CN115304961A - Color paste containing functional crosslinking assistant capable of promoting stability of color paste system, preparation method thereof and application thereof in neutral ink - Google Patents

Color paste containing functional crosslinking assistant capable of promoting stability of color paste system, preparation method thereof and application thereof in neutral ink Download PDF

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Publication number
CN115304961A
CN115304961A CN202211161663.2A CN202211161663A CN115304961A CN 115304961 A CN115304961 A CN 115304961A CN 202211161663 A CN202211161663 A CN 202211161663A CN 115304961 A CN115304961 A CN 115304961A
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color paste
stability
promoting
cylinder
grinding cylinder
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CN115304961B (en
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马振海
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Guangdong Baoke Stationery Co ltd
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Guangdong Baoke Stationery Co ltd
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D17/00Pigment pastes, e.g. for mixing in paints
    • C09D17/001Pigment pastes, e.g. for mixing in paints in aqueous medium
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B02CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02CCRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C17/00Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls
    • B02C17/16Mills in which a fixed container houses stirring means tumbling the charge
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B02CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02CCRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C17/00Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls
    • B02C17/16Mills in which a fixed container houses stirring means tumbling the charge
    • B02C17/161Arrangements for separating milling media and ground material
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B02CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02CCRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C17/00Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls
    • B02C17/16Mills in which a fixed container houses stirring means tumbling the charge
    • B02C17/163Stirring means
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B02CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02CCRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C17/00Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls
    • B02C17/18Details
    • B02C17/183Feeding or discharging devices
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B02CRUSHING, PULVERISING, OR DISINTEGRATING; PREPARATORY TREATMENT OF GRAIN FOR MILLING
    • B02CCRUSHING, PULVERISING, OR DISINTEGRATING IN GENERAL; MILLING GRAIN
    • B02C17/00Disintegrating by tumbling mills, i.e. mills having a container charged with the material to be disintegrated with or without special disintegrating members such as pebbles or balls
    • B02C17/18Details
    • B02C17/24Driving mechanisms
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D11/00Inks
    • C09D11/16Writing inks
    • C09D11/18Writing inks specially adapted for ball-point writing instruments

Abstract

The invention relates to the technical field of color paste, and discloses color paste containing a functional crosslinking assistant capable of promoting the stability of a color paste system, a preparation method thereof and application thereof in neutral ink. The color paste containing the functional crosslinking assistant capable of promoting the stability of the color paste system and the preparation method thereof comprise the following steps: the method comprises the steps of stirring and mixing propylene glycol, polyethylene glycol 200, antirust benzotriazole, preservative, polystyrene maleic anhydride copolymerized ammonium salt, defoaming agent, acrylic resin, functional crosslinking auxiliary agent capable of promoting stability of a color paste system, pigment and deionized water, adding triethanolamine to adjust pH, stirring by using a high-speed shearing emulsifying stirrer to obtain a color paste raw material, and transferring the color paste raw material into a sand mill to grind to obtain the color paste. The invention has the advantages of stable dispersion, prevention of flocculation and precipitation of color paste, and improvement of thermal stability and mechanical stability.

Description

Color paste containing functional crosslinking assistant capable of promoting stability of color paste system, preparation method thereof and application thereof in neutral ink
Technical Field
The invention relates to the technical field of color paste, in particular to color paste containing a functional crosslinking assistant capable of promoting the stability of a color paste system, a preparation method thereof and application thereof in neutral ink.
Background
The gel pen is a novel variety in ball-point pen products, combines the advantages of the traditional oil ball-point pen and water ball-point pen, and has the advantages of smooth writing, light and comfortable hand feeling, clear handwriting, good color and luster feeling, water resistance, sun resistance, long storage life and the like. The colored gel liquid filled in the gel ink pen holder is the gel ink.
The neutral ink is prepared from pigment color paste as a main medium component, and water, a thickening agent, a surfactant, a lubricant, a humectant, a pH regulator, a sterilizing preservative, a defoaming agent, an auxiliary agent and the like. The quality of the prepared neutral ink is greatly influenced by selecting proper and stable pigment color paste. The general pigment for neutral ink is high pigment carbon black, phthalocyanine blue, hurst red, permanent red and the like, for example, chinese patent CN101768389B discloses a preparation method of black color-regulating ink paste for neutral ink, which comprises the following steps: reserving the balance of 20wt% of deionized water, and adding the balance of 80wt% of deionized water, 2.0-20.0 wt% of dispersing and wetting agent and 5.0-10.0 wt% of alkyd resin or aldehyde ketone resin into a mixer to disperse for 15 minutes at the speed of 400-800r/min to obtain a uniform mixed solution; adding 25.0-40.0 wt% of carbon black pigment into the uniformly mixed solution, and uniformly mixing to obtain premixed carbon black pigment slurry; grinding the pre-mixed carbon black pigment paste, stopping grinding when the particle size of the pre-mixed carbon black pigment paste reaches 50% and the particle size is less than or equal to 1.0 mu m, and dispersing for 15 minutes at 1500r/min to obtain carbon black color paste; diluting the pH regulator accounting for 0.1 to 2.0 percent by weight with the deionized water accounting for 20 percent by weight of the reserved balance, and adding the diluted pH regulator into the obtained carbon black color paste under the condition of stirring speed of 1500r/min to obtain the final product.
However, in the chinese patent CN101768389B and the prior art, most of the color pastes for neutral ink preparation are prepared by one or a combination of a sand mill, a ball mill and a colloid mill by using pigments, dispersants and auxiliaries, so as to realize sub-nanometer or nanometer dispersion of the pigments, and the color pastes prepared by the process have the following problems: the particle size is not uniform, when the pigment particles are ground to be finer, the surface energy is larger, the mutual cohesion of the particles is stronger, and the pigment particles are easy to flocculate and settle, so that the prepared finished product of the neutral ink has poor stability, and the quality problem of pen point blockage is easy to cause.
Disclosure of Invention
In order to solve the technical problem, the invention provides a preparation method of color paste containing functional cross-linking auxiliary agent capable of promoting the stability of a color paste system, which comprises the following steps:
mixing attapulgite and toluene, performing ultrasonic dispersion for 10-30min, adding gamma-aminopropyltriethoxysilane, reacting at 70-100 ℃ for 6-10h, filtering to obtain filter residue, washing the filter residue with ethanol, and drying at 60-80 ℃ for 10-12h to obtain modified attapulgite; wherein the mass ratio of the attapulgite to the gamma-aminopropyltriethoxysilane to the toluene is 1:1: (10-30); the ultrasonic power is 600-800W;
dispersing the crosslinking aid in deionized water, adding the modified attapulgite under stirring, continuing stirring for 30-60min, filtering to obtain filter residue, washing the filter residue with deionized water, and drying at 60-100 ℃ for 3-6h to obtain the functional crosslinking aid capable of promoting the stability of the color paste system; wherein the stirring speed is 500-2000r/min; the mass ratio of the crosslinking auxiliary agent to the deionized water to the modified attapulgite is (5-10): (100-150): (2-4.5); the crosslinking auxiliary agent comprises any one of citric acid and malic acid;
step (3) mixing propylene glycol, polyethylene glycol 200, antirust benzotriazole, preservative, polystyrene maleic anhydride copolymer ammonium salt (CAS number: 26022-09-3), defoaming agent, acrylic resin, functional cross-linking auxiliary agent capable of promoting the stability of a color paste system, pigment and deionized water, adding triethanolamine to adjust the pH value, stirring by using a high-speed shearing emulsifying mixer to obtain a color paste raw material, transferring the color paste raw material into a sand mill to grind, and obtaining the color paste containing the functional cross-linking auxiliary agent capable of promoting the stability of the color paste system; wherein the mass ratio of propylene glycol, polyethylene glycol 200, antirust benzotriazole, preservative, polystyrene maleic anhydride copolymerized ammonium salt, defoaming agent, acrylic resin, functional cross-linking auxiliary agent capable of promoting stability of color paste system, pigment, deionized water and triethanolamine is 25:25:15:15:2:0.5:62.5: (12-20): 75: (215-223): 15.
preferably, the color paste containing the functional cross-linking auxiliary agent capable of promoting the stability of the color paste system is prepared by adopting the method.
Preferably, the neutral ink prepared by the color paste containing the functional crosslinking assistant capable of promoting the stability of the color paste system comprises the following steps:
stirring and mixing propylene glycol, polyethylene glycol 200, a lubricant, a thickening agent and deionized water, then adding triethanolamine to adjust the pH value, adding color paste containing a functional cross-linking auxiliary agent capable of promoting the stability of a color paste system under the stirring condition, continuously stirring, and filtering to obtain neutral ink; wherein, the mass ratio of the propylene glycol, the polyethylene glycol 200, the lubricant, the thickening agent, the deionized water, the triethanolamine and the color paste containing the functional cross-linking auxiliary agent capable of promoting the stability of the color paste system is 25:25:5: (11-13): 173:10:250.
the invention also provides a sand mill which can be used for grinding the color paste raw material in the method. The sand mill comprises a sand mill body, an outer material conveying barrel is fixedly installed on the sand mill body, an inner grinding barrel is rotatably assembled inside the outer material conveying barrel, a dispersion disc is rotatably assembled inside the inner grinding barrel, zirconia beads are filled inside the inner grinding barrel, the inner grinding barrel and the dispersion disc are driven by a driving assembly to synchronously and reversely rotate so as to drive the zirconia beads filled between the dispersion discs to move; the discharge holes capable of discharging materials in one direction are uniformly formed in the surface of the side wall of the inner grinding cylinder, so that color paste raw materials are ground in the inner grinding cylinder through zirconia beads, and can be thrown into the conveying cavity formed between the outer wall of the inner grinding cylinder and the inner wall of the outer conveying cylinder from the discharge holes under the action of centrifugal force.
Interior grinding vessel one end fixedly connected with extends a section of thick bamboo and separator in proper order, interior grinding vessel with extend a section of thick bamboo outer wall surface and all be provided with the screw thread arch, the protruding lateral wall of screw thread with form helical channel between interior grinding vessel and the interior extension section of thick bamboo outer wall, interior grinding vessel with interior grinding vessel rotates and can make the mill base that gets into defeated material intracavity evenly carry extremely along helical channel discharge behind the separator, the separator rotation can be sieved out relatively great granule in the mill base.
Preferably, the inner grinding cylinder comprises a grinding cylinder body, a first sealing cover and a first shaft sleeve, the first sealing covers are respectively and fixedly arranged at two ends of the grinding cylinder body, the first shaft sleeves are respectively arranged on the first sealing covers, one end of the inner extension cylinder is fixedly connected with one end of the grinding cylinder body, the other end of the inner extension cylinder is fixedly connected with the separator, and the separator is communicated with the material conveying cavity; the separator end part is rotatably assembled with a second sealing cover, the separator end part and the surface of the second sealing cover are kept sealed, the second sealing cover is fixedly connected with a second shaft sleeve, two ends of an outer material conveying cylinder are respectively provided with an outer shaft sleeve, the outer wall of one first shaft sleeve far away from the separator is in rotating fit with the inner wall of the outer shaft sleeve corresponding to the position through a first bearing, and the outer wall of the second shaft sleeve is fixedly connected with the inner wall of the outer shaft sleeve corresponding to the position through a sealing sleeve.
Preferably, an inner feed port is formed in one end, away from the separator, of the grinding cylinder body, an outer feed pipe is arranged on the outer feed cylinder, a feed valve is arranged on the inner feed port, and when the grinding cylinder body rotates to the position where the inner feed port corresponds to the outer feed pipe, an outer pipeline can penetrate through the outer feed pipe to be inserted into the inner feed port to feed materials after the feed valve is opened;
and a discharge pipe is arranged on the second sealing cover, a discharge valve is arranged on the discharge pipe, and the discharge pipe extends to the outside of the outer material conveying barrel and is communicated with a liquid outlet in the separator.
Preferably, the inner grinding cylinder further comprises a one-way valve, the one-way valve is respectively arranged on a discharge hole formed in the surface of the side wall of the inner grinding cylinder, a filter screen is arranged on one side of the discharge hole and located on one side of a liquid inlet of the one-way valve, and the one-way valve is respectively located between two adjacent circles of thread protrusions on the surface of the outer wall of the grinding cylinder body.
Preferably, the driving assembly includes a driving source, a first rotating shaft and a second rotating shaft, a belt pulley is respectively disposed at one end of the driving shaft of the driving source and one end of the first rotating shaft, a transmission belt is disposed between the two belt pulleys, the first rotating shaft extends into the inner extending cylinder and the inner grinding cylinder, and the dispersion discs are respectively fixedly sleeved on the surface of the first rotating shaft; second pivot one end is rotated the assembly and is in on the outer defeated feed cylinder tip inner wall, first pivot with fixed cover is equipped with intermeshing's first gear and second gear respectively in the second pivot, interior extension section of thick bamboo inner wall surface encircles and is provided with the transmission rack, the second gear with the meshing of transmission rack.
Preferably, both ends of the first rotating shaft are rotatably assembled inside the first shaft sleeve and the second shaft sleeve which correspond in position through second bearings respectively.
Preferably, two sides of the first bearing and two sides of the second bearing are respectively provided with a sealing ring.
Preferably, the inner wall surface of the grinding cylinder body is uniformly provided with a convex ring, two openings which are opposite in position are formed in the convex ring, and the openings and the one-way valves are distributed on the same axis respectively.
Preferably, the sander main body comprises a base and a machine shell, a control unit and a bearing frame which are fixedly installed on the base, the driving source is provided with the belt pulley, the transmission belt and one end of the first rotating shaft are arranged inside the machine shell, the outer material conveying barrel is fixedly installed on the bearing frame, and the control unit is used for controlling the operation of the device.
Compared with the prior art, the invention has the following beneficial effects: the attapulgite is used as an anti-settling agent, amino is introduced on the surface of the attapulgite through an aminosilane coupling agent, and the amino is combined with carboxyl in a crosslinking assistant through electrostatic adsorption, so that active groups of amino and carboxyl are introduced on the surface of the attapulgite and can be combined with active groups on acrylic resin to form a crosslinking system with high crosslinking degree; furthermore, the cross-linked acrylic resin can be adsorbed to the surface of the pigment through chemical acting forces such as pi-pi bonds, hydrogen bonds, van der waals force and the like, has the functions of charge repulsion and steric hindrance, avoids the large agglomeration of the surface of pigment particles with smaller particle sizes, enables the pigment to be dispersed stably, prevents the flocculation and precipitation of color paste, and improves the thermal stability and the mechanical stability of the pigment.
According to the sand mill, the discharge holes for discharging materials in one direction are uniformly formed in the side wall of the grinding cylinder, and the ground color paste raw materials obtained by grinding the color paste raw materials by the zirconia beads are uniformly thrown out of the discharge holes under the driving of centrifugal force generated in the high-speed rotation process of the dispersion disc, so that the ground color paste raw materials are separated from the zirconia beads, and the situation that the discharge holes are blocked by a large amount of aggregated zirconia beads to be difficult to discharge the ground color paste raw materials completely can be avoided.
Drawings
FIG. 1 is a flow chart of a process for preparing a functional crosslinking assistant capable of promoting the stability of a color paste system according to the invention;
FIG. 2 is a flow chart of a process for preparing the gel ink of the present invention;
FIG. 3 is a graph of D color pastes prepared in examples 1-5 and comparative examples 1-3 of the present invention 90 Particle size test contrast chart;
FIG. 4 is a comparison graph of specific absorbance tests of color pastes prepared in examples 1-5 and comparative examples 1-3 of the present invention;
FIG. 5 is a schematic view of a sand mill according to the present invention in a partial cross-sectional configuration;
FIG. 6 is a schematic perspective view of a sander according to the present invention;
FIG. 7 is a schematic sectional view of an external feed cylinder of the sander according to the present invention;
FIG. 8 is an exploded view of a portion of the components of the sander of the present invention.
In the figure: 1. a sand mill body; 11. a machine base; 12. a housing; 13. a control unit; 14. a carrier; 2. an external feed cylinder; 21. an outer sleeve; 22. an outer feed pipe; 3. an inner grinding cylinder; 31. grinding the cylinder body; 311. a convex ring; 32. a first sealing cover; 33. a first bushing; 34. a one-way valve; 35. an inner feed inlet; 4. a dispersion tray; 5. an inner extension cylinder; 51. a drive rack; 6. a separator; 61. a second sealing cover; 62. a second shaft sleeve; 63. a discharge pipe; 7. a drive assembly; 71. a drive source; 72. a first rotating shaft; 721. a first gear; 73. a second rotating shaft; 731. a second gear.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, rather than all embodiments, and all other embodiments obtained by a person of ordinary skill in the art without any creative work based on the embodiments of the present invention belong to the protection scope of the present invention.
Example 1
A method for preparing color paste containing functional cross-linking auxiliary agent capable of promoting the stability of a color paste system comprises the following steps:
1. mixing attapulgite and toluene, carrying out ultrasonic dispersion for 30min under the condition that the ultrasonic power is 600W, adding gamma-aminopropyltriethoxysilane, and reacting for 10h at 70 ℃; after the reaction is finished, filtering to obtain filter residues, washing the filter residues with ethanol, and drying at 60 ℃ for 12 hours to obtain modified attapulgite; wherein the mass ratio of the attapulgite, the gamma-aminopropyltriethoxysilane and the toluene is 1:1:10;
2. dispersing citric acid in deionized water, adding modified attapulgite at a stirring speed of 500r/min, continuously stirring for 60min, filtering to obtain filter residue, washing the filter residue with deionized water, and drying at 60 ℃ for 6h to obtain a functional crosslinking auxiliary agent capable of promoting the stability of a color paste system; the mass ratio of the citric acid to the deionized water to the modified attapulgite is 5:100:2;
3. stirring propylene glycol, polyethylene glycol 200, antirust benzotriazole, preservative GXL, polystyrene maleic anhydride copolymerized ammonium salt, defoaming agent SN-1340, acrylic resin, functional cross-linking auxiliary agent capable of promoting stability of a color paste system, pigment and deionized water at a stirring speed of 600r/min for 40min, adding triethanolamine to adjust pH, stirring at a stirring speed of 3000r/min at room temperature for 30min by using a high-speed shearing emulsion stirrer to obtain a color paste raw material, and transferring the color paste raw material to a sand mill for grinding to obtain color paste containing the functional cross-linking auxiliary agent capable of promoting stability of the color paste system; the mass ratio of propylene glycol, polyethylene glycol 200, antirust agent benzotriazole, preservative GXL, polystyrene maleic anhydride copolymer ammonium salt, defoaming agent SN-1340, acrylic resin, functional cross-linking auxiliary agent capable of promoting the stability of a color paste system, pigment, deionized water and triethanolamine is 25:25:15:15:2:0.5:62.5:12:75:223:15.
example 2
A method for preparing color paste containing functional cross-linking auxiliary agent capable of promoting the stability of a color paste system comprises the following steps:
1. mixing attapulgite with toluene, performing ultrasonic dispersion for 10min under the condition of ultrasonic power of 800W, adding gamma-aminopropyltriethoxysilane, and reacting for 6h at 100 ℃; after the reaction is finished, filtering to obtain filter residues, washing the filter residues with ethanol, and drying at 80 ℃ for 10 hours to obtain modified attapulgite; wherein the mass ratio of the attapulgite, the gamma-aminopropyltriethoxysilane and the toluene is 1:1:30, of a nitrogen-containing gas;
2. dispersing citric acid in deionized water, adding modified attapulgite at a stirring speed of 2000r/min, continuously stirring for 30min, filtering to obtain filter residue, washing the filter residue with deionized water, and drying at 100 ℃ for 3h to obtain a functional crosslinking auxiliary agent capable of promoting the stability of a color paste system; the mass ratio of the citric acid to the deionized water to the modified attapulgite is 10:150:4.5;
3. stirring propylene glycol, polyethylene glycol 200, antirust benzotriazole, preservative GXL, polystyrene maleic anhydride copolymerized ammonium salt, defoaming agent SN-1340, acrylic resin, functional cross-linking auxiliary agent capable of promoting stability of a color paste system, pigment and deionized water at a stirring speed of 600r/min for 40min, adding triethanolamine to adjust pH, stirring at a stirring speed of 3000r/min at room temperature for 30min by using a high-speed shearing emulsion stirrer to obtain a color paste raw material, and transferring the color paste raw material to a sand mill for grinding to obtain color paste containing the functional cross-linking auxiliary agent capable of promoting stability of the color paste system; the mass ratio of propylene glycol, polyethylene glycol 200, antirust agent benzotriazole, preservative GXL, polystyrene maleic anhydride copolymer ammonium salt, defoaming agent SN-1340, acrylic resin, functional cross-linking auxiliary agent capable of promoting the stability of a color paste system, pigment, deionized water and triethanolamine is 25:25:15:15:2:0.5:62.5:20:75:215:15.
example 3
A method for preparing color paste containing functional cross-linking auxiliary agent capable of promoting stability of color paste system comprises the following steps:
1. mixing attapulgite and toluene, carrying out ultrasonic dispersion for 25min under the condition that the ultrasonic power is 650W, adding gamma-aminopropyltriethoxysilane, and reacting for 9h at 80 ℃; after the reaction is finished, filtering to obtain filter residues, washing the filter residues with ethanol, and drying at 70 ℃ for 11 hours to obtain modified attapulgite; wherein the mass ratio of the attapulgite to the gamma-aminopropyltriethoxysilane to the toluene is 1:1:15;
2. dispersing citric acid in deionized water, adding modified attapulgite at a stirring speed of 1000r/min, continuously stirring for 50min, filtering to obtain filter residue, washing the filter residue with deionized water, and drying at 75 ℃ for 4h to obtain a functional crosslinking auxiliary agent capable of promoting the stability of a color paste system; the mass ratio of the citric acid to the deionized water to the modified attapulgite is 7:120:3;
3. stirring propylene glycol, polyethylene glycol 200, antirust benzotriazole, preservative GXL, polystyrene maleic anhydride copolymerized ammonium salt, defoaming agent SN-1340, acrylic resin, functional cross-linking auxiliary agent capable of promoting stability of a color paste system, pigment and deionized water at a stirring speed of 600r/min for 40min, adding triethanolamine to adjust pH, stirring at a stirring speed of 3000r/min at room temperature for 30min by using a high-speed shearing emulsion stirrer to obtain a color paste raw material, and transferring the color paste raw material to a sand mill for grinding to obtain color paste containing the functional cross-linking auxiliary agent capable of promoting stability of the color paste system; the mass ratio of propylene glycol, polyethylene glycol 200, antirust agent benzotriazole, preservative GXL, polystyrene maleic anhydride copolymer ammonium salt, defoaming agent SN-1340, acrylic resin, functional cross-linking auxiliary agent capable of promoting the stability of a color paste system, pigment, deionized water and triethanolamine is 25:25:15:15:2:0.5:62.5:15:75:220:15.
example 4
A method for preparing color paste containing functional cross-linking auxiliary agent capable of promoting stability of color paste system comprises the following steps:
1. mixing attapulgite with toluene, performing ultrasonic dispersion for 20min under the condition of ultrasonic power of 700W, adding gamma-aminopropyltriethoxysilane, and reacting for 8h at 90 ℃; after the reaction is finished, filtering to obtain filter residues, washing the filter residues with ethanol, and drying at 75 ℃ for 10.5 hours to obtain modified attapulgite; wherein the mass ratio of the attapulgite, the gamma-aminopropyltriethoxysilane and the toluene is 1:1:22;
2. dispersing citric acid in deionized water, adding modified attapulgite at a stirring speed of 1500r/min, continuously stirring for 45min, filtering to obtain filter residue, washing the filter residue with deionized water, and drying at 85 ℃ for 3h to obtain a functional crosslinking auxiliary agent capable of promoting the stability of a color paste system; the mass ratio of the citric acid to the deionized water to the modified attapulgite is 8.5:135:3.8 of the total weight of the mixture;
3. stirring propylene glycol, polyethylene glycol 200, antirust benzotriazole, preservative GXL, polystyrene maleic anhydride copolymerized ammonium salt, defoaming agent SN-1340, acrylic resin, functional cross-linking auxiliary agent capable of promoting stability of a color paste system, pigment and deionized water at a stirring speed of 600r/min for 40min, adding triethanolamine to adjust pH, stirring at a stirring speed of 3000r/min at room temperature for 30min by using a high-speed shearing emulsion stirrer to obtain a color paste raw material, and transferring the color paste raw material to a sand mill for grinding to obtain color paste containing the functional cross-linking auxiliary agent capable of promoting stability of the color paste system; the mass ratio of propylene glycol, polyethylene glycol 200, antirust agent benzotriazole, preservative GXL, polystyrene maleic anhydride copolymer ammonium salt, defoaming agent SN-1340, acrylic resin, functional cross-linking auxiliary agent capable of promoting the stability of a color paste system, pigment, deionized water and triethanolamine is 25:25:15:15:2:0.5:62.5:18:75:217:15.
example 5
A method for preparing color paste containing functional cross-linking auxiliary agent capable of promoting the stability of a color paste system comprises the following steps:
1. mixing attapulgite and toluene, carrying out ultrasonic dispersion for 25min under the condition that the ultrasonic power is 650W, adding gamma-aminopropyltriethoxysilane, and reacting for 9h at 80 ℃; after the reaction is finished, filtering to obtain filter residues, washing the filter residues with ethanol, and drying at 70 ℃ for 11 hours to obtain modified attapulgite; wherein the mass ratio of the attapulgite to the gamma-aminopropyltriethoxysilane to the toluene is 1:1:15;
2. dispersing malic acid in deionized water, adding modified attapulgite at a stirring speed of 1000r/min, continuously stirring for 50min, filtering to obtain filter residue, washing the filter residue with deionized water, and drying at 75 ℃ for 4h to obtain a functional crosslinking auxiliary agent capable of promoting the stability of a color paste system; the mass ratio of malic acid to deionized water to modified attapulgite is 7:120:3;
3. stirring propylene glycol, polyethylene glycol 200, antirust benzotriazole, preservative GXL, polystyrene maleic anhydride copolymer ammonium salt, defoaming agent SN-1340, acrylic resin, functional cross-linking assistant capable of promoting stability of a color paste system, pigment and deionized water at a stirring speed of 600r/min for 40min, adding triethanolamine to adjust pH, stirring for 30min at a stirring speed of 3000r/min by using a high-speed shearing emulsifying mixer at room temperature to obtain a color paste raw material, and transferring the color paste raw material into a sand mill to grind to obtain a color paste containing the functional cross-linking assistant capable of promoting stability of the color paste system; the mass ratio of propylene glycol, polyethylene glycol 200, antirust agent benzotriazole, preservative GXL, polystyrene maleic anhydride copolymer ammonium salt, defoaming agent SN-1340, acrylic resin, functional cross-linking auxiliary agent capable of promoting the stability of a color paste system, pigment, deionized water and triethanolamine is 25:25:15:15:2:0.5:62.5:15:75:220:15.
in examples 1 to 5, the conditions for grinding the color paste raw material were as follows: the grain diameter of zirconia beads in the sand mill is 0.5mm, and the ball-material ratio is 4:1, the rotating speed of the sand mill is 1500r/min, and the grinding time is 2h.
Example 6
The embodiment discloses a preparation method of neutral ink, which comprises the following steps:
adding propylene glycol, polyethylene glycol 200, a lubricant MOA-3P, a thickening agent ALCOGUARD5800, a thickening agent T-938 and deionized water into the mixture, adding triethanolamine into the mixture to adjust the pH value of the mixture, adding color paste containing functional cross-linking auxiliaries capable of promoting the stability of a color paste system into the mixture at a stirring speed of 600r/min, continuously stirring the mixture for 2 hours, and filtering the mixture to obtain neutral ink; wherein the mass ratio of propylene glycol, polyethylene glycol 200, a lubricant MOA-3P, a thickening agent ALCOGUARD5800, a thickening agent T-938, deionized water, triethanolamine and color paste containing a functional cross-linking auxiliary agent capable of promoting the stability of a color paste system is 25:25:5:2.5:9.5:173:10:250.
the color paste containing the functional cross-linking assistant capable of promoting the stability of the color paste system in the embodiment is the color paste containing the functional cross-linking assistant capable of promoting the stability of the color paste system prepared in the embodiment 3.
Comparative example 1
The preparation method of the color paste comprises the following steps:
1. dispersing citric acid in deionized water, adding attapulgite at the stirring speed of 1000r/min, continuously stirring for 50min, filtering to obtain filter residue, washing the filter residue with deionized water, and drying at 75 ℃ for 4h to obtain a functional crosslinking auxiliary agent capable of promoting the stability of a color paste system; wherein the mass ratio of the citric acid to the deionized water to the attapulgite is 7:120:3;
2. stirring propylene glycol, polyethylene glycol 200, antirust benzotriazole, preservative GXL, polystyrene maleic anhydride copolymerized ammonium salt, defoaming agent SN-1340, acrylic resin, functional crosslinking auxiliary agent capable of promoting the stability of a color paste system, pigment and deionized water at a stirring speed of 600r/min for 40min, adding triethanolamine to adjust the pH value, stirring for 30min at a stirring speed of 3000r/min by using a high-speed shearing emulsion stirrer to obtain a color paste raw material, and transferring the color paste raw material to a sand mill to grind to obtain color paste; the mass ratio of propylene glycol, polyethylene glycol 200, antirust agent benzotriazole, preservative GXL, polystyrene maleic anhydride copolymer ammonium salt, defoaming agent SN-1340, acrylic resin, functional cross-linking auxiliary agent capable of promoting the stability of a color paste system, pigment, deionized water and triethanolamine is 25:25:15:15:2:0.5:62.5:15:75:220:15.
comparative example 2
The preparation method of the color paste comprises the following steps:
1. mixing attapulgite and toluene, carrying out ultrasonic dispersion for 25min under the condition that the ultrasonic power is 650W, adding gamma-aminopropyltriethoxysilane, and reacting for 9h at 80 ℃; after the reaction is finished, filtering to obtain filter residues, washing the filter residues with ethanol, and drying at 70 ℃ for 11 hours to obtain modified attapulgite; wherein the mass ratio of the attapulgite to the gamma-aminopropyltriethoxysilane to the toluene is 1:1:15;
2. stirring propylene glycol, polyethylene glycol 200, antirust benzotriazole, preservative GXL, polystyrene maleic anhydride copolymerized ammonium salt, defoaming agent SN-1340, acrylic resin, modified attapulgite, pigment and deionized water at a stirring speed of 600r/min for 40min, adding triethanolamine to adjust the pH value, stirring for 30min at a stirring speed of 3000r/min by using a high-speed shearing emulsion stirrer to obtain a color paste raw material, and transferring the color paste raw material into a sand mill to grind to obtain color paste; the weight ratio of propylene glycol, polyethylene glycol 200, antirust benzotriazole, preservative GXL, polystyrene maleic anhydride copolymer ammonium salt, defoaming agent SN-1340, acrylic resin, modified attapulgite, pigment, deionized water and triethanolamine is 25:25:15:15:2:0.5:62.5:15:75:220:15.
comparative example 3
The preparation method of the color paste comprises the following steps:
stirring propylene glycol, polyethylene glycol 200, antirust benzotriazole, preservative GXL, polystyrene maleic anhydride copolymerized ammonium salt, defoaming agent SN-1340, acrylic resin, pigment and deionized water at a stirring speed of 600r/min for 40min, adding triethanolamine to adjust the pH value, stirring for 30min at a stirring speed of 3000r/min by using a high-speed shearing emulsifying mixer at room temperature to obtain a color paste raw material, and transferring the color paste raw material into a sand mill to grind to obtain color paste; the weight ratio of propylene glycol, polyethylene glycol 200, antirust benzotriazole, preservative GXL, polystyrene maleic anhydride copolymer ammonium salt, defoaming agent SN-1340, acrylic resin, pigment, deionized water and triethanolamine is 25:25:15:15:2:0.5:62.5:75:220:15.
in comparative examples 1 to 3, the conditions for grinding the color paste raw material were the same as in examples 1 to 5.
The pigment used in all the above examples and comparative examples is not particularly limited, and pigments generally used for water-based inks can be used, and specifically, it includes inorganic pigments such as carbon black, which can be used for making black neutral inks; organic pigments such as copper phthalocyanine blue 15:1 or copper phthalocyanine blue 15:3, the blue neutral ink can be prepared; the organic pigment permanent red P.R.9 or permanent red P.R.16 can be used for preparing red neutral ink.
In all of the above examples and comparative examples, the attapulgite was obtained from Dongguan Shengde New Material Co., ltd, model number R-860; preservative GXL, from Nanjing chime sea commercial trade Co., ltd, model: PROXEL-GXL; the defoaming agent SN-1340 is from Nopopco auxiliary company, model number: SN-DEFAOMER 1340; acrylic resins are available from Shanghai Yue New Material science and technology Co., ltd, type: TY773; lubricant MOA-3P (fatty alcohol ether phosphate) from Haian petrochemical plant, CAS number 25852-45-3; thickener ALCOGUARD5800 (hydrophobically modified acrylic acid alkali swellable type) from akksonobel surface chemistry ltd, netherlands; thickener T-938 (hydrophobically modified acrylic acid alkali swellable type) from Guangzhou Wen and trade company Limited.
Test examples
(1) D for testing color paste 90 Particle size: the particle size of the color paste prepared in the examples 1-5 and the comparative examples 1-3 is measured, and the test method comprises the following steps: taking 0.4g of color paste, adding 250g of deionized water for dilution, dispersing for 6min by using ultrasonic waves, standing for 5min, adding into a circulating sample injection system, and starting to test the particle size when the shading degree is about 9.0. Considering that the larger the subscript, the worse the reliability of the measured value, D was used for the experiment 90 I.e. the particle size at which the cumulative distribution is 90%, is characterized as a determination. The test results are shown in table 1:
TABLE 1
Figure 465298DEST_PATH_IMAGE001
As can be seen from the test results in Table 1, the color pastes prepared in examples 1-5 and comparative examples 1-3 of the present invention have good fineness and particle uniformity, and the particle size is about 129 nm. The smaller the fineness is, the higher the particle uniformity is, and the higher the stability of the color paste is.
(2) Testing the stability of the color paste: the specific absorbance of the color pastes prepared in the examples 1-5 and the comparative examples 1-3 is measured, and the test method comprises the following steps: diluting a small amount of color paste by several times, measuring the absorbance A at the wavelength of 510nm by using an ultraviolet-visible spectrophotometer, then placing a certain amount of diluted color paste in a high-speed centrifuge, setting the centrifugation speed to 3000r/min, centrifuging for 30min, measuring the absorbance A 'of the centrifuged system, comparing the absorbance A' with the absorbance A, and calculating the specific absorbance. 3 samples were tested and averaged.
The calculation formula of the specific absorbance is as follows:
r/%=A′/A×100
in the formula:Ais the absorbance at the maximum absorption wavelength before centrifugation;A′is the absorbance at the maximum absorption wavelength after centrifugation;ris the specific absorbance.
The test results are shown in table 2:
TABLE 2
Figure 585701DEST_PATH_IMAGE002
As can be seen from the test results in Table 2, the color paste prepared in the embodiments 1-5 of the present invention can maintain a specific absorbance of more than 90% after being centrifuged at a centrifugation speed of 3000r/min for 30min, and has good stability; in comparative examples 1-3, even though the fineness and uniformity of the color paste are equivalent to those of examples 1-5, in comparative example 1, when the color paste is prepared, the attapulgite is not modified by gamma-aminopropyltriethoxysilane, the amino group is lack of the combination effect of the amino group and carboxyl group in the crosslinking assistant, the crosslinking degree of a crosslinking system is reduced, and the stability of the color paste is reduced; in the comparative example 2, when the color paste is prepared, the modified attapulgite does not react with the cross-linking assistant citric acid, so that the groups on the surface of the attapulgite, which are combined with the active groups on the acrylic resin, are reduced, the cross-linking degree of a cross-linking system is reduced, and the stability of the color paste is reduced; in the comparative example 3, no additive capable of promoting the stability of the color paste system is added, and the stability of the color paste is obviously reduced.
Example 7
This example provides a sand mill which satisfies the grinding treatment of the mill base in the preparation of mill base in examples 1 to 5 and comparative examples 1 to 3.
Referring to fig. 5-6, a sand mill comprises a sand mill body 1, an outer feeding cylinder 2 is fixedly installed on the sand mill body 1, an inner grinding cylinder 3 is rotatably assembled inside the outer feeding cylinder 2, a dispersion disc 4 is rotatably assembled inside the inner grinding cylinder 3, zirconia beads are filled inside the inner grinding cylinder 3, the inner grinding cylinder 3 and the dispersion disc 4 are driven by a driving assembly 7 to synchronously rotate in reverse direction so as to drive the zirconia beads filled between the dispersion discs 4 to move, so that the zirconia beads in the inner grinding cylinder 3 are driven to move at high speed and generate strong collision, friction and shearing action with color paste raw materials through the reverse rotation of the inner grinding cylinder 3 and the dispersion disc 4, and the grinding and dispersion of particles in the color paste raw materials are realized; discharge holes capable of discharging materials in one direction are uniformly formed in the surface of the side wall of the inner grinding cylinder 3, so that the ground color paste raw materials obtained by grinding the color paste raw materials in the inner grinding cylinder 3 by zirconia beads can be uniformly thrown into a material conveying cavity formed between the outer wall of the inner grinding cylinder 3 and the inner wall of the outer material conveying cylinder 2 from each discharge hole under the action of centrifugal force; specifically, 4 rotational speeds of dispersion impeller are the twice of interior grinding vessel 3 rotational speeds at least, to guarantee that 4 centrifugal forces that rotate the in-process production of dispersion impeller can drive the zirconia pearl and the mill base raw materials in interior grinding vessel 3 and throw away the inner wall to interior grinding vessel 3 vigorously, thereby the mill base raw materials in interior grinding vessel 3 are by the zirconia pearl fully grinding with the dispersion back, the mill base raw materials after zirconia pearl and grinding can be by even striking to 3 inner wall surfaces of interior grinding vessel, make the zirconia pearl that disperses to each discharge gate department and the mill base raw materials evenly distributed after the grinding, and then avoid appearing the condition that the discharge gate is blockked up by the zirconia pearl of a large amount of aggregations.
Further, referring to fig. 7-8, the inner grinding cylinder 3 further includes a plurality of check valves 34 respectively disposed on the discharge holes disposed on the sidewall surface of the inner grinding cylinder 3, a filter screen is disposed on one side of the discharge holes and located on one side of the liquid inlet of the check valve 34, the check valves 34 are respectively located between two adjacent circles of threaded protrusions on the outer wall surface of the grinding cylinder 31, so that when the inner grinding cylinder 3 grinds and disperses the color paste raw material, the check valves 34 are kept closed when the grinding time does not reach the set grinding time, the color paste raw material having a particle diameter smaller than the pore diameter of the filter screen but not fully mixed with other components can be prevented from being directly discharged to the material delivery cavity for discharging, the influence on the component uniformity of the color paste is avoided, when the grinding time reaches the set grinding time, and the color paste raw material is basically dispersed and mixed, the check valves 34 are opened, and then along with the centrifugal force that the dispersion disk 4 rotates and produces, drive the mill base raw materials of zirconia pearl and mill and throw away to the inner wall of interior grinding vessel 3 vigorously, the granule that the particle diameter is greater than the filter screen aperture in the mill base raw materials after the mill can't pass through the filter screen, will sneak into and continue to grind between the zirconia pearl, the granule that the particle diameter is less than the filter screen aperture in the mill base raw materials after the mill can be thrown away directly fast through the filter screen and the check valve 34 of discharge opening one side, and evenly disperse to the spiral channel in the grinding barrel 31 outside, and arrange to the mill base raw materials after the spiral channel in can't get into inside grinding barrel 31 again, make the mill base raw materials after the mill that remains in interior grinding vessel 3 reduce gradually until discharging completely, can not produce material and repeated grinding, in order to improve the mill base's the grinding of the inside residual mill base of interior grinding vessel 3 that blocks up, the separation effect.
Furthermore, the aperture of the filter screen is 0.15 μm, and the ground color paste raw material passing through the filter screen of the discharge hole is the color paste; when the grinding device is used, after color paste raw materials are placed in the inner grinding cylinder 3, the driving assembly 7 is started, the driving assembly 7 can drive the inner grinding cylinder 3 and the dispersion disc 4 to rotate reversely, and the rotating speed of the dispersion disc 4 is at least twice of that of the inner grinding cylinder 3, so that the dispersion disc 4 drives the zirconia beads filled in the inner grinding cylinder 3 to move at a high speed in the process of high-speed rotation, and the zirconia beads in the inner grinding cylinder 3 and the color paste raw materials generate strong collision, friction and shearing actions with each other, thereby realizing grinding and dispersion of color paste raw material particles; mill base raw materials in interior grinding vessel 3 is after fully grinding, 4 centrifugal force drive zirconia pearls that rotate the production of dispersion impeller and mill base raw materials after grinding vigorously get rid of the inner wall to interior grinding vessel 3, the granule that the particle diameter is greater than filter screen aperture in the mill base raw materials after grinding can't be sneaked into between the zirconia pearls through the discharge opening and is continued the grinding, the granule that the particle diameter is less than filter screen aperture in the mill base raw materials after grinding can directly be thrown away by directly after being thrown away the discharge opening place on 3 inner walls of interior grinding vessel, and the even dispersion is to the defeated material intracavity that forms between 3 outer walls of interior grinding vessel and the outer 2 inner walls of outer conveying tube, be provided with out the discharge gate on the outer discharge gate, can emit the mill base through opening the discharge gate.
Further, the color paste is further screened according to the particle size, one end of an inner grinding cylinder 3 is fixedly connected with an inner extending cylinder 5 and a separator 6 in sequence, the outer wall surfaces of the inner grinding cylinder 3 and the inner extending cylinder 5 are respectively provided with a threaded bulge, a spiral channel is formed between the side wall of the threaded bulge and the outer wall of the inner grinding cylinder 3 and the outer wall of the inner extending cylinder 5, the inner grinding cylinder 3 and the inner extending cylinder 5 rotate to enable the color paste entering a material conveying cavity to be uniformly conveyed to the separator 6 along the spiral channel and then discharged, the separator 6 rotates to screen the color paste, so that the color paste entering the material conveying cavity is uniformly dispersed in the spiral channel and is uniformly and continuously conveyed to the position of the separator 6 along with the rotation of the inner grinding cylinder 3 and the inner extending cylinder 5, the separator 6 only needs to separate a small amount of color paste within a unit time in the high-speed rotation process, further, a large amount of color paste is prevented from being accumulated in the working area of the separator 6, the separator 6 can efficiently separate relatively large particles in the color paste, large particles and small particles in the color paste can be screened, and actual requirements of different particle sizes of color pastes can be met in factories.
Along with the rotation of the inner grinding cylinder 3 and the inner extension cylinder 5, color paste in the material conveying cavity can be uniformly and continuously conveyed to the position of the separator 6 along the spiral channel, the color paste is discharged through the high-speed rotation of the separator 6, and relatively large particles in the color paste are screened out, so that the color paste is further screened.
Further, referring to fig. 7-8, the inner grinding cylinder 3 includes a grinding cylinder 31, first sealing caps 32, and first shaft sleeves 33, the first sealing caps 32 are respectively and fixedly mounted at two ends of the grinding cylinder 31, the first shaft sleeves 33 are respectively disposed on the two first sealing caps 32, one end of the inner extending cylinder 5 is fixedly connected with one end of the grinding cylinder 31, the other end of the inner extending cylinder 5 is fixedly connected with the separator 6, and the separator 6 is communicated with the material conveying cavity, so that the driving assembly 7 can drive the inner extending cylinder 5 and the separator 6 to synchronously rotate when driving the inner grinding cylinder 3 to rotate, so that the color paste discharged from the discharge hole and dispersed in the spiral channel at the outer side of the inner grinding cylinder 3 can be sequentially conveyed into the spiral channel at the outer side of the inner extending cylinder 5 in a uniformly dispersed state, and then continuously conveyed to the position of the separator 6, as the separator 6 rotates at a high speed to generate turbulence, relatively large particles in the color paste are screened and blocked at the outer side of the separator 6, and small amount of the color paste screened in the separator 6 per unit time can greatly improve the screening effect on the color paste; 6 tip of separator rotates and is equipped with the sealed lid 61 of second and 6 tip of separator and the sealed lid 61 surface of second keep sealed, in order to guarantee the gas tightness of 6 tips of separator, avoid the interior fluid of separator 6 to spill over, fixedly connected with second shaft sleeve 62 on the sealed lid 61 of second, outer defeated feed cylinder 2 both ends are provided with outer shaft sleeve 21 respectively, keep away from and pass through first bearing normal running fit between the outer wall of a first shaft sleeve 33 of separator 6 and the outer shaft sleeve 21 inner wall that the position corresponds, pass through seal cover fixed connection between the outer wall of second shaft sleeve 62 and the outer shaft sleeve 21 inner wall that the position corresponds, first bearing both sides are provided with the sealing washer respectively, in order to guarantee the gas tightness at outer defeated feed cylinder 2 both ends, avoid outer defeated feed cylinder 2 internal fluid to spill over.
Further, referring to fig. 7-8, an inner feed port 35 is disposed at an end of the mill cylinder 31 away from the separator 6, an outer feed pipe 22 is disposed on the outer feed cylinder 2, a feed valve is disposed on the inner feed port 35, when the mill cylinder 31 rotates to a position where the inner feed port 35 corresponds to the outer feed pipe 22, after the feed valve is opened, an outer pipe can be inserted into the inner feed port 35 through the outer feed pipe 22 for feeding, so that the outer pipe can be inserted into the inner feed port 35 through the outer feed pipe 22, and the feed valve is opened, so that the color paste raw material can sequentially enter the mill cylinder 31 through the outer pipe, the outer feed pipe 22, and the inner feed port 35 for feeding; the second sealing cover 61 is provided with a discharging pipe 63, the discharging pipe 63 is provided with a discharging valve, the discharging pipe 63 extends to the outside of the outer feeding barrel 2, and the discharging pipe 63 is communicated with a liquid outlet in the separator 6, so that the discharging pipe 63 is communicated with an external pipeline, after grinding and separation of color paste are completed in the outer feeding barrel 2, the discharging valve is opened, the color paste screened by the separator 6 can be discharged into a storage container through the discharging pipe 63 and the external pipeline in sequence, and screening and discharging of the color paste are completed.
Further, referring to fig. 5 and 7, the driving assembly 7 includes a driving source 71, a first rotating shaft 72, and a second rotating shaft 73, belt pulleys are respectively disposed at one end of a driving shaft of the driving source 71 and one end of the first rotating shaft 72, a transmission belt is disposed between the two belt pulleys, the first rotating shaft 72 extends into the inner extending cylinder 5 and the inner grinding cylinder 3, the dispersion discs 4 are respectively fixedly sleeved on the surface of the first rotating shaft 72, so that the driving source 71 can drive the corresponding belt pulley to rotate, the transmission belt drives the other belt pulley to rotate, and further drives the first rotating shaft 72 to rotate, and the first rotating shaft 72 drives the dispersion discs 4 to rotate at a high speed, so that the zirconia beads between the dispersion discs 4 move at a high speed to grind and disperse the color paste raw material in the grinding cylinder 31; second pivot 73 one end is rotated and is assembled at 2 tip on the defeated feed cylinder outside, fixed cover respectively is equipped with intermeshing's first gear 721 and second gear 731 on first pivot 72 and the second pivot 73, it is provided with drive rack 51 to extend 5 inner wall surfaces of section of thick bamboo to encircle, second gear 731 meshes with drive rack 51, thereby during the first pivot 72 of driving source 71 drive is rotatory, first pivot 72 can be rotatory through the meshing transmission drive second pivot 73 between first gear 721 and the second gear 731, it is rotatory to extend 5 in the meshing transmission drive between rethread second gear 731 and the drive rack 51, and then extend 5 drives grinding vessel 31, separator 6 synchronous revolution. Specifically, the driving source 71 is preferably a servo motor.
The two ends of the first rotating shaft 72 are respectively assembled inside the first shaft sleeve 33 and the second shaft sleeve 62 corresponding to the positions through the rotation of the second bearings, and the two sides of the second bearings are respectively provided with a sealing ring so as to ensure the air tightness of the end part of the grinding cylinder body 31 and avoid the overflow of fluid in the grinding cylinder body 31.
Further, referring to fig. 7-8, the inner wall surface of the grinding cylinder 31 is uniformly provided with a convex ring 311, the convex ring 311 and the dispersion plate 4 are distributed in a staggered manner, two openings with opposite positions are formed on the convex ring 311, and the openings and the check valves 34 are respectively distributed on the same axis, so that the collision frequency of the zirconia beads in the grinding cylinder 31 is increased through the staggered distribution of the convex ring 311 and the dispersion plate 4, and the grinding effect of the zirconia beads on the color paste raw material in the high-speed movement process is further improved.
Further, referring to fig. 5 to 6, the main body 1 of the sand mill includes a base 11, a housing 12, a control unit 13 and a carrier 14, the housing 12, the control unit 13 and the carrier 14 are respectively fixedly installed on the base 11, a driving source 71 is fixedly installed inside the housing 12, the outer feed cylinder 2 is fixedly installed on the carrier 14, and the control unit 13 is used for controlling the operation of the device.
When the mill is used, an external pipeline penetrates through the external feeding pipe 22 and is inserted into the internal feeding hole 35, the feeding valve is opened, color paste raw materials sequentially enter the interior of the grinding cylinder 31 through the external pipeline, the external feeding pipe 22 and the internal feeding hole 35, the feeding valve is closed after the feeding is finished, and the external pipeline is taken down; keeping the one-way valve 34 closed, starting the driving source 71, wherein the driving source 71 can drive the first rotating shaft 72 to rotate through the cooperation of a belt pulley and a transmission belt, the first rotating shaft 72 drives the dispersion disc 4 to rotate at a high speed, the first rotating shaft 72 can drive the inner extension cylinder 5 to rotate through the meshing transmission between the first gear 721 and the second gear 731 and the meshing transmission between the second gear 731 and the transmission rack 51 while rotating, the inner extension cylinder 5 drives the grinding cylinder body 31 and the separator 6 to synchronously rotate, and the rotating directions of the inner extension cylinder 5 and the dispersion disc 4 are opposite; the dispersion disc 4 drives the zirconia beads filled in the grinding cylinder 31 to move at a high speed in the process of high-speed rotation, and the zirconia beads and the color paste raw materials generate strong collision, friction and shearing actions with each other to grind and disperse the color paste raw material particles; after the set grinding time is reached, the one-way valve 34 is opened, the centrifugal force generated by the rotation of the dispersion disc 4 drives the zirconia beads and the color paste to be greatly thrown to the inner wall of the grinding cylinder 31, particles with the particle diameter larger than the aperture of the filter screen in the ground color paste raw materials cannot pass through the filter screen and can be mixed into the zirconia beads to be continuously ground, and particles with the particle diameter smaller than the aperture of the filter screen in the ground color paste raw materials can be directly and quickly thrown out through the filter screen and the one-way valve 34 and are uniformly dispersed into a spiral channel on the outer side of the grinding cylinder 31; the discharge pipe 63 is communicated with an external pipeline, the discharge valve is opened, color paste in the spiral channel can be continuously conveyed to the position of the separator 6 in a uniformly dispersed state along with the synchronous rotation of the grinding cylinder body 31, the inner extension cylinder 5 and the separator 6, turbulence is generated along with the high-speed rotation of the separator 6, relatively large particles in the color paste are screened and blocked outside the separator 6, and the rest color paste completely enters a liquid outlet at the inner side of the separator 6 and is discharged into a storage container through the discharge pipe 63 and the external pipeline in sequence; further, the sum of the set grinding time before the check valve 34 is opened and the time for continuing grinding after the check valve 34 is opened is the grinding time.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that various changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (10)

1. The preparation method of the color paste containing the functional cross-linking auxiliary agent capable of promoting the stability of the color paste system is characterized by comprising the following steps:
mixing attapulgite and toluene, performing ultrasonic dispersion, adding gamma-aminopropyltriethoxysilane, reacting at 70-100 ℃ for 6-10h, filtering to obtain filter residue, washing the filter residue, and drying to obtain modified attapulgite;
dispersing the crosslinking aid in deionized water, adding the modified attapulgite under stirring, continuing stirring for 30-60min, filtering to obtain filter residue, and washing and drying the filter residue to obtain the functional crosslinking aid capable of promoting the stability of the color paste system;
stirring and mixing propylene glycol, polyethylene glycol 200, antirust benzotriazole, preservative, polystyrene maleic anhydride copolymer ammonium salt, defoaming agent, acrylic resin, functional cross-linking auxiliary capable of promoting stability of a color paste system, pigment and deionized water, adding triethanolamine to adjust pH, stirring by using a high-speed shearing emulsifying stirrer to obtain a color paste raw material, transferring the color paste raw material into a sand mill, and grinding to obtain a color paste containing the functional cross-linking auxiliary capable of promoting stability of the color paste system; wherein, the mass ratio of the propylene glycol, the polyethylene glycol 200, the antirust agent benzotriazole, the preservative, the polystyrene maleic anhydride copolymerized ammonium salt, the defoaming agent, the acrylic resin, the functional cross-linking auxiliary agent capable of promoting the stability of the color paste system, the pigment, the deionized water and the triethanolamine is 25:25:15:15:2:0.5:62.5: (12-20): 75: (215-223): 15.
2. the method for preparing color paste containing functional crosslinking assistant capable of promoting stability of color paste system according to claim 1, wherein in the step (1), the mass ratio of attapulgite, gamma-aminopropyltriethoxysilane and toluene is 1:1: (10-30).
3. The method for preparing the color paste containing the functional crosslinking assistant capable of promoting the stability of the color paste system according to claim 1, wherein in the step (2), the mass ratio of the crosslinking assistant to the deionized water to the modified attapulgite is (5-10): (100-150): (2-4.5); the crosslinking assistant comprises any one of citric acid and malic acid.
4. A mill base containing a functional cross-linking aid for promoting the stability of the mill base system, prepared by a process according to any one of claims 1 to 3.
5. A neutral ink prepared from a mill base containing a functional cross-linking aid for enhancing the stability of a mill base system according to claim 4, wherein the neutral ink is prepared by the steps of:
stirring and mixing propylene glycol, polyethylene glycol 200, a lubricant, a thickening agent and deionized water, then adding triethanolamine to adjust the pH value, adding color paste containing a functional cross-linking auxiliary agent capable of promoting the stability of a color paste system under the stirring condition, continuously stirring, and filtering to obtain neutral ink; the weight ratio of propylene glycol, polyethylene glycol 200, lubricant, thickener, deionized water, triethanolamine and color paste containing functional cross-linking auxiliary agent capable of promoting the stability of color paste system is 25:25:5: (11-13): 173:10:250.
6. a sand mill used for the preparation method of color paste containing functional cross-linking auxiliary agent capable of promoting the stability of color paste system according to claim 1, which is characterized by comprising a sand mill main body, wherein an outer feeding cylinder is fixedly arranged on the sand mill main body, an inner grinding cylinder is rotationally assembled in the outer feeding cylinder, a dispersion disc is rotationally assembled in the inner grinding cylinder, zirconium oxide beads are filled in the inner grinding cylinder, and the inner grinding cylinder and the dispersion disc are driven by a driving component to synchronously rotate in reverse directions so as to drive the zirconium oxide beads filled in the dispersion disc to move; the surface of the side wall of the inner grinding cylinder is uniformly provided with discharge holes capable of discharging materials in a one-way mode, so that color paste raw materials are ground in the inner grinding cylinder through zirconia beads, and are thrown into a material conveying cavity formed between the outer wall of the inner grinding cylinder and the inner wall of the outer material conveying cylinder from the discharge holes under the action of centrifugal force.
7. The sand mill for preparing color paste containing functional crosslinking aids for promoting the stability of a color paste system according to claim 6, wherein one end of the inner grinding cylinder is fixedly connected with an inner extending cylinder and a separator in sequence, the outer wall surfaces of the inner grinding cylinder and the inner extending cylinder are both provided with threaded protrusions, a spiral channel is formed between the side wall of each threaded protrusion and the outer wall of the inner grinding cylinder and the outer wall of the inner extending cylinder, and the color paste entering a material conveying cavity can be uniformly conveyed to the separator along the spiral channel by the rotation of the inner grinding cylinder and the inner extending cylinder; the inner grinding cylinder comprises a grinding cylinder body, a first sealing cover and a first shaft sleeve, the first sealing covers are respectively and fixedly arranged at two ends of the grinding cylinder body, the first shaft sleeves are respectively arranged on the first sealing covers, one end of the inner extension cylinder is fixedly connected with one end of the grinding cylinder body, the other end of the inner extension cylinder is fixedly connected with the separator, and the separator is communicated with the material conveying cavity; the separator end part is rotatably assembled with a second sealing cover, the separator end part and the surface of the second sealing cover are kept sealed, the second sealing cover is fixedly connected with a second shaft sleeve, two ends of an outer material conveying cylinder are respectively provided with an outer shaft sleeve, the outer wall of one first shaft sleeve far away from the separator is in rotating fit with the inner wall of the outer shaft sleeve corresponding to the position through a first bearing, and the outer wall of the second shaft sleeve is fixedly connected with the inner wall of the outer shaft sleeve corresponding to the position through a sealing sleeve.
8. The sand mill for the preparation method of color paste containing functional cross-linking agents capable of promoting the stability of a color paste system according to claim 7, wherein an inner feed port is arranged at one end of the grinding cylinder body away from the separator, an outer feed pipe is arranged on the outer feed cylinder, a feed valve is arranged on the inner feed port, when the grinding cylinder body rotates to the position that the inner feed port corresponds to the outer feed pipe, an outer pipeline can be inserted into the inner feed port through the outer feed pipe to feed materials after the feed valve is opened; a discharge pipe is arranged on the second sealing cover, a discharge valve is arranged on the discharge pipe, the discharge pipe extends to the outside of the outer material conveying barrel and is communicated with a liquid outlet in the separator; the inner grinding cylinder further comprises a one-way valve, the one-way valve is arranged on a discharge hole formed in the surface of the side wall of the inner grinding cylinder respectively, a filter screen is arranged on one side of the discharge hole and located on one side of a liquid inlet of the one-way valve, and the one-way valve is located between two adjacent circles of thread protrusions on the surface of the outer wall of the grinding cylinder body respectively.
9. The sand mill for the preparation method of color paste containing functional cross-linking agents capable of promoting the stability of color paste systems according to claim 7, wherein the inner wall surface of the grinding cylinder body is uniformly provided with a convex ring, the convex ring is provided with two openings at opposite positions, and the openings are respectively distributed on the same axis with the one-way valve.
10. The sander for use in a process for producing mill base containing functional coupling aids that promote stability of mill base systems as set forth in claim 6, wherein said drive assembly comprises a drive source, a first shaft, a second shaft, a pulley is disposed at each of a drive shaft of said drive source and an end of said first shaft, a drive belt is disposed between said pulleys, said first shaft extends into said inner extension drum and said inner grinding drum, and said dispersion discs are respectively fixedly attached to a surface of said first shaft; second pivot one end is rotated the assembly and is in on the outer defeated feed cylinder tip inner wall, first pivot with fixed cover is equipped with intermeshing's first gear and second gear respectively in the second pivot, interior extension section of thick bamboo inner wall surface encircles and is provided with the transmission rack, the second gear with the meshing of transmission rack.
CN202211161663.2A 2022-09-23 2022-09-23 Color paste containing functional crosslinking auxiliary agent capable of promoting stability of color paste system, preparation method thereof and application thereof in neutral ink Active CN115304961B (en)

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Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102532975A (en) * 2011-12-27 2012-07-04 深圳市乐普泰科技股份有限公司 Nano aqueous conductive carbon black color paste and preparation method thereof
CN109021697A (en) * 2018-06-25 2018-12-18 太原理工大学 A kind of preparation method of lubricious Pigment type neutral ink
CN208407180U (en) * 2018-05-24 2019-01-22 武汉宏桥涂料股份有限公司 A kind of horizontal sand mill
CN110523371A (en) * 2019-09-10 2019-12-03 河海大学 It is a kind of attapulgite modified and its preparation method and application
CN110947471A (en) * 2018-09-26 2020-04-03 安徽儒特实业有限公司 Sand mill with high efficiency and stable performance

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102532975A (en) * 2011-12-27 2012-07-04 深圳市乐普泰科技股份有限公司 Nano aqueous conductive carbon black color paste and preparation method thereof
CN208407180U (en) * 2018-05-24 2019-01-22 武汉宏桥涂料股份有限公司 A kind of horizontal sand mill
CN109021697A (en) * 2018-06-25 2018-12-18 太原理工大学 A kind of preparation method of lubricious Pigment type neutral ink
CN110947471A (en) * 2018-09-26 2020-04-03 安徽儒特实业有限公司 Sand mill with high efficiency and stable performance
CN110523371A (en) * 2019-09-10 2019-12-03 河海大学 It is a kind of attapulgite modified and its preparation method and application

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