CN111117372A - Reactive color paste and preparation method thereof - Google Patents
Reactive color paste and preparation method thereof Download PDFInfo
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- CN111117372A CN111117372A CN201911384272.5A CN201911384272A CN111117372A CN 111117372 A CN111117372 A CN 111117372A CN 201911384272 A CN201911384272 A CN 201911384272A CN 111117372 A CN111117372 A CN 111117372A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D17/00—Pigment pastes, e.g. for mixing in paints
- C09D17/004—Pigment pastes, e.g. for mixing in paints containing an inorganic pigment
- C09D17/005—Carbon black
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
- B01F35/20—Measuring; Control or regulation
- B01F35/22—Control or regulation
- B01F35/221—Control or regulation of operational parameters, e.g. level of material in the mixer, temperature or pressure
- B01F35/2214—Speed during the operation
- B01F35/22142—Speed of the mixing device during the operation
- B01F35/221422—Speed of rotation of the mixing axis, stirrer or receptacle during the operation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
- B01F35/20—Measuring; Control or regulation
- B01F35/22—Control or regulation
- B01F35/221—Control or regulation of operational parameters, e.g. level of material in the mixer, temperature or pressure
- B01F35/2215—Temperature
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/44—Carbon
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/44—Carbon
- C09C1/48—Carbon black
- C09C1/56—Treatment of carbon black ; Purification
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- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/04—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
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- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/06—Treatment with inorganic compounds
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/08—Treatment with low-molecular-weight non-polymer organic compounds
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
- C09D11/037—Printing inks characterised by features other than the chemical nature of the binder characterised by the pigment
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- C09D17/00—Pigment pastes, e.g. for mixing in paints
- C09D17/002—Pigment pastes, e.g. for mixing in paints in organic medium
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- C09D17/00—Pigment pastes, e.g. for mixing in paints
- C09D17/004—Pigment pastes, e.g. for mixing in paints containing an inorganic pigment
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- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/60—Additives non-macromolecular
- C09D7/61—Additives non-macromolecular inorganic
- C09D7/62—Additives non-macromolecular inorganic modified by treatment with other compounds
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/65—Additives macromolecular
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F2101/00—Mixing characterised by the nature of the mixed materials or by the application field
- B01F2101/30—Mixing paints or paint ingredients, e.g. pigments, dyes, colours, lacquers or enamel
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- Chemical Kinetics & Catalysis (AREA)
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Abstract
The invention relates to a reactive color paste and a preparation method thereof, wherein the reactive color paste comprises the following raw materials in parts by weight: the paint comprises a styrene-maleic anhydride copolymer, an aminated pigment and a diluent, wherein the styrene-maleic anhydride copolymer and the aminated pigment are added in an amount such that the molar weight ratio of maleic anhydride to the molar weight of amino is 1:1-1:2, and the diluent is added to adjust the viscosity to be in a range of 20-100 s. Stirring and mixing the styrene-maleic anhydride copolymer and the aminated pigment uniformly under the addition of the diluent; heating to 90-150 ℃ and reacting for 2.0-6.0h to obtain the reactive color paste. Compared with the prior art, the color paste has good storage stability, good dispersibility and color developability for other pigments and fillers, can form a color paste system with good performance, and can be widely applied to the fields of coatings and printing ink.
Description
Technical Field
The invention relates to the field of paint and ink color paste, in particular to reactive color paste and a preparation method thereof.
Background
At present, with the development of technology and industry, the requirements of products such as paint and ink on color are almost strict, which depends on high-performance color paste, and the traditional color paste dispersing process is to fully disperse and grind pigment and dispersant in an organic solvent medium to form color paste with uniform texture. However, such mill base systems formed by physical mechanical action are unstable, have short storage times and are prone to agglomerate and settle, thereby causing various problems in paints and inks using these mill bases, such as flooding, blooming, pigment particles, and the like.
As for the hyperdispersant of the styrene-maleic anhydride system, the styrene has a benzene ring structure, so that the dispersion effect on the phthalocyanine pigment is good, and the maleic anhydride is used as an anchoring group for dispersing the inorganic filler, so that the research on the dispersant is focused. On a microscopic level, the dispersion of such dispersants on pigments also rests on molecular scales such as van der waals forces, hydrogen bonding, and charge attraction.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a reactive color paste which has good storage stability, has the performance of dispersing other pigments and is formed by linking chemical covalent bonds and a preparation method thereof.
The purpose of the invention can be realized by the following technical scheme:
the reactive color paste comprises raw materials of styrene-maleic anhydride copolymer, aminated pigment and diluent, wherein the addition amount of the styrene-maleic anhydride copolymer and the aminated pigment is such that the ratio of the molar weight of maleic anhydride to the molar weight of amino is 1 (1-2), the addition amount of the diluent is such that the viscosity of the color paste is adjusted to be between 20 and 100s, and the measuring condition is to coat a No. 4 cup.
Furthermore, the molecular weight of the styrene-maleic anhydride copolymer is between 1000-10000, the molecular weight distribution index is between 1.0-2.0, the styrene-maleic anhydride copolymer is any one of trackless, block and alternating structures, and the molar ratio of the maleic anhydride monomer is between 30-80%; the diluent comprises one or two of butyl acetate or ethyl acetate.
Further, the aminated pigment comprises aminated carbon black or aminated carbon nanotube, and is prepared by the following method:
(1) surface modification of carbon black or carbon nanotubes: ultrasonically dispersing carbon black or carbon nano tubes in a solvent, adding an initiator, introducing inert gas for protection, and then carrying out initiation reaction; then filtering and separating, and washing with a solvent to obtain surface modified carbon black or surface modified carbon nano tubes;
(2) hydrolyzing the surface-modified carbon black or the surface-modified carbon nanotubes: adding the surface modified carbon black or the surface modified carbon nano tube into an aqueous solution, refluxing, filtering and separating, washing with deionized water, and finally drying to obtain carboxyl modified carbon black or carboxyl modified carbon nano tube;
(3) acylating chlorination of the carboxyl modified carbon black or the carboxyl modified carbon nanotube: putting the carboxyl modified carbon black or the carboxyl modified carbon nano tube into a solvent, heating, condensing, refluxing, decompressing, filtering, repeatedly washing and drying to obtain the acyl chlorinated carbon black or the acyl chlorinated carbon nano tube;
(4) amidating an acyl-chlorinated carbon black or an acyl-chlorinated carbon nanotube: adding excessive ammonium carbonate and concentrated ammonia water into the acyl chlorinated carbon black or the acyl chlorinated carbon nano tube, stirring for reaction, filtering, repeatedly washing with distilled water, and drying to obtain amidated carbon black or amidated carbon nano tube;
(5) amination of amidated carbon black or amidated carbon nanotubes: putting the amidated carbon black or the amidated carbon nano tube into ice water, adding excessive sodium hypochlorite for 20-40min, carrying out stirring reaction, heating the mixture to carry out water bath reaction, then cooling and filtering, washing the mixture by distilled water, and drying the washed product to obtain the aminated carbon black or the aminated carbon nano tube.
Further, the carbon nanotubes in step (1) comprise single-walled carbon nanotubes or multi-walled carbon nanotubes; the solvent comprises one or more of toluene, tetrahydrofuran, N-dimethylformamide or N-methylpyrrolidone; the initiator comprises one or more of azobisisobutyronitrile, azobisisoheptonitrile, azobisisooctonitrile, 2 '-azobis (2, 4-dimethylvaleronitrile) or 1, 1' -azobis (cyclohexanecarbonitrile); the mass volume ratio of the carbon black or the carbon nano tube, the solvent and the initiator is (20-35) mg, (2-20) g:50ml, the frequency of the ultrasonic is 30-90kHz, and the time is 30-60 min; the inert gas comprises nitrogen or argon, and the protection time is 20-40 min; the reaction temperature is 60-80 ℃ and the reaction time is 90-150 min; the filtration adopts a polyvinylidene fluoride membrane or a polytetrafluoroethylene membrane with the aperture of 0.30-0.60 mu m; the number of washing times is 3-5.
Further, the aqueous solution in the step (2) includes an acid solution or an alkali solution, the acid solution is configured by one or more of hydrochloric acid, sulfuric acid and phosphoric acid, the concentration of the acid solution is 0.5-2mol/L, the alkali solution is configured by sodium hydroxide or potassium hydroxide, and the concentration of the alkali solution is 0.5-2 mol/L; the mass-volume ratio of the surface modified carbon black or the surface modified carbon nano tube to the aqueous solution is (20-60) mg:50 ml; the refluxing time is 90-150min, and the filtration adopts a polyvinylidene fluoride membrane or a polytetrafluoroethylene membrane with the pore diameter of 0.30-0.60 mu m; the washing times are 3-5 times, the drying temperature is 35-50 ℃, the pressure is-0.09-0.01 MPa, and the time is 60-120 min.
Further, the solvent in the step (3) comprises dimethyl sulfoxide or N, N-dimethylformamide; the mass volume ratio of the carboxyl modified carbon black or the carboxyl modified carbon nano tube to the solvent is (20-60) mg:50 ml; the temperature of the heating, condensing and refluxing is 60-80 ℃, the time is 12-36h, the suction filtration adopts a polyvinylidene fluoride membrane or a polytetrafluoroethylene membrane with the aperture of 0.30-0.60 mu m, the pressure of the suction filtration is-0.09 MPa to-0.01 MPa, and tetrahydrofuran is selected as a washing agent for washing; the drying temperature is 35-50 ℃, the pressure is-0.09-0.01 MPa, and the time is 60-120 min.
Further, the concentration of the concentrated ammonia water in the step (4) is 8-10mol/L, the mass volume ratio of the carbon black or carbon nano tube, ammonium carbonate and concentrated ammonia water is (20-35) mg (2-20) mg:50ml, the stirring speed of the stirring reaction is 150-200rpm, the time is 5-10h, and the filtration adopts a polyvinylidene fluoride membrane or a polytetrafluoroethylene membrane with the aperture of 0.30-0.60 mu m; the washing times are 3-5 times, the drying temperature is 35-50 ℃, the pressure is-0.09-0.01 MPa, and the time is 60-120 min.
Further, the mass-volume ratio of the amidated carbon black or the amidated carbon nano-tube, the sodium hypochlorite and the water in the step (5) is (20-35) mg, the mass-volume ratio of (20-50) mg to 50ml, the stirring speed of the stirring reaction is 150-200rpm, the temperature is 0-5 ℃, the time is 1-5h, the temperature of the water bath reaction is 60-80 ℃, the time is 1-5h, the suction filtration adopts a polyvinylidene fluoride membrane or a polytetrafluoroethylene membrane with the aperture of 0.30-0.60 mu m, the pressure of the suction filtration is-0.09-0.01 MPa, and the washing times are 3-5 times; the drying temperature is 35-50 ℃, the pressure is-0.09-0.01 MPa, and the time is 60-120 min.
The preparation method of the reactive color paste comprises the steps of uniformly stirring and mixing the styrene-maleic anhydride copolymer and the aminated pigment according to the proportion, adding the diluent to adjust the viscosity, and then heating for reaction to obtain the reactive color paste.
Further, the rotation speed of the stirring and mixing is 150-200rpm, the time is 1-5h, the temperature of the heating reaction is 90-150 ℃, and the time is 2-6 h.
The pressure in the invention refers to gauge pressure, and absolute pressure is larger than the value of gauge pressure by one atmosphere.
Intermolecular forces are also difficult to achieve relative to the stability provided by covalent bonds. The development of surface modification of carbon black and carbon nano tubes as common black pigments provides new possibility for realizing a dispersing means in color paste. Currently, various active centers can be conveniently formed on the surface of carbon black pigment by an oxidation method, wherein amino is a common active center.
The invention adopts the mode that maleic anhydride in styrene maleic anhydride copolymer reacts with amino in pigment to form amido bond, and connects the pigment and dispersant resin together by chemical bond. A stable dispersion system is formed, and the problems of sedimentation, thickening and the like of the traditional color paste are avoided.
In fact, the amidation reaction in the invention is a reversible reaction, the reaction of the styrene-maleic anhydride copolymer and the aminated pigment cannot be 100%, the main control factor lies in whether to remove the moisture generated by the reaction in time, because of the introduction of the diluent, the concentration of the reactive center of the whole system is reduced at this time, the difficulty of the reaction of the amino group and the acid anhydride in the pigment is increased, and the gel caused by the cross-linking formed when the multifunctional pigment molecules participate in the reaction is effectively avoided; on the other hand, the probability of the reaction of the active center can be increased by measures of increasing the stirring speed, increasing the reaction temperature and the like, so that the reaction efficiency is improved. By the above two measures, we can control the reaction degree, and do not form a gel system, but make the aminated pigment and the dispersant resin (styrene maleic anhydride copolymer) react effectively.
Therefore, the pigment dispersion system formed by the invention has obvious linkage of covalent bond-amido bond between pigments such as carbon black and the like and the styrene maleic anhydride copolymer dispersant, and has quite superior storage stability compared with the traditional process.
The styrene-maleic anhydride copolymer adopted in the invention contains groups for dispersing other pigments, such as benzene rings which are beneficial to dispersing phthalocyanine pigments, carboxyl groups formed by maleic anhydride which are beneficial to dispersing inorganic pigments, such as titanium dioxide, calcium carbonate and the like. The formed color paste can disperse various organic and inorganic pigments at the same time, and has quite good toner compatibility, dispersibility and color rendering property.
Compared with the prior art, the invention has the following advantages:
(1) the maleic anhydride in the styrene maleic anhydride copolymer reacts with amino in the pigment to form amido bond, the pigment and the dispersing agent resin are linked together by chemical bonds to form a stable dispersing system, the storage stability of the dispersing system is excellent, the adverse phenomena of sedimentation, layering and the like are greatly reduced, and the problems of flooding, floating, sedimentation, thickening and the like of the coating prepared from the dispersing system are avoided;
(2) by introducing the diluent, the concentration of the reactive center of the whole system is reduced, the difficulty of the reaction of amino and acid anhydride in the pigment is increased, and the gel caused by the cross-linking formed by the multi-functional pigment molecules participating in the reaction is effectively avoided;
(3) the probability of the reaction of the active center can be increased by improving the stirring speed, the reaction temperature and other reaction conditions, so that the reaction efficiency is improved, and the crosslinking degree of the reaction is well controlled;
(4) the styrene-maleic anhydride copolymer adopted in the invention contains groups for dispersing other pigments, such as benzene rings which are beneficial to dispersing phthalocyanine pigments, carboxyl groups formed by maleic anhydride which are beneficial to dispersing inorganic pigments, such as titanium dioxide, calcium carbonate and the like. The formed color paste can disperse various organic and inorganic pigments at the same time, and has quite good toner compatibility, dispersibility and color rendering property.
Detailed Description
The following examples are given for the detailed implementation and specific operation of the present invention, but the scope of the present invention is not limited to the following examples.
Example 1
The aminated pigment in the reaction color paste is an aminated carbon nanotube and is prepared by the following method:
(1) carrying out surface modification on the carbon nano tube: ultrasonically dispersing carbon nano tubes in a toluene solvent, adding an initiator azobisisobutyronitrile, introducing nitrogen for protection for 20min, and then carrying out initiation reaction at 60 ℃ for 90 min; then filtering and separating, and washing for 3-5 times by using a solvent toluene to obtain a surface modified carbon nano tube; wherein the mass volume ratio of the carbon nano tube to the solvent to the initiator is 20mg:2g:50ml, the ultrasonic frequency is 30kHz, and the ultrasonic time is 30 min; filtering with polyvinylidene fluoride membrane or polytetrafluoroethylene membrane with pore diameter of 0.30-0.60 μm;
(2) hydrolyzing the surface modified carbon nano tube: adding the surface modified carbon nano tube into 0.5mol/L hydrochloric acid, refluxing for 90min, filtering, separating, washing with deionized water for 3-5 times, and finally drying at 35 ℃ and-0.09 MPa for 60min to obtain the carboxyl modified carbon nano tube; wherein, the mass volume ratio of the surface modified carbon nano tube to the hydrochloric acid is 20mg:50ml, and the polyvinylidene fluoride membrane or the polytetrafluoroethylene membrane with the aperture of 0.30-0.60 mu m is adopted for filtration;
(3) acylating chlorination of the carboxyl modified carbon nano tube: putting the carboxyl modified carbon nano tube into a solvent dimethyl sulfoxide, condensing and refluxing for 12h at 60 ℃, then carrying out vacuum filtration, repeatedly washing for 3-5 times, and drying for 60min at 35 ℃ and-0.09 MPa to obtain an acyl chlorinated carbon nano tube; wherein, the mass volume ratio of the carboxyl modified carbon nano tube to the solvent is 20mg:50ml, the filtration adopts a polyvinylidene fluoride membrane or a polytetrafluoroethylene membrane with the aperture of 0.30-0.60 mu m, the pressure of the filtration is-0.09 MPa, and tetrahydrofuran is selected as a washing agent for washing;
(4) amidating an acyl-chlorinated carbon black or an acyl-chlorinated carbon nanotube: adding excessive ammonium carbonate and concentrated ammonia water into the carbon black or carbon nano tube subjected to acyl chlorination, stirring and reacting at the rotating speed of 150-200rpm, filtering for 5h, repeatedly washing for 3-5 times by using distilled water, and drying for 60min at 35 ℃ and-0.09 MPa to obtain the amidated carbon nano tube; wherein, the concentration of the strong ammonia water is 8mol/L, the mass volume ratio of the carbon nano tube subjected to acyl chlorination, the ammonium carbonate and the strong ammonia water is 20mg:2mg:50ml, and a polyvinylidene fluoride membrane or a polytetrafluoroethylene membrane with the aperture of 0.30-0.60 mu m is adopted for filtration;
(5) amination of amidated carbon nanotubes: putting the amidated carbon black or the amidated carbon nano tube into ice water, adding excessive sodium hypochlorite for 20min, stirring and reacting for 1h at the rotation speed of 150-200rpm and the temperature of 0-5 ℃, then carrying out water bath reaction for 1h at the temperature of 60 ℃, then cooling and pumping, washing with distilled water for 3-5 times, and drying for 60min at the temperature of 35 ℃ and under the pressure of-0.09 MPa to obtain the aminated carbon nano tube, wherein the mass-volume ratio of the amidated carbon nano tube, the sodium hypochlorite and the water is 20mg to 50ml, and the pumping adopts a polyvinylidene fluoride film or a polytetrafluoroethylene film with the aperture of 0.30-0.60 mu m, and the pressure of the pumping is-0.09 MPa.
The molecular weight of the styrene-maleic anhydride copolymer in the color paste is 2000, the molecular weight distribution index is 1.5, the color paste is any one of trackless, block and alternate structures, and the molar ratio of the maleic anhydride monomer is 20%; the diluent in the color paste is ethyl acetate.
Stirring the styrene-maleic anhydride copolymer and the aminated pigment for 1-5 hours at the rotating speed of 150-200rpm until the mixture is uniformly mixed, adding the styrene-maleic anhydride copolymer and the aminated pigment in such an amount that the molar weight ratio of the maleic anhydride to the molar weight of the amino is 1:1, adding a diluent to adjust the viscosity to 50s (the test condition is 25 ℃, coating a No. 4 cup), and reacting for 2 hours at 90 ℃ to obtain the reactive color paste.
Example 2
The aminated pigment in the reaction color paste is aminated carbon black and is prepared by the following method:
(1) surface modification of carbon black: ultrasonically dispersing carbon black in a toluene solvent, adding an initiator azobisisobutyronitrile, introducing nitrogen for protection for 20min, and then carrying out initiation reaction at 60 ℃ for 90 min; then filtering and separating, and washing for 3-5 times by using a solvent toluene to obtain surface modified carbon black; wherein the mass volume ratio of the carbon black, the solvent and the initiator is 20mg:2g:50ml, the ultrasonic frequency is 30kHz, and the time is 30 min; filtering with polyvinylidene fluoride membrane or polytetrafluoroethylene membrane with pore diameter of 0.30-0.60 μm;
(2) subjecting the surface-modified carbon black to hydrolysis: adding the surface modified carbon black into 0.5mol/L sodium hydroxide, refluxing for 90min, filtering, separating, washing with deionized water for 3-5 times, and drying at 35 deg.C and-0.09 MPa for 60min to obtain carboxyl modified carbon black; wherein, the mass volume ratio of the surface modified carbon black to the sodium hydroxide is 20mg:50ml, and the filtration adopts a polyvinylidene fluoride membrane or a polytetrafluoroethylene membrane with the aperture of 0.30-0.60 mu m;
(3) acylating chlorination of the carboxyl modified carbon black: putting the carbon black modified by carboxyl into dimethyl sulfoxide solvent, condensing and refluxing for 12h at 60 ℃, then carrying out vacuum filtration, repeatedly washing for 3-5 times, and drying for 60min at 35 ℃ and-0.09 MPa to obtain the carbon black subjected to acyl chlorination; wherein, the mass volume ratio of the carboxyl modified carbon black to the solvent is 20mg:50ml, the filtration adopts a polyvinylidene fluoride membrane or a polytetrafluoroethylene membrane with the aperture of 0.30-0.60 mu m, the pressure of the filtration is-0.09 MPa, and tetrahydrofuran is selected as a washing agent for washing;
(4) amidating an acyl chlorinated carbon black or an acyl chlorinated carbon black: adding excessive ammonium carbonate and concentrated ammonia water into the acyl chloride carbon black or the acyl chloride carbon black, stirring and reacting at the rotating speed of 150-200rpm, filtering for 5h, repeatedly washing for 3-5 times by using distilled water, and drying for 60min at the temperature of 35 ℃ and the pressure of-0.09 MPa to obtain amidated carbon black; wherein, the concentration of the strong ammonia water is 8mol/L, the mass volume ratio of the carbon black, ammonium carbonate and the strong ammonia water is 20mg:2mg:50ml, and the polyvinylidene fluoride membrane or the polytetrafluoroethylene membrane with the aperture of 0.30-0.60 mu m is adopted for filtration;
(5) amination of amidated carbon black: putting the amidated carbon black or the amidated carbon black into ice water, adding excessive sodium hypochlorite for 20min, stirring and reacting for 1h at the rotation speed of 150-200rpm and the temperature of 0-5 ℃, then carrying out water bath reaction for 1h at the temperature of 60 ℃, then cooling and pumping, washing with distilled water for 3-5 times, drying for 60min at the temperature of 35 ℃ and under the pressure of-0.09 MPa, and obtaining the aminated carbon black, wherein the mass-volume ratio of the amidated carbon black, the sodium hypochlorite and the water is 20mg:20mg:50ml, the pumping adopts a polyvinylidene fluoride membrane or a polytetrafluoroethylene membrane with the aperture of 0.30-0.60 mu m, and the pumping pressure is-0.09 MPa.
The molecular weight of the styrene-maleic anhydride copolymer in the color paste is 10000, the molecular weight distribution index is 1.0, the color paste is any one of trackless, block and alternate structures, and the molar ratio of the maleic anhydride monomer is 80 percent; the diluent in the color paste is butyl acetate.
Stirring the styrene-maleic anhydride copolymer and the aminated pigment for 1-5 hours at the rotating speed of 150-200rpm until the mixture is uniformly mixed, adding the styrene-maleic anhydride copolymer and the aminated pigment in such an amount that the molar weight ratio of the maleic anhydride to the molar weight of the amino is 1:1, adding a diluent to adjust the viscosity to 20s (the test condition is 25 ℃, coating a No. 4 cup), and reacting for 6 hours at 150 ℃ to obtain the reactive color paste.
Example 3
The aminated pigment in the reaction color paste is aminated carbon black and is prepared by the following method:
(1) surface modification of carbon black: ultrasonically dispersing carbon black in a toluene solvent, adding an initiator azobisisobutyronitrile, introducing nitrogen for protection for 40min, and then carrying out initiation reaction at 80 ℃ for 150 min; then filtering and separating, and washing for 3-5 times by using a solvent toluene to obtain surface modified carbon black; wherein the mass volume ratio of the carbon black, the solvent and the initiator is 35mg:20g:50ml, the ultrasonic frequency is 90kHz, and the time is 60 min; filtering with polyvinylidene fluoride membrane or polytetrafluoroethylene membrane with pore diameter of 0.30-0.60 μm;
(2) subjecting the surface-modified carbon black to hydrolysis: adding the surface modified carbon black into 2mol/L sodium hydroxide, refluxing for 150min, filtering, separating, washing with deionized water for 3-5 times, and drying at 50 ℃ and 0.01MPa for 120min to obtain carboxyl modified carbon black; wherein, the mass volume ratio of the surface modified carbon black to the sodium hydroxide is 60mg:50ml, and the filtration adopts a polyvinylidene fluoride membrane or a polytetrafluoroethylene membrane with the aperture of 0.30-0.60 mu m;
(3) acylating chlorination of the carboxyl modified carbon black: putting the carbon black modified by carboxyl into dimethyl sulfoxide as a solvent, condensing and refluxing for 36h at 80 ℃, then carrying out vacuum filtration, repeatedly washing for 3-5 times, and drying for 120min at 50 ℃ and 0.01MPa to obtain the carbon black subjected to acyl chlorination; wherein, the mass volume ratio of the carboxyl modified carbon black to the solvent is 60mg:50ml, the filtration adopts a polyvinylidene fluoride membrane or a polytetrafluoroethylene membrane with the aperture of 0.30-0.60 mu m, the pressure of the filtration is-0.01 MPa, and tetrahydrofuran is selected as a washing agent for washing;
(4) amidating an acyl chlorinated carbon black or an acyl chlorinated carbon black: adding excessive ammonium carbonate and concentrated ammonia water into the carbon black subjected to acyl chlorination or the carbon black subjected to acyl chlorination, stirring and reacting at the rotation speed of 150-200rpm, filtering for 10h, repeatedly washing for 3-5 times by using distilled water, and drying for 120min at 50 ℃ and 0.01MPa to obtain amidated carbon black; wherein, the concentration of the strong ammonia water is 10mol/L, the mass volume ratio of the carbon black, ammonium carbonate and the strong ammonia water is 35mg:20mg:50ml, and the polyvinylidene fluoride membrane or the polytetrafluoroethylene membrane with the aperture of 0.30-0.60 mu m is adopted for filtration;
(5) amination of amidated carbon black: putting the amidated carbon black or the amidated carbon black into ice water, adding excessive sodium hypochlorite for 40min, stirring and reacting for 5h at the rotation speed of 150-200rpm and the temperature of 0-5 ℃, performing water bath reaction for 5h at the temperature of 80 ℃, then cooling and pumping, washing for 3-5 times by distilled water, and drying for 120min at the temperature of 50 ℃ and the pressure of 0.01MPa to obtain the aminated carbon black, wherein the mass-volume ratio of the amidated carbon black, the sodium hypochlorite and the water is 20mg:50mg:50ml, and the pumping adopts a polyvinylidene fluoride membrane or a polytetrafluoroethylene membrane with the aperture of 0.30-0.60 mu m, and the pressure of the pumping is-0.01 MPa.
The molecular weight of the styrene-maleic anhydride copolymer in the color paste is 1000, the molecular weight distribution index is 2.0, the color paste is any one of trackless, block and alternate structures, and the molar ratio of the maleic anhydride monomer is 50 percent; the diluent in the color paste is isobutyl acetate.
Stirring the styrene-maleic anhydride copolymer and the aminated pigment for 1-5 hours at the rotating speed of 150-200rpm until the mixture is uniformly mixed, adding the styrene-maleic anhydride copolymer and the aminated pigment in such an amount that the molar weight ratio of the maleic anhydride to the molar weight of the amino is 1:1, adding a diluent to adjust the viscosity to 100s (the test condition is 25 ℃, coating a No. 4 cup), and reacting for 6 hours at 100 ℃ to obtain the reactive color paste.
Example 4
The aminated pigment in the reaction color paste is an aminated carbon nanotube and is prepared by the following method:
(1) carrying out surface modification on the carbon nano tube: ultrasonically dispersing carbon nano tubes in a toluene solvent, adding an initiator azobisisobutyronitrile, introducing nitrogen for protection for 40min, and then carrying out initiation reaction at 80 ℃ for 150 min; then filtering and separating, and washing for 3-5 times by using a solvent toluene to obtain a surface modified carbon nano tube; wherein the mass volume ratio of the carbon nano tube to the solvent to the initiator is 35mg to 20g to 50ml, the ultrasonic frequency is 90kHz, and the ultrasonic time is 60 min; filtering with polyvinylidene fluoride membrane or polytetrafluoroethylene membrane with pore diameter of 0.30-0.60 μm;
(2) hydrolyzing the surface modified carbon nano tube: adding the surface modified carbon nano tube into 2mol/L hydrochloric acid, refluxing for 150min, filtering and separating, washing for 3-5 times by using deionized water, and finally drying for 120min at 50 ℃ and 0.01MPa to obtain the carboxyl modified carbon nano tube; wherein, the mass volume ratio of the surface modified carbon nano tube to the hydrochloric acid is 60mg:50ml, and the filtration adopts a polyvinylidene fluoride membrane or a polytetrafluoroethylene membrane with the aperture of 0.30-0.60 mu m;
(3) acylating chlorination of the carboxyl modified carbon nano tube: putting the carboxyl modified carbon nano tube into a solvent dimethyl sulfoxide, condensing and refluxing for 36h at 80 ℃, then performing vacuum filtration, repeatedly washing for 3-5 times, and drying for 120min at 50 ℃ and 0.01MPa to obtain an acyl chlorinated carbon nano tube; wherein, the mass volume ratio of the carboxyl modified carbon nano tube to the solvent is 60mg:50ml, the filtration adopts a polyvinylidene fluoride membrane or a polytetrafluoroethylene membrane with the aperture of 0.30-0.60 mu m, the pressure of the filtration is-0.01 MPa, and tetrahydrofuran is selected as a washing agent for washing;
(4) amidating an acyl-chlorinated carbon black or an acyl-chlorinated carbon nanotube: adding excessive ammonium carbonate and concentrated ammonia water into the carbon black or carbon nano tube subjected to acyl chlorination, stirring and reacting at the rotation speed of 150-200rpm, filtering for 10h, repeatedly washing for 3-5 times by using distilled water, and drying for 120min at 50 ℃ and 0.01MPa to obtain the amidated carbon nano tube; wherein, the concentration of the strong ammonia water is 10mol/L, the mass volume ratio of the carbon nano tube of acyl chloride, ammonium carbonate and the strong ammonia water is 35mg:20mg:50ml, and the polyvinylidene fluoride membrane or the polytetrafluoroethylene membrane with the aperture of 0.30-0.60 mu m is adopted for filtration;
(5) amination of amidated carbon nanotubes: putting the amidated carbon black or the amidated carbon nano tube into ice water, adding excessive sodium hypochlorite for 40min, stirring and reacting for 5h at the rotation speed of 150-200rpm and the temperature of 0-5 ℃, performing water bath reaction for 5h at the temperature of 80 ℃, then cooling and pumping, washing with distilled water for 3-5 times, and drying for 120min at the temperature of 50 ℃ and the pressure of 0.01MPa to obtain the aminated carbon nano tube, wherein the mass-volume ratio of the amidated carbon nano tube, the sodium hypochlorite and the water is 35mg:50mg:50ml, and the pumping adopts a polyvinylidene fluoride film or a polytetrafluoroethylene film with the aperture of 0.30-0.60 mu m, and the pressure of the pumping is-0.01 MPa.
The molecular weight of the styrene-maleic anhydride copolymer in the color paste is 2000, the molecular weight distribution index is 2.0, the color paste is any one of trackless, block and alternate structures, and the molar ratio of the maleic anhydride monomer is 50 percent; the diluent in the color paste is butyl acetate.
Stirring the styrene-maleic anhydride copolymer and the aminated pigment for 1-5 hours at the rotating speed of 150-200rpm until the mixture is uniformly mixed, adding the styrene-maleic anhydride copolymer and the aminated pigment in such an amount that the molar weight ratio of the maleic anhydride to the molar weight of the amino is 1:2, adding a diluent to adjust the viscosity to 100s (the test condition is 25 ℃, coating a No. 4 cup), and reacting for 6 hours at 100 ℃ to obtain the reactive color paste.
Comparative example 1:
a commercially available dispersant Kaysa DS 7560 is matched according to the following formula:
kaysa DS 7560 mass ═ mass of styrene-maleic anhydride alternating copolymer in example 1
Carbon black pigment content of aminated carbon nanotube in example 1
Ethyl acetate was added in the amount of ethyl acetate added for viscosity adjustment in example 1
Uniformly mixing at a high speed, and grinding and dispersing for 3 hours at the rotating speed of 800-.
Comparative example 2:
a commercially available dispersant Kaysa DS 7560 is matched according to the following formula:
kaysa DS 7560 Mass-Mass of styrene-maleic anhydride random copolymer in example 2
Carbon black pigment content of aminated carbon black pigment in example 2
Butyl acetate-amount of butyl acetate added for adjusting viscosity in example 2
Uniformly mixing at a high speed, and grinding and dispersing for 3 hours at the rotating speed of 800-.
Comparative example 3:
a commercially available dispersant Kaysa DS 7560 is matched according to the following formula:
kaysa DS 7560 mass ═ mass of styrene-maleic anhydride block copolymer in example 3
Carbon black pigment content of aminated carbon black pigment in example 3
Isobutyl acetate-amount of isobutyl acetate added for viscosity adjustment in example 3
Uniformly mixing at a high speed, and grinding and dispersing for 3 hours at the rotating speed of 800-.
Comparative example 4:
a commercially available dispersant Kaysa DS 7560 is matched according to the following formula:
kaysa DS 7560 Mass-Mass of styrene-maleic anhydride alternating copolymer in example 4
Carbon black pigment content of aminated carbon nanotubes in example 4
Diluent-amount of butyl acetate added for adjusting viscosity in example 4
Uniformly mixing at a high speed, and grinding and dispersing for 3 hours at the rotating speed of 800-.
The properties of the mill pastes prepared in the examples and comparative examples are shown in Table 1:
TABLE 1
Continuously dispersing the following pigments in the 8 groups of color pastes according to the following proportion:
phthalocyanine blue: 1 percent of
Barium sulfate: 5 percent of
Calcium carbonate: 5 percent of
Titanium dioxide: 3 percent of
Color paste of example/comparative example color paste: 80 percent of
Butyl acetate: 6 percent of
After grinding, stirring and dispersing for 3h at the rotating speed of 800-1000r/min, the performance is tested again, and the results are shown in table 2:
TABLE 2
Claims (10)
1. The reactive color paste is characterized in that the raw materials of the color paste comprise styrene-maleic anhydride copolymer, aminated pigment and diluent, wherein the addition amount of the styrene-maleic anhydride copolymer and the aminated pigment is such that the ratio of the molar weight of maleic anhydride to the molar weight of amino is 1 (1-2), the addition amount of the diluent is such that the viscosity of the color paste is adjusted to be between 20 and 100s, and the measuring condition is to coat a No. 4 cup.
2. The reactive color paste according to claim 1, wherein the styrene-maleic anhydride copolymer has a molecular weight of 1000-10000, a molecular weight distribution index of 1.0-2.0, and is any one of trackless, block and alternating structure, and the molar ratio of maleic anhydride monomer is 30-80%; the diluent comprises one or two of butyl acetate or ethyl acetate.
3. The reactive color paste according to claim 1, wherein the aminated pigment comprises aminated carbon black or aminated carbon nanotubes, and is prepared by the following method:
(1) surface modification of carbon black or carbon nanotubes: ultrasonically dispersing carbon black or carbon nano tubes in a solvent, adding an initiator, introducing inert gas for protection, and then carrying out initiation reaction; then filtering and separating, and washing with a solvent to obtain surface modified carbon black or surface modified carbon nano tubes;
(2) hydrolyzing the surface-modified carbon black or the surface-modified carbon nanotubes: adding the surface modified carbon black or the surface modified carbon nano tube into an aqueous solution, refluxing, filtering and separating, washing with deionized water, and finally drying to obtain carboxyl modified carbon black or carboxyl modified carbon nano tube;
(3) acylating chlorination of the carboxyl modified carbon black or the carboxyl modified carbon nanotube: putting the carboxyl modified carbon black or the carboxyl modified carbon nano tube into a solvent, heating, condensing, refluxing, decompressing, filtering, repeatedly washing and drying to obtain the acyl chlorinated carbon black or the acyl chlorinated carbon nano tube;
(4) amidating an acyl-chlorinated carbon black or an acyl-chlorinated carbon nanotube: adding excessive ammonium carbonate and concentrated ammonia water into the acyl chlorinated carbon black or the acyl chlorinated carbon nano tube, stirring for reaction, filtering, repeatedly washing with distilled water, and drying to obtain amidated carbon black or amidated carbon nano tube;
(5) amination of amidated carbon black or amidated carbon nanotubes: putting the amidated carbon black or the amidated carbon nano tube into ice water, adding excessive sodium hypochlorite for 20-40min, carrying out stirring reaction, heating the mixture to carry out water bath reaction, then cooling and filtering, washing the mixture by distilled water, and drying the washed product to obtain the aminated carbon black or the aminated carbon nano tube.
4. The reactive color paste according to claim 3, wherein the carbon nanotubes in step (1) comprise single-walled carbon nanotubes or multi-walled carbon nanotubes; the solvent comprises one or more of toluene, tetrahydrofuran, N-dimethylformamide or N-methylpyrrolidone; the initiator comprises one or more of azobisisobutyronitrile, azobisisoheptonitrile, azobisisooctonitrile, 2 '-azobis (2, 4-dimethylvaleronitrile) or 1, 1' -azobis (cyclohexanecarbonitrile); the mass volume ratio of the carbon black or the carbon nano tube, the solvent and the initiator is (20-35) mg, (2-20) g:50ml, the frequency of the ultrasonic is 30-90kHz, and the time is 30-60 min; the inert gas comprises nitrogen or argon, and the protection time is 20-40 min; the reaction temperature is 60-80 ℃ and the reaction time is 90-150 min; the filtration adopts a polyvinylidene fluoride membrane or a polytetrafluoroethylene membrane with the aperture of 0.30-0.60 mu m; the number of washing times is 3-5.
5. The reactive color paste according to claim 3, wherein the aqueous solution in step (2) comprises an acid solution or an alkali solution, the acid solution is one or more of hydrochloric acid, sulfuric acid and phosphoric acid, the concentration of the acid solution is 0.5-2mol/L, the alkali solution is sodium hydroxide or potassium hydroxide, and the concentration of the alkali solution is 0.5-2 mol/L; the mass-volume ratio of the surface modified carbon black or the surface modified carbon nano tube to the aqueous solution is (20-60) mg:50 ml; the refluxing time is 90-150min, and the filtration adopts a polyvinylidene fluoride membrane or a polytetrafluoroethylene membrane with the pore diameter of 0.30-0.60 mu m; the washing times are 3-5 times, the drying temperature is 35-50 ℃, the pressure is-0.09-0.01 MPa, and the time is 60-120 min.
6. The reactive color paste according to claim 3, wherein the solvent in step (3) comprises dimethyl sulfoxide or N, N-dimethylformamide; the mass volume ratio of the carboxyl modified carbon black or the carboxyl modified carbon nano tube to the solvent is (20-60) mg:50 ml; the temperature of the heating, condensing and refluxing is 60-80 ℃, the time is 12-36h, the suction filtration adopts a polyvinylidene fluoride membrane or a polytetrafluoroethylene membrane with the aperture of 0.30-0.60 mu m, the pressure of the suction filtration is-0.09 MPa to-0.01 MPa, and tetrahydrofuran is selected as a washing agent for washing; the drying temperature is 35-50 ℃, the pressure is-0.09-0.01 MPa, and the time is 60-120 min.
7. The reactive color paste according to claim 3, wherein the concentration of the concentrated ammonia water in step (4) is 8-10mol/L, the mass-to-volume ratio of the acyl chlorinated carbon black or the acyl chlorinated carbon nanotube, ammonium carbonate and concentrated ammonia water is (20-35) mg (2-20) mg:50ml, the stirring speed of the stirring reaction is 150-200rpm, the time is 5-10h, and the filtration is performed by using a polyvinylidene fluoride membrane or a polytetrafluoroethylene membrane with an aperture of 0.30-0.60 μm; the washing times are 3-5 times, the drying temperature is 35-50 ℃, the pressure is-0.09-0.01 MPa, and the time is 60-120 min.
8. The reactive color paste according to claim 3, wherein the mass-to-volume ratio of the amidated carbon black or amidated carbon nanotube, sodium hypochlorite and water in step (5) is (20-35) mg (20-50) mg:50ml, the stirring speed of the stirring reaction is 150-200rpm, the temperature is 0-5 ℃, the time is 1-5h, the temperature of the water bath reaction is 60-80 ℃, the time is 1-5h, the filtration adopts a polyvinylidene fluoride membrane or a polytetrafluoroethylene membrane with an aperture of 0.30-0.60 μm, the pressure of the filtration is-0.09 MPa to-0.01 MPa, and the number of washing times is 3-5; the drying temperature is 35-50 ℃, the pressure is-0.09-0.01 MPa, and the time is 60-120 min.
9. The method for preparing the reactive color paste according to claim 1, wherein the reactive color paste is prepared by uniformly mixing the styrene-maleic anhydride copolymer and the aminated pigment in proportion, adding the diluent to adjust the viscosity, and heating for reaction.
10. The method for preparing the reactive color paste according to claim 9, wherein the stirring and mixing speed is 150-200rpm for 1-5 hours, the heating reaction temperature is 90-150 ℃ and the heating reaction time is 2-6 hours.
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Application publication date: 20200508 |