosphoric acid, sulfuric acid or hydrofluoric acid have determining acid strength and acid as acidic catalyst Type, and have quite high catalytic activity at a lower temperature.
The present invention also provides the preparation methods of above-mentioned graphene dispersion agent, including following operating procedure:
(1) weigh each raw material by above-mentioned parts by weight, then by trimethylolpropane-three (3- aziridinyl propionic ester), Organic amine and acidic catalyst respectively it is soluble in water be configured to trimethylolpropane-three (3- aziridinyl propionic ester) aqueous solution, Polyacrylic resin is dissolved in the ethyl alcohol that ethyl alcohol is configured to polyacrylic resin by organic amine aqueous solution and acidic catalyst aqueous solution Solution;
(2) organic amine aqueous solution and acidic catalyst aqueous solution are mixed, under continuous agitation, to mixed solution In trimethylolpropane-three (3- aziridinyl propionic ester) aqueous solution is slowly added dropwise, stop stirring after being added dropwise, heating is anti- It answers;
(3) reaction solution in step (2) is adjusted to pH=8-9, under continuous agitation, by polyacrylic resin Ethanol solution is slowly dropped in reaction solution, temperature reaction;
(4) it filters after reaction, concentration of reaction solution is isolated and purified with product, is dried under vacuum to constant weight up to above-mentioned stone Black alkene dispersing agent.
The beneficial effects of the present invention are:
(1) trimethylolpropane-three (3- aziridinyl propionic ester) under the catalytic action of acidic catalyst with organic amine Aziridine ring-opening reaction occurs, adds the ethanol solution temperature reaction of polyacrylic resin, aziridine type prepolymer is connected Onto polyacrylic resin, a kind of dispersing agent of special construction is obtained;
(2) the preparation method reaction condition is mild, and reagent and equipment are fairly simple, and operating procedure is simple, and cost of manufacture It is lower, facilitate implementation.
Further, above-mentioned trimethylolpropane-three (3- aziridinyl propionic ester) the preparation method comprises the following steps: by trihydroxy methyl third The dichloroethane solution of alkane triacrylate is added in aziridine aqueous solution, continues insulated and stirred after being sufficiently mixed to get upper State trimethylolpropane-three (3- aziridinyl propionic ester).
Preferably, the mass fraction of the dichloroethane solution of above-mentioned trimethylolpropane trimethacrylate be 60%~ 70%, the mass fraction of above-mentioned aziridine aqueous solution is 70-75%, above-mentioned trimethylolpropane trimethacrylate and aziridine Molar ratio is 1: 2.8~3.2, and above-mentioned heat-retaining condition is 12-15 DEG C, and above-mentioned mixing time is 10-12h.
It is using above-mentioned further beneficial effect, after trimethylolpropane trimethacrylate is dissolved in dichloroethane solution Addition reaction occurs with aziridine aqueous solution, trimethylolpropane-three (3- aziridinyl propionic ester), the preparation method item is made Part is mild, and one step of reaction is completed, and simplifies practical operation step, and yield is higher, reduces production cost.
Further, the mass fraction of above-mentioned trimethylolpropane-three (3- aziridinyl propionic ester) aqueous solution is 75- 85%, the mass fraction of above-mentioned organic amine aqueous solution is 30-40%, and the mass fraction of above-mentioned acidic catalyst aqueous solution is 50- 60%, the mass fraction of above-mentioned polyacrylic resin ethanol solution is 70-80%.
It is using above-mentioned further beneficial effect, by organic amine, acidic catalyst and (the 3- a word used for translation of trimethylolpropane-three Third piperidinyl propionic ester) be dissolved in water after, increase the contact area of each reactant, be more advantageous to the progress of ring-opening reaction;Polypropylene The acid resin lotion soluble in water that will form hinders reaction to carry out, and has very high solubility in ethanol, so selection quality Score is the polyacrylic resin ethanol solution of 70-80%.
Further, the stirring in step (2) is magnetic agitation, speed of agitator 150-200r/min, mixing time 45- 60min;It is warming up to 70-80 DEG C of reaction 6-8h.
It is that magnetic agitation 45-60min can make (the 3- of trimethylolpropane-three using above-mentioned further beneficial effect Aziridinyl propionic ester) and organic amine aziridine ring-opening reaction is sufficiently carried out under the action of acidic catalyst;It is warming up to 70- 80 DEG C provide suitable reaction temperature for reaction, accelerate the progress of reaction.
Further, the stirring in step (3) is magnetic agitation, speed of agitator 100-150r/min, mixing time 30- 45min;It is warming up to 70-80 DEG C of reaction 12-14h.
It is using above-mentioned further beneficial effect, magnetic agitation 30-45min can be such that aziridine type prepolymer more fills It is connected on polyacrylic resin with dividing;It is warming up to 70-80 DEG C and provides suitable reaction temperature for reaction, accelerate reaction It carries out.
The present invention also provides application of the above-mentioned graphene dispersion agent in epoxy zinc rich primer.
It can be seen via above technical scheme that the present disclosure provides a kind of graphene dispersion agent and preparation method thereof and Using compared with prior art, dispersing agent prepared by the present invention has splendid hydration capability and thermal stability, special structure The steric restriction effect between graphene particle is increased, dispersion effect is more efficient, and dispersion stabilization is good.The present invention is made Standby graphene dispersion agent is applied in the epoxy zinc rich primer of containing graphene, can significantly improve the dispersibility of graphene, from And the dosage of zinc powder in priming paint is reduced, improve the utilization rate of zinc powder.
Specific embodiment
The following is a clear and complete description of the technical scheme in the embodiments of the invention, it is clear that described embodiment Only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, the common skill in this field Art personnel every other embodiment obtained without making creative work belongs to the model that the present invention protects It encloses.
In following embodiment, trimethylolpropane-three (3- aziridinyl propionic ester) the preparation method comprises the following steps:
60g trimethylolpropane trimethacrylate is taken to be dissolved in the dichloroethanes of 40mL, then taking mass fraction is 70% nitrogen The dichloroethane solution of trimethylolpropane trimethacrylate is slowly added by the third pyridine aqueous solution 30g under conditions of 13 DEG C In aziridine aqueous solution, after adding, reaction system insulated and stirred 10 hours at 13 DEG C, stratification extracts lower layer's organic phase, It is evaporated under reduced pressure at 40 DEG C, after removing solvent, obtains trimethylolpropane-three (3- aziridinyl propionic ester).
Embodiment 1
Graphene dispersion agent is prepared by the raw material of following weight: (the 3- aziridinyl propionic acid of trimethylolpropane-three Ester) 40g, polyacrylic resin 20g, methylamine 8g, phosphatase 11 g, water 27g and ethyl alcohol 8g.
The preparation method of graphene dispersion agent, including following operating procedure:
(1) each raw material is weighed by above-mentioned weight;
It (2) (is wherein 50% containing methylamine 8g) and 2g mass fraction by the methylamine water solution that 24g mass fraction is 30% Phosphoric acid solution (wherein phosphoric acid 1g) is uniformly mixed, molten to mixing under conditions of revolving speed is that 150r/min continuing magnetic force stirs Trimethylolpropane-three (3- aziridinyl propionic ester) aqueous solution that 50g mass fraction is 80% is slowly added dropwise in liquid (wherein to contain Trimethylolpropane-three (3- aziridinyl propionic ester) 40g), time for adding 45min stops stirring, heating after being added dropwise To 70 DEG C of reaction 6h;
(3) reaction solution in step (2) is adjusted to the alkalescent of pH value of solution=8 with NaOH, is 100r/ in speed of agitator Min continuing magnetic force stirring stirring under conditions of, by 28g mass fraction be 70% polyacrylic resin ethanol solution (wherein It is slowly dropped in reaction solution containing polyacrylic resin 20g), time for adding 30min, stops stirring, heating after being added dropwise To 70 DEG C of reaction 12h;
(4) it is filtered to remove insoluble matter after reaction, concentration of reaction solution is isolated and purified with product, is dried under vacuum to perseverance Weight is up to the graphene dispersion agent.
Embodiment 2
Graphene dispersion agent is prepared by the raw material of following weight: (the 3- aziridinyl propionic acid of trimethylolpropane-three Ester) 50g, polyacrylic resin 25g, methylamine 12g, phosphoric acid 3g, water 29g and ethyl alcohol 6g.
The preparation method of graphene dispersion agent, including following operating procedure:
(1) each raw material is weighed by above-mentioned weight;
It (2) (is wherein 60% containing methylamine 12g) and 5g mass fraction by the ethylamine solution that 30g mass fraction is 40% Phosphoric acid solution (wherein phosphoric acid 3g) is uniformly mixed, molten to mixing under conditions of revolving speed is that 200r/min continuing magnetic force stirs Trimethylolpropane-three (3- aziridinyl propionic ester) aqueous solution that 59g mass fraction is 85% is slowly added dropwise in liquid (wherein to contain Trimethylolpropane-three (3- aziridinyl propionic ester) 50g), time for adding 60min stops stirring, heating after being added dropwise To 80 DEG C of reaction 8h;
(3) reaction solution in step (2) is adjusted to the alkalescent of pH value of solution=9 with NaOH, is 150r/ in speed of agitator Min continuing magnetic force stirring stirring under conditions of, by 31g mass fraction be 80% polyacrylic resin ethanol solution (wherein It is slowly dropped in reaction solution containing polyacrylic resin 25g), time for adding 45min, stops stirring, heating after being added dropwise To 80 DEG C of reaction 14h;
(4) it is filtered to remove insoluble matter after reaction, concentration of reaction solution is isolated and purified with product, is dried under vacuum to constant weight Up to the graphene dispersion agent.
Embodiment 3
Graphene dispersion agent is prepared by the raw material of following weight: (the 3- aziridinyl propionic acid of trimethylolpropane-three Ester) 45g, polyacrylic resin 22g, methylamine 10g, phosphoric acid 2g, water 30g and ethyl alcohol 8g.
The preparation method of graphene dispersion agent, including following operating procedure:
(1) each raw material is weighed by above-mentioned weight;
It (2) (is wherein 50% containing methylamine 10g) and 4g mass fraction by the methylamine water solution that 25g mass fraction is 40% Phosphoric acid solution (wherein phosphoric acid 2g) is uniformly mixed, molten to mixing under conditions of revolving speed is that 180r/min continuing magnetic force stirs Trimethylolpropane-three (3- aziridinyl propionic ester) aqueous solution that 56g mass fraction is 80% is slowly added dropwise in liquid (wherein to contain Trimethylolpropane-three (3- aziridinyl propionic ester) 45g), time for adding 50min stops stirring, heating after being added dropwise To 75 DEG C of reaction 7h;
(3) reaction solution in step (2) is adjusted to the alkalescent of pH value of solution=8 with NaOH, is 120r/ in speed of agitator Min continuing magnetic force stirring stirring under conditions of, by 30g mass fraction be 75% polyacrylic resin ethanol solution (wherein It is slowly dropped in reaction solution containing polyacrylic resin 22g), time for adding 40min, stops stirring, heating after being added dropwise To 75 DEG C of reaction 13h;
(4) it is filtered to remove insoluble matter after reaction, concentration of reaction solution is isolated and purified with product, is dried under vacuum to perseverance Weight is up to the graphene dispersion agent.
Performance test
1, three kinds of graphene dispersion agent for preparing embodiment 1-3 carry out after mixing respectively with graphene in 1: 10 ratio Preimpregnation dispersion, by three kinds of mixtures respectively with 0,0.5%, 0.8%, 1.0%, 1.5% and 2.0% amount and epoxy resin, molten Agent, auxiliary agent, pigments and fillers are added sequentially to mix in stainless steel barrel, high speed dispersion, are eventually adding zinc powder, high speed dispersion 60min, Discharging, obtained epoxy zinc rich primer is respectively as experimental group A, experimental group B and experimental group C.
Selection specification is three blocks of steel plates of 15mm × 10mm × 5mm, respectively with experimental group A, experimental group B and experimental group C Epoxy zinc rich primer carries out blasting treatment according to GB/T 8923.1-2011, and paint film coating thickness is 100um, is meeting GB/T After conserving 10d under the conditions of as defined in 9278-2008, experimental group A coating carries out salt fog resistance test according to GB/T 1771-2007, Experimental group B coating carries out the test of paint film impact resistance according to GB/T 20624-2006, and experimental group C coating is according to GB/T 5210- 2006 carry out adhesive force test, and test result is as shown in table 1.
1 experimental group A, B, C test result of table
As can be seen from Table 1, addition graphene dispersion agent has better salt spray resistance with the coating after graphene mixture Property, impact resistance and adhesive force, and with the increase of graphene dispersion agent and graphene mixture content, the salt spray resistance of coating Property, impact resistance and adhesive force be all first to increase afterwards to reduce, applied when it is 1% that graphene dispersion agent is with graphene mixture content Salt fog resistance, impact resistance and the adhesive force of layer reach best.
2, preimpregnation dispersion is carried out after mixing graphene dispersion agent prepared by embodiment 3 and graphene in 1: 10 ratio, Mixture is added sequentially to mix in stainless steel barrel with 1.0% amount with epoxy resin, solvent, auxiliary agent, pigments and fillers, high speed Dispersion is eventually adding 25% zinc powder, and high speed dispersion 60min, discharging, obtained epoxy zinc rich primer is as experimental group 1.
1% graphene is subjected to preimpregnation dispersion, then successively adds epoxy resin, solvent, auxiliary agent, pigments and fillers and graphite Entering into stainless steel barrel and mixes, high speed dispersion is separately added into the zinc powder that mass fraction is 0,25%, 50%, 75%, 80%, High speed dispersion 60min, discharging obtain containing graphene but the epoxy zinc rich primer without graphene dispersion agent respectively as experimental group 2, experimental group 3, experimental group 4, experimental group 5 and experimental group 6.
Selection specification be six blocks of steel plates of 15mm × 10mm × 5mm, respectively with experimental group 1-6 epoxy zinc rich primer according to GB/T 8923.1-2011 carries out blasting treatment, and paint film coating thickness is 100um, is meeting item as defined in GB/T 9278-2008 After conserving 10d under part, salt fog resistance test is carried out according to GB/T 1771-2007 respectively, is carried out according to GB/T 20624-2006 The test of paint film impact resistance, coating carry out adhesive force test according to GB/T 5210-2006, and test result is as shown in table 2.
2 experimental group 1-6 test result of table
As can be seen from Table 2, the compound painting of zinc alkene containing 1% graphene dispersion agent and graphene mixture and zincilate 25% Material relative to containing 1% graphene but without graphene dispersion agent, the coating below of zincilate 50% have better salt fog resistance, Impact resistance and adhesive force.
The above experimental result is shown, graphene dispersion agent prepared by the present invention is applied to the epoxy zinc-rich bottom of containing graphene Qi Zhong, can significantly improve the dispersibility of graphene, to reduce the dosage of zinc powder in priming paint, improve the utilization rate of zinc powder.
The foregoing description of the disclosed embodiments enables those skilled in the art to implement or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, as defined herein General Principle can be realized in other embodiments without departing from the spirit or scope of the present invention.Therefore, of the invention It is not intended to be limited to the embodiments shown herein, and is to fit to and the principles and novel features disclosed herein phase one The widest scope of cause.

Claims (10)

1. a kind of graphene dispersion agent, which is characterized in that be prepared by the raw material of following parts by weight: trimethylolpropane-three 40-50 parts of (3- aziridinyl propionic ester), 20-25 parts of polyacrylic resin, 8-12 parts of organic amine, 1-3 parts of acidic catalyst, water 25-30 parts and ethyl alcohol 5-10 parts.
2. a kind of graphene dispersion agent according to claim 1, which is characterized in that the organic amine be methylamine or ethamine, The acidic catalyst is any one in phosphoric acid, sulfuric acid or hydrofluoric acid, and the ethyl alcohol is dehydrated alcohol.
3. a kind of preparation method of graphene dispersion agent, which is characterized in that including following operating procedure:
(1) each raw material is weighed by the parts by weight of graphene dispersion agent described in claim any one of 1-2, then by three hydroxyl first Base propane-three (3- aziridinyl propionic ester), organic amine and acidic catalyst is soluble in water respectively is configured to trimethylolpropane- Three (3- aziridinyl propionic ester) aqueous solution, organic amine aqueous solution and acidic catalyst aqueous solutions, polyacrylic resin is dissolved in Ethyl alcohol is configured to the ethanol solution of polyacrylic resin;
(2) organic amine aqueous solution and acidic catalyst aqueous solution are mixed, under continuous agitation, is delayed into mixed solution It is slow that trimethylolpropane-three (3- aziridinyl propionic ester) aqueous solution is added dropwise, stop stirring, temperature reaction after being added dropwise;
(3) reaction solution in step (2) is adjusted to pH value of solution=8-9, under continuous agitation, by polyacrylic resin Ethanol solution is slowly dropped in reaction solution, temperature reaction;
(4) it filters after reaction, concentration of reaction solution is isolated and purified with product, is dried under vacuum to constant weight up to the graphene Dispersing agent.
4. a kind of preparation method of graphene dispersion agent according to claim 3, which is characterized in that described in step (1) Trimethylolpropane-three (3- aziridinyl propionic ester) the preparation method comprises the following steps: by the dichloro of trimethylolpropane trimethacrylate Ethane solution is added in aziridine aqueous solution, continues insulated and stirred after being sufficiently mixed to get the trimethylolpropane-three (3- aziridinyl propionic ester).
5. a kind of preparation method of graphene dispersion agent according to claim 4, which is characterized in that the trihydroxy methyl third The mass fraction of the dichloroethane solution of alkane triacrylate is 60%~70%, and the mass fraction of the aziridine aqueous solution is The molar ratio of 70-75%, the trimethylolpropane trimethacrylate and aziridine is 1: 2.8~3.2.
6. a kind of preparation method of graphene dispersion agent according to claim 4, which is characterized in that the heat-retaining condition is 12-15 DEG C, the mixing time is 10-12h.
7. a kind of preparation method of graphene dispersion agent according to claim 3, which is characterized in that described in step (1) The mass fraction of trimethylolpropane-three (3- aziridinyl propionic ester) aqueous solution is 75-85%, organic amine aqueous solution Mass fraction is 30-40%, and the mass fraction of the acidic catalyst aqueous solution is 50-60%, the polyacrylic resin second The mass fraction of alcoholic solution is 70-80%.
8. a kind of preparation method of graphene dispersion agent according to claim 3, which is characterized in that described in step (2) Stirring is magnetic agitation, speed of agitator 150-200r/min, mixing time 45-60min;It is warming up to 70-80 DEG C of reaction 6- 8h。
9. a kind of preparation method of graphene dispersion agent according to claim 3, which is characterized in that described in step (3) Stirring is magnetic agitation, speed of agitator 100-150r/min, mixing time 30-45min;It is warming up to 70-80 DEG C of reaction 12- 14h。
10. a kind of such as application of the described in any item graphene dispersion agent of claim 1-2 in epoxy zinc rich primer.
CN201811485544.6A 2018-12-05 2018-12-05 A kind of graphene dispersion agent and its preparation method and application Pending CN109735161A (en)

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Publication number Priority date Publication date Assignee Title
CN110655596A (en) * 2019-10-18 2020-01-07 常州碳孚新材料技术有限公司 Star-shaped cationic graphene dispersant and application thereof
CN110655596B (en) * 2019-10-18 2021-10-01 常州碳孚新材料技术有限公司 Star-shaped cationic graphene dispersant and application thereof

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Application publication date: 20190510