CN112280381A

CN112280381A - Neutral erasable ink composition and preparation method thereof

Info

Publication number: CN112280381A
Application number: CN202011284820.XA
Authority: CN
Inventors: 马振海; 闫西安
Original assignee: Individual
Current assignee: Individual
Priority date: 2020-11-17
Filing date: 2020-11-17
Publication date: 2021-01-29

Abstract

The invention discloses a neutral erasable ink composition and a preparation method thereof, belonging to the technical field of ink preparation and comprising the following raw materials: 2-10% of alcohol-soluble dye, 25-35% of film-forming agent, 0.5-1% of lubricating agent, 0.5-1% of surfactant, 0.5-1% of stabilizing agent, 1-2% of thickening agent, 10-15% of dispersing agent, 30-45% of solvent, 0.5-1% of flatting agent and 0.05-0.5% of defoaming agent; the preparation method comprises the following preparation steps: pretreating the color base pigment, adding auxiliary materials, mixing, ball milling, dispersing, preparing and softening pigment aggregates in the form of an atomized solvent and a wetting agent, performing high-speed shearing, depolymerization and pre-dispersion to obtain sub-nanometer particles, defoaming and filtering. The ink has good writing performance, no obvious trace on the back of writing paper, and can be easily erased by using a common eraser.

Description

Neutral erasable ink composition and preparation method thereof

Technical Field

The invention relates to the technical field of ink preparation, in particular to a neutral erasable ink composition and a preparation method thereof.

Background

Ink is one of important writing materials in human society, and neutral ink is an important reason for restricting the development of neutral pens due to its special properties. The current market has large demand for neutral ink, and the development market prospect and the economic benefit are very considerable.

In the prior art, the quality of the properties of the gel-ink pen is mainly reflected in the formula of the ink components and the preparation method. During the preparation process, the viscosity, surface tension and pH value of the ink must be kept at certain values so as to ensure the quality of the ink. Meanwhile, the prepared ink is smooth and continuous in writing, the stability of the ink is kept, the ink is ensured not to deteriorate, the phenomena of layering, precipitation and the like are avoided after the ink is kept for a long time, and the safety, the non-toxicity and the non-corrosiveness of the ink are also ensured.

Meanwhile, the writing of the ordinary gel ink pen is usually difficult to erase in the actual use process. However, in many cases, for example, students are inevitably wrongly written in the actual use process, and need to modify the writing by using a correction fluid or a correction tape, which often causes untidy rolling surface and inconvenience.

The development of the gel ink pen is severely restricted by the ink preparation process of the gel ink pen. The quality index of the gel pen requires that the ink reaches a certain particle fineness which is lower than the gap between the ball and the ball seat, and has strong dispersing capacity to prevent the pen point from being blocked to influence writing, which puts high requirements on the ball milling process. However, in the ball milling step, because the ball mill is not sufficient in grinding the materials when processing the materials, the grinding effect is not good, the particles are not uniform, the particle size does not meet the requirements, and the quality of the prepared finished product is poor; simultaneously, when stirring thick liquids, the thick liquids spatters on the barrel inner wall, makes original material ratio unbalance, and production efficiency is lower.

Disclosure of Invention

Technical problem to be solved

Aiming at the defects in the prior art, the invention aims to provide a neutral erasable ink composition, which has the advantages of uniform ink discharge flow, smooth writing, better stability and durability, safety and environmental protection, and most importantly, handwriting can be easily erased, so that the problems in the background art are solved, and meanwhile, in the ball milling step, the problems of insufficient ball milling, non-uniform particle size and the like exist due to the low efficiency of a used ball mill, so that the quality of a finished product is poor, and the grinding step is improved.

(II) technical scheme

In order to achieve the purpose, the invention provides the following technical scheme:

the neutral erasable ink composition is characterized by comprising the following raw materials in percentage by mass:

2-10% of alcohol-soluble dye;

25-35% of film-forming agent;

0.5-1% of lubricant;

0.5-1% of surfactant;

0.5 to 1 percent of stabilizer;

1-2% of a thickening agent;

10-15% of a dispersant;

30-45% of a solvent;

3-5% of a wetting agent;

0.5 to 1 percent of flatting agent;

0.05 to 0.5 percent of defoaming agent;

the film forming agent is one or more of hydroxymethyl cellulose, acrylic resin modified casein film forming agent, acrylic resin polyurethane copolymer resin, polyethylene, acrylic ester modified butadiene resin and polyurethane modified nitrocellulose film forming agent;

the lubricant is one or more of glycerol, fatty acyl diethanolamine and methyl silicone oil;

the surfactant is one or more of sodium lauryl sulfate, fatty alcohol-polyoxyethylene ether and monolauryl phosphate;

the stabilizer is one or more of sodium alginate and ethanolamine;

the thickening agent is one or more of polyacrylic acid, polyacrylamide, polyvinyl alcohol, polyvinylpyrrolidone and polyethylene oxide;

the dispersing agent is one or more of methylene dinaphthalene sodium sulfonate, triethyl hexyl phosphoric acid, sodium dodecyl sulfate, methyl amyl alcohol, polyacrylamide and fatty acid polyglycol ester;

the solvent is one or more of ethanol, n-propanol, butanol, isopropanol and pentanol;

the leveling agent is one or more of octylphenol, 4-nonylphenol ethoxylate, acetylenic diol or polyether modified polysiloxane;

the defoaming agent is fumed silica or polysiloxane, or organic silicon compound and surfactant are compounded, polyether and organic silicon are compounded, and water-soluble or oil-soluble polyether and silicon-containing polyether are compounded.

Preferably, the method of preparing the neutral erasable ink composition comprises the steps of:

s1, preprocessing alcohol-soluble dye, putting different color-based pigments into a wet ball mill, grinding for 10-20min, and then sieving with a 100-mesh sieve;

s2, preparing a mixed solution, mixing the stabilizer and the dispersant in parts by weight in a wet ball mill according to a proportion, grinding for 10-20min, then adding the thickener and the flatting agent in parts by weight again, adjusting the stirring speed to 400-600rpm, and stirring for 10-20min to ensure that the viscosity of the mixed solution is 0.01-0.05 cP;

s3, centrifuging and washing the mixed solution, adjusting the pH value of the mixed solution to be within the range of 7.0-7.5 by using an ammonium acetate buffer solution, standing for 1-2h at room temperature, placing the mixed solution in a centrifuge for centrifugation, adjusting the centrifugation speed to 3000-5000rpm, centrifuging for 10-15min, repeating the centrifugation for three times, collecting the precipitate, and washing and purifying the precipitate for multiple times by using deionized water;

s4, preparing a pigment aggregate, blowing and drying the obtained precipitate by nitrogen, controlling the temperature of the nitrogen flow to be 40-60 ℃ to obtain a dried dispersed pigment, flatly paving the pigment, and atomizing a solvent to disperse the pigment on the surface of pigment powder to form the pigment aggregate; softening the pigment aggregates, atomizing the wetting agent to disperse the wetting agent on the outer surface of the pigment powder, and softening the pigment aggregates;

s5, placing the pigment aggregate in a closed container, adding acrylic emulsion, polyester vinyl emulsion and triethanolamine in parts by weight, adjusting the pressure in the container to 3-5MPa, maintaining the pressure for 1-2h, then reducing the pressure to normal pressure, removing the upper suspension, transferring to a high-speed dispersion machine, adding a film forming agent, adjusting the rotation speed to 600-800rpm, and performing shear dispersion until the particle size is sub-nanometer;

and S6, defoaming, namely adding a defoaming agent into the pigment aggregate subjected to high-speed shearing and dispersion, defoaming and filtering by using a defoaming screen with the sub-nanometer diameter and a filter screen, and repeating the steps for 3-5 times to prepare the ink composition.

Preferably, the preparation and softening steps of the pigment aggregate are as follows:

(1) atomizing a solvent and a wetting agent by using an atomizer, and controlling the atomizing flow rate to be 0.2-0.5m/s so that the particle diameter of the atomized liquid is less than 0.1 mu m;

(2) spreading the dried dispersed pigment, keeping the dispersibility of the pigment, and uniformly dispersing a solvent on the surface of the pigment powder in a mist form instead of air to form an aggregate of the pigment;

(3) meanwhile, the wetting agent is dispersed on the surface of the pigment powder in a mist form to soften the aggregates of the pigment, facilitating uniform dispersion of the pigment particles.

Preferably, the wet ball mill comprises a barrel, a base and a driving component, the driving component is connected to one side of the upper end of the base through a bolt, the other side of the upper end of the base is connected with a supporting seat through a bolt, the upper end of the supporting seat is connected with a bearing seat through a bolt, the end part of the barrel is clamped in the middle of the bearing seat, the main gear is connected to the main shaft end of the driving component through a coupling, the side wall of the end part of the barrel is connected with a gear ring through a bolt, the main gear is meshed with the gear ring, the driving component installed at the upper end of the base is used for driving the barrel to rotate through the gear ring installed by matching the main gear with the side wall of the barrel, the power supply of the driving component is switched on, the driving component can, the height of the supporting seat is adjusted, so that the supporting seat can be suitable for installation of cylinders with different specifications;

the inner plate is connected with the inside of the barrel through bolts, through holes are formed in the inner plate at equal intervals, a feeding pipe is welded at one end of the barrel, a feeder is inserted into the feeding pipe, the inner plate with the through holes is arranged in the barrel and used for being matched with grinding and crushing work, meanwhile, the feeder is arranged at the position of the feeding pipe at the end part of the barrel and used for assisting the feeding of the barrel and maintaining the stability of the feeding, and the crushed materials are discharged from a discharging pipe at the other end of the barrel;

the ball mill is characterized in that a support is connected to the middle of the base through a bolt, a support table is connected to the top of the support through a bolt, a slide rail is connected to the middle of the upper end of the support table through a bolt, a slide block is connected to the middle of the slide rail in a sliding manner, a pipe clamp is connected to the middle of the slide block through a bolt, a liquid supply pipeline is clamped in the middle of the pipe clamp, a fixing plate is welded to the side wall of the end of the liquid supply pipeline, a branch pipe is welded to the side wall of the fixing plate, one end of the branch pipe is communicated with the liquid supply pipeline through a pipeline, a sleeve is sleeved on the side wall of the end of the branch pipe, a drain hole is formed in the side wall of the sleeve pipe, a tension spring is connected to the middle of the inner side wall of the, the spray cleaning device comprises a barrel, a liquid supply pipeline, a slide block assembly, a slide rail, a fixing plate, a branch pipe assembly, a branch pipe, a sleeve pipe, a drain hole and a liquid spraying device.

Preferably, bolted connection is passed through at the supporting seat upper end lateral wall in the feeder bottom, the feeder is the screw feeder, just the welding of feeder feed inlet has the hopper, the hopper lateral wall is the trapezium structure, and the feeder adopts the screw feeder, can stably carry out the feed to the barrel inside from the port of inlet pipe, maintains the stable work of barrel inside subassembly.

Preferably, a valve is connected to one end of the support table through a bolt, the valve is communicated with the liquid supply pipeline through a pipeline, and the valve is mounted on the side wall of the support table and is in butt joint with the liquid supply pipeline, so that liquid inlet of the liquid supply pipeline can be conveniently adjusted, and the state of liquid conveying of the liquid supply pipeline can be adjusted in time.

Preferably, the lateral wall of the upper end of the supporting table is connected with a screw rod through a bearing, the middle of the screw rod is in threaded connection with a ball nut, the lateral wall of the ball nut is connected with a sliding block through a bolt, a screw rod assembly with the ball nut is installed on the supporting table, the screw rod is driven to rotate, the ball nut can be driven to translate along the surface of the supporting table, the ball nut drives the sliding block assembly to move, and the position of the sliding block assembly is adjusted.

Preferably, the supporting table lateral wall has a first motor through bolted connection, first motor spindle end passes through coupling joint and is connected with the lead screw, the supporting table lateral wall has the two direction switch that is located first motor one side through bolted connection, two direction switch pass through wire and first motor electric connection, and the first motor that has the lead screw subassembly is installed to the supporting table upper end, and through the power of two direction switch-on first motor, first motor can drive the lead screw and rotate, under the drive of lead screw, can drive ball nut translation for ball nut drives the slider and removes along the slide rail, will install and send into inside the barrel at the confession liquid pipeline subassembly of slider top from the manhole of barrel lateral wall, wash the barrel and maintain.

Preferably, drive assembly comprises second motor, speed reducer and speed governing switch, second motor, speed reducer and speed governing switch are respectively through bolted connection at base upper end lateral wall, the speed reducer output shaft passes through the shaft coupling and is connected with the master gear, second motor main shaft end passes through shaft coupling and speed reducer input shaft, the speed governing switch passes through wire and second motor electric connection, and the drive assembly who comprises second motor, speed reducer and speed governing switch is used for driving the barrel and rotates, switches on the power of second motor through the speed governing switch, and the second motor passes through speed reducer drive master gear and rotates, can drive the ring gear rotation when the master gear moves, and the barrel that the ring gear drive was installed on the bearing frame rotates, constantly with comminuted.

Preferably, the sleeve pipe tip is pegged graft and is had the center tube, the wash port with the specification is seted up to the center tube lateral wall, branch pipe tip inside wall bonds with the bushing junction and has sealing rubber pad, the sleeve pipe inside wall bonds and has sealing rubber pad with the specification, and the center tube is used for further extending the length of sleeve pipe and branch pipe, conveniently sprays cleaning work to ball mill inside, simultaneously at the inboard sealing rubber pad of installing of sleeve pipe and branch pipe, can avoid branch pipe and center tube and sheathed tube junction weeping, guarantees the carrying capacity of water pipe.

Preferably, there is the blend stop through bolted connection center tube tip lateral wall, sleeve pipe tip lateral wall set up with blend stop assorted dodge the groove, the sleeve pipe tip outside even has the blend stop with the specification through the bolt, just branch pipe tip lateral wall sets up with the specification dodge the groove, at center tube tip installation blend stop, increase at the sleeve pipe tip simultaneously and dodge the groove with blend stop matched with for the center tube can dodge under the spacing in groove at the sleeve pipe tip, and can be under the pulling force effect of extension spring, to the inside shrink of sleeve pipe, until the joint is at the sleeve pipe tip, avoid the center tube shrink to go into inside the cover pipe, guarantee center tube and bushing's stability.

Preferably, the outer pipe sleeve is sleeved at the end part of the branch pipe, the outer pipe sleeve is sleeved outside the sleeve pipe, a handle bolt is connected to the side wall of the outer pipe sleeve in a threaded mode, the end part of the handle bolt penetrates through the side wall of the outer pipe sleeve to be in contact with the branch pipe, the outer pipe sleeve is additionally arranged on the side wall of the branch pipe and used for shielding the end part of the branch pipe, parts such as the sleeve pipe and the like arranged at the end part of the branch pipe are protected, meanwhile, the handle bolt is installed on the side wall of the outer pipe sleeve, the handle bolt is screwed down, the.

(III) advantageous effects

Compared with the prior art, the invention provides the neutral ink composition which has extremely high stability and durability, is smooth to write, safe and environment-friendly and can be easily erased and the preparation method thereof, and the neutral ink composition has the following beneficial effects:

1. the neutral erasable ink has the characteristics of fluent and clean writing, good stability, high durability and the like, can keep the property of the ink unchanged for a long time, is beneficial to storage, has good writing effect, has no obvious trace on the back of writing paper, and can easily erase handwriting by using a common eraser.

2. The neutral erasable ink prepared by taking the alcohol-soluble dye as a color base material, adding the hydroxymethyl cellulose, the acrylic resin modified casein film forming agent, the acrylic resin polyurethane copolymer resin, the acrylic ester modified butadiene resin and the like as auxiliary materials and taking the low-toxicity and harmless compounds as raw materials is low in toxicity, safe, free of stimulation, green, environment-friendly and wide in application range.

3. The invention prepares the sub-nanometer-scale color-based pigment by the ball milling process, so that the alcohol-soluble dye is fully mixed with other auxiliary materials; the simultaneous use of the forms of the atomizing solvent and humectant to prepare and soften the pigment aggregates provides the finished ink with extremely high stability and durability.

4. In the writing process of the neutral erasable ink, the ink can form a layer of pigment film on paper through the pen point, so that handwriting can be easily erased within a certain time, no trace is left, and the paper surface is not damaged; meanwhile, after the handwriting is kept for a corresponding time, the handwriting does not blur when meeting water and does not fade after being dried for a long time, and the handwriting becomes permanent handwriting which can not be wiped off and can be kept for a long time.

5. In the ball milling step, a screw feeder inserted in a feeding pipe of a wet ball mill assists in feeding the cylinder body, so that the feeding stability is maintained; the barrel is driven to rotate by control driving, and ball milling and crushing work is carried out in a matching way, so that the grinding efficiency is improved, and the full grinding is ensured; discharging the ball-milled materials from a discharge pipe at the other end of the cylinder body, and keeping the ball-milled materials clean.

Drawings

FIG. 1 is a flow chart of the preparation of a neutral erasable ink composition of the present invention;

FIG. 2 is a schematic structural diagram of a wet ball mill according to the present invention;

FIG. 3 is a schematic side view of a ball mill of the present invention;

FIG. 4 is a schematic top view of a ball mill according to the present invention;

FIG. 5 is a schematic structural diagram of a branch pipe assembly of a wet ball mill according to the present invention;

FIG. 6 is a schematic front view of a branch tube assembly of a wet ball mill according to the present invention;

FIG. 7 is a schematic view showing the structure of a branch pipe assembly of a wet ball mill according to the present invention in an extended state;

FIG. 8 is a schematic view showing the structure of the internal components of the branch pipe of a wet ball mill according to the present invention;

fig. 9 is a schematic structural view of an inner assembly of a wet ball mill cylinder according to the present invention.

In the figure: 1. a barrel; 2. a base; 3. a drive assembly; 4. a supporting seat; 5. a bearing seat; 6. a main gear; 7. a ring gear; 8. an inner plate; 9. a through hole; 10. a feed pipe; 11. a feeder; 12. a support; 13. a support table; 14. a slide rail; 15. a slider; 16. a pipe clamp; 17. a liquid supply conduit; 18. a fixing plate; 19. a branch pipe; 20. a sleeve; 21. a drain hole; 22. a tension spring; 23. a hopper; 24. a valve; 25. a screw rod; 26. a ball nut; 27. a first motor; 28. a second motor; 29. a speed reducer; 30. a speed regulating switch; 31. a reversing switch; 32. a central tube; 33. sealing the rubber pad; 34. blocking strips; 35. an avoidance groove; 36. an outer pipe sleeve; 37. a handle bolt.

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, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.

Example 1:

s1, preprocessing alcohol-soluble dye, weighing alcohol-soluble aniline black with the weight part ratio of 3%, placing the alcohol-soluble aniline black in a wet ball mill, grinding for 10min, and then sieving by a 100-mesh sieve;

s2, preparing a mixed solution, weighing a stabilizer and a dispersant in parts by weight, 0.5% of sodium alginate and 10% of sodium methylene dinaphthalene sulfonate, mixing, placing in a wet ball mill, grinding for 10min, then adding 0.5% of polyacrylic acid, 0.5% of polyacrylamide and 0.5% of octylphenol inwards again, adjusting the stirring speed to 400rpm, and stirring for 10min to enable the viscosity of the mixed solution to be 0.01-0.05 cP;

s3, centrifuging and washing the mixed solution, adjusting the pH value of the mixed solution to be within the range of 7.0-7.5 by using an ammonium acetate buffer solution, standing for 1-2h at room temperature, placing the mixed solution in a centrifuge for centrifugation, adjusting the centrifugation speed to 3000rpm, centrifuging for 10min, repeatedly centrifuging for three times, collecting precipitates, and washing and purifying the precipitates for multiple times by using deionized water;

s4, preparing a pigment aggregate, blowing and drying the obtained precipitate by nitrogen, controlling the temperature of the nitrogen flow to be 40-60 ℃ to obtain a dried dispersed pigment, flatly paving the pigment, and atomizing an ethanol solvent to disperse the solvent on the surface of the pigment powder to form the pigment aggregate; softening the pigment aggregates, atomizing the glycerol wetting agent to disperse on the outer surface of the pigment powder, and softening the pigment aggregates;

s5, placing the pigment aggregate in a closed container, adding acrylic emulsion, polyester vinyl emulsion and triethanolamine in parts by weight, adjusting the pressure in the container to be 3MPa, maintaining the pressure for 1h, then reducing the pressure to normal pressure, removing the upper suspension, transferring to a high-speed dispersion machine, adding a film forming agent, adjusting the rotating speed to be 600rpm, and carrying out shear dispersion until the particle size is sub-nanometer;

and S6, defoaming, namely adding fumed silica into the pigment aggregate subjected to high-speed shearing dispersion to serve as a defoaming agent, defoaming and filtering by using a defoaming screen with a sub-nanometer-scale screen diameter and a filter screen, and repeating the steps for 3 times to prepare the ink composition.

The preparation and softening steps of the pigment aggregate are specifically as follows:

Example 2:

s1, preprocessing alcohol-soluble dye, weighing 5% alcohol-soluble aniline black in parts by weight, placing the alcohol-soluble aniline black in a wet ball mill, grinding for 15min, and then sieving by a 100-mesh sieve;

s2, preparing a mixed solution, weighing a stabilizer and a dispersant in parts by weight, 0.8% of sodium alginate and 12% of sodium methylene dinaphthalene sulfonate in proportion, mixing, placing in a wet ball mill, grinding for 15min, then adding 0.75% of polyacrylic acid, 0.75% of polyacrylamide and 0.75% of octylphenol inwards again, adjusting the stirring speed to 500rpm, and stirring for 15min to enable the viscosity of the mixed solution to be 0.01-0.05 cP;

s3, centrifuging and washing the mixed solution, adjusting the pH value of the mixed solution to be within the range of 7.0-7.5 by using an ammonium acetate buffer solution, standing for 1-2h at room temperature, placing the mixed solution in a centrifuge for centrifugation, adjusting the centrifugation speed to be 4000rpm, centrifuging for 12min, repeatedly centrifuging for three times, collecting precipitates, and washing and purifying the precipitates for multiple times by using deionized water;

s5, placing the pigment aggregate in a closed container, adding acrylic emulsion, polyester vinyl emulsion and triethanolamine in parts by weight, adjusting the pressure in the container to be 3-5MPa, maintaining the pressure for 1-2h, then reducing the pressure to normal pressure, removing the upper suspension, transferring to a high-speed dispersion machine, adding a film forming agent, adjusting the rotating speed to be 700rpm, and carrying out shear dispersion until the particle size is sub-nanometer;

and S6, defoaming, namely adding a defoaming agent into the pigment aggregate subjected to high-speed shearing and dispersion, defoaming and filtering by using a defoaming screen with the sub-nanometer diameter and a filter screen, and repeating the steps for 3 times to prepare the ink composition.

Example 3:

s1, preprocessing alcohol-soluble dye, weighing alcohol-soluble aniline black with the weight part ratio of 7%, placing the alcohol-soluble aniline black in a wet ball mill, grinding for 20min, and then sieving with a 100-mesh sieve;

s2, preparing a mixed solution, weighing 1.0% of a stabilizer and a dispersant in parts by weight, mixing 1.0% of sodium alginate and 15% of sodium methylene dinaphthalene sulfonate, placing the mixture in a wet ball mill, grinding for 20min, then adding 1.0% of polyacrylic acid, 1.0% of polyacrylamide and 1.0% of octylphenol inwards again, adjusting the stirring speed to 600rpm, and stirring for 20min to enable the viscosity of the mixed solution to be 0.01-0.05 cP;

s3, centrifuging and washing the mixed solution, adjusting the pH value of the mixed solution to be within the range of 7.0-7.5 by using an ammonium acetate buffer solution, standing for 1-2h at room temperature, placing the mixed solution in a centrifuge for centrifugation, adjusting the centrifugation speed to be 5000rpm, centrifuging for 15min, repeatedly centrifuging for three times, collecting precipitates, and washing and purifying the precipitates for multiple times by using deionized water;

s5, placing the pigment aggregate in a closed container, adding acrylic emulsion, polyester vinyl emulsion and triethanolamine in parts by weight, adjusting the pressure in the container to be 3-5MPa, maintaining the pressure for 1-2h, then reducing the pressure to normal pressure, removing the upper suspension, transferring to a high-speed dispersion machine, adding a film forming agent, adjusting the rotating speed to be 800rpm, and carrying out shear dispersion until the particle size is sub-nanometer;

Examples of the experiments

First, testing basic properties of ink

Test methods and results

Test samples: examples 1 to 3.

The neutral erasable inks of example 1, example 2 and example 3 were analyzed and tested, and the relative density, surface tension, pH, viscosity, initial drying, tinting strength, surface diffusion, light resistance, light fastness, temperature resistance, etc. of the inks were mainly tested.

The results are shown in Table 1.

TABLE 1

And (4) conclusion: the neutral erasable ink has strong universality, good writing effect, corresponding pseudoshrinkage and viscosity denaturation, high intermittence performance of the ink, long uncapping time, good stability and enough writing length.

Secondly, testing the erasable performance of the ink

Test methods and results

Test samples: examples 1 to 3, control groups 1 to 2.

The neutral erasable ink of example 1, example 2 and example 3 was taken and sealed to prepare neutral pen refills, and two different types of erasable neutral pens were purchased from the market, and the erasability of the writing at different times was examined.

The results are shown in Table 2.

TABLE 2

Time of measurement

6 hours

12 hours

18 hours

24 hours

36 hours

48 hours

Example 1

Easy to erase

Difficult to erase

Non-erasable

Example 2

Easy to erase

Difficult to erase

Non-erasable

Example 3

Easy to erase

Difficult to erase

Non-erasable

Control group

1

Easy to erase

Difficult to erase

Non-erasable

Control group

2

Difficult to erase

Non-erasable

And (4) conclusion: the writing handwriting of the neutral erasable ink can be easily erased by using a common eraser within 18 hours, and the time is longer than that of a contrast group on the market.

Example 4:

the technical scheme solves the problem that the common neutral ink handwriting can not be easily erased by using a common eraser, but in the process production, the problems of poor quality of finished products exist due to low efficiency, insufficient grinding and non-uniform particle size of the ball mill. As shown in fig. 2-9, in the wet ball mill used in the ball milling step, the screw feeder inserted into the feeding pipe assists the feeding of the barrel, the barrel is driven to rotate by the control drive to perform the grinding and crushing work, and the ground material is discharged from the discharging pipe at the other end of the barrel. The wet ball mill comprises a barrel 1, a base 2 and a driving component 3, wherein the driving component 3 is connected to one side of the upper end of the base 2 through a bolt, the other side of the upper end of the base 2 is connected with a supporting seat 4 through a bolt, the upper end of the supporting seat 4 is connected with a bearing seat 5 through a bolt, the end part of the barrel 1 is clamped in the middle of the bearing seat 5, the main shaft end of the driving component 3 is connected with a main gear 6 through a coupling, the side wall of the end part of the barrel 1 is connected with a gear ring 7 through a bolt, the main gear 6 is meshed with the gear ring 7, the driving component 3 arranged at the upper end of the base 2 is used for driving the barrel 1 to rotate through the main gear 6 matched with the gear ring 7 arranged on the side wall of the barrel 1, the power supply of the driving component 3 is switched on, the driving component 3 can drive, the height of the supporting seat 4 is adjusted, so that the installation of the cylinder bodies 1 with different specifications can be adapted.

Further, 1 inside bolted connection has the inner panel 8 through the barrel, through-hole 9 has been seted up to 8 inside equidistant intervals of inner panel, 1 one end welding of barrel has inlet pipe 10, the inside grafting of inlet pipe 10 has feeder 11, 1 internally mounted's of barrel has the inner panel 8 of through-hole 9, a crushing work of polishing is used for the cooperation, simultaneously at the inlet pipe 10 position installation feeder 11 of 1 tip of barrel, a material for assisting 1 feeding of barrel, maintain the stability of feeding, the discharging pipe of the material of accomplishing from the 1 other end of barrel of smashing is discharged.

Further, the middle position of the base 2 is connected with a support 12 through a bolt, the top of the support 12 is connected with a support table 13 through a bolt, the middle position of the upper end of the support table 13 is connected with a slide rail 14 through a bolt, the middle of the slide rail 14 is connected with a slide block 15 in a sliding manner, the middle of the slide block 15 is connected with a pipe clamp 16 through a bolt, the middle of the pipe clamp 16 is connected with a liquid supply pipeline 17 in a clamping manner, the side wall of the end part of the liquid supply pipeline 17 is welded with a fixing plate 18, the side wall of the fixing plate 18 is welded with a branch pipe 19, one end of the branch pipe 19 is communicated with the liquid supply pipeline 17 through a pipeline, the side wall of the end part of the branch pipe 19 is sleeved with a sleeve pipe 20, the middle position of the inner side of the sleeve pipe 20 is connected, the cleaning device comprises a barrel body 1, a liquid supply pipeline 17, a slide block 15, a slide rail 14, a slide block 15, a support pipe 17, a branch pipe 19, a sleeve pipe 20 and a water discharge hole 21, wherein the liquid supply pipeline 17 extends into the barrel body 1 from an access hole in the side wall of the barrel body 1, the spray cleaning work is carried out on the interior of the barrel body 1, the liquid supply pipeline 17 is installed on a slide block 15 assembly through a pipe clamp 16, the slide block 15 is moved along the slide rail 14, the liquid supply pipeline 17 assembly can be moved and conveyed into the barrel body 1, cleaning liquid is conveyed to the liquid supply pipeline 17, the branch pipe 19 assembly is installed at the end part of the liquid supply pipeline 17 through.

Further, feeder 11 bottom is through bolted connection in supporting seat 4 upper end lateral wall, and feeder 11 is the screw feeder, and the welding of feeder 11 feed inlet has hopper 23, and hopper 23 lateral wall is the trapezium structure, and feeder 11 adopts the screw feeder, can stably follow the port of inlet pipe 10 and supply the inside barrel 1, maintains the stable work of barrel 1 internal component.

Furthermore, one end of the support table 13 is connected with a valve 24 through a bolt, the valve 24 is communicated with the liquid supply pipeline 17 through a pipeline, and the valve 24 is mounted on the side wall of the support table 13 and is in butt joint with the liquid supply pipeline 17, so that liquid feeding of the liquid supply pipeline 17 can be conveniently adjusted, and the state of liquid conveying of the liquid supply pipeline 17 can be adjusted in time.

Further, the side wall of the upper end of the support platform 13 is connected with a screw 25 through a bearing, the middle of the screw 25 is in threaded connection with a ball nut 26, the side wall of the ball nut 26 is connected with the slide block 15 through a bolt, the side wall of the support platform 13 is connected with a first motor 27 through a bolt, the main shaft end of the first motor 27 is connected with the screw 25 through a coupling joint, the side wall of the support platform 13 is connected with a forward and backward switch 31 positioned on one side of the first motor 27 through a bolt, the forward and backward switch 31 is electrically connected with the first motor 27 through a lead wire, the first motor 27 with a screw 25 component is installed on the upper end of the support platform 13, the power supply of the first motor 27 is switched on through the forward and backward switch 31, the first motor 27 can drive the screw 25 to rotate, the ball nut 26 can be driven to translate under the drive of the screw 25, so that the ball nut 26 drives the slide block 15 to move, and cleaning and maintaining the cylinder 1.

Further, the driving assembly 3 is composed of a second motor 28, a speed reducer 29 and a speed regulation switch 30, the second motor 28, the speed reducer 29 and the speed regulation switch 30 are respectively connected to the side wall of the upper end of the base 2 through bolts, an output shaft of the speed reducer 29 is connected with the main gear 6 through a coupler, a main shaft end of the second motor 28 is connected with an input shaft of the speed reducer 29 through a coupler, the speed regulation switch 30 is electrically connected with the second motor 28 through a wire, the driving assembly 3 composed of the second motor 28, the speed reducer 29 and the speed regulation switch 30 is used for driving the barrel 1 to rotate, a power supply of the second motor 28 is connected through the speed regulation switch 30, the second motor 28 drives the main gear 6 to rotate through the speed reducer 29, the main gear 6 drives the gear ring 7 to rotate when in operation, and the gear ring 7 drives the barrel.

Furthermore, a central tube 32 is inserted into the end of the sleeve 20, a drain hole 21 with the same specification is formed in the side wall of the central tube 32, a sealing rubber pad 33 is bonded at the joint of the inner side wall of the end of the branch tube 19 and the sleeve 20, a sealing rubber pad 33 with the same specification is bonded on the inner side wall of the sleeve 20, a barrier strip 34 is connected on the side wall of the end of the central tube 32 through a bolt, an avoiding groove 35 matched with the barrier strip 34 is formed in the side wall of the end of the sleeve 20, a avoiding groove 35 with the same specification is formed in the side wall of the end of the branch tube 19, the central tube 32 with the drain hole 21 with the same specification is installed at the end of the sleeve 20, the central tube 32 is used for further extending the lengths of the sleeve 20 and the branch tube 19, so as to facilitate the spray cleaning work inside the ball mill, and meanwhile, the sealing rubber pads 33 are installed at, guarantee the transport capacity of water pipe, at central tube 32 tip installation blend stop 34 simultaneously, increase at sleeve pipe 20 tip simultaneously and dodge groove 35 with blend stop 34 matched with for central tube 32 can dodge under the spacing of groove 35 at sleeve pipe 20 tip, and can be under the pulling force effect of extension spring 22, to the inside shrink of sleeve pipe 20, until the joint at sleeve pipe 20 tip, avoid the central tube 32 shrink to go into inside sleeve pipe 20, guarantee the stability that central tube 32 and sleeve pipe 20 are connected.

Furthermore, an outer sleeve 36 is sleeved at the end part of the branch pipe 19, the outer sleeve 36 is sleeved outside the sleeve 20, a handle bolt 37 is in threaded connection with the side wall of the outer sleeve 36, the end part of the handle bolt 37 penetrates through the side wall of the outer sleeve 36 to be in contact with the branch pipe 19, the outer sleeve 36 is additionally arranged on the side wall of the branch pipe 19, the outer sleeve 36 is used for shielding the end part of the branch pipe 19, the components such as the sleeve 20 and the like mounted at the end part of the branch pipe 19 are protected, meanwhile, the handle bolt 37 is mounted on the side wall of the outer sleeve 36, the handle bolt 37 is screwed, the outer sleeve 36 can be fixed outside.

When the wet ball mill is used, the driving assembly arranged at the upper end of the base of the wet ball mill is used for driving the cylinder to rotate by matching the main gear with the gear ring arranged on the side wall of the cylinder, the power supply of the driving assembly is switched on, the driving assembly can drive the main gear to rotate, the main gear can further drive the gear ring to drive the cylinder arranged on the bearing seat to rotate, the grinding work is carried out in a matching way, the bearing seat is connected with the base through the supporting seat, the height of the supporting seat is adjusted, and the wet ball mill can adapt; the inner plate with the through hole is arranged inside the barrel and used for being matched with grinding and smashing work, the feeder is arranged at the position of the feeding pipe at the end part of the barrel and used for assisting the feeding of the barrel, the feeding stability is maintained, and the smashed material is discharged from the discharging pipe at the other end of the barrel. When the device is used, a support table assembly is installed at the upper end of a support in the middle of a base of a wet ball mill, a liquid supply pipeline installed on a support table is used for stretching into the barrel from an access hole in the side wall of the barrel when the ball mill stops working, spraying and cleaning work is carried out on the interior of the barrel, the liquid supply pipeline is installed on a sliding block assembly through a pipe clamp, a sliding block is moved along a sliding rail, the liquid supply pipeline assembly can be moved and sent into the interior of the barrel, cleaning liquid is conveyed to the liquid supply pipeline, a branch pipe assembly is installed at the end part of the liquid supply pipeline through a fixing plate, when the cleaning liquid enters the interior of a branch pipe from the liquid supply pipeline, the pressure in the branch pipe is increased, the stress of a.

When the wet ball mill supporting table is used, the first motor with the screw rod assembly is installed at the upper end of the wet ball mill supporting table, the power supply of the first motor is switched on through the reversing switch, the first motor can drive the screw rod to rotate, the ball nut can be driven to translate under the driving of the screw rod, the ball nut drives the sliding block to move along the sliding rail, the liquid supply pipeline assembly installed above the sliding block is sent into the barrel from the access hole in the side wall of the barrel, and the barrel is cleaned and maintained.

When using, through the center tube that has the wash port with specification at wet-type ball mill sleeve pipe tip installation, the center tube is used for further extending the length of sleeve pipe and branch pipe, the washing work is sprayed to the ball mill inside to the convenience, simultaneously at cover inboard and branch pipe inboard installation sealing rubber pad, can avoid branch pipe and center tube and sheathed tube junction weeping, guarantee the conveying capacity of water pipe, simultaneously at center tube tip installation blend stop, increase at the sleeve pipe tip simultaneously and dodge the groove with blend stop matched with, make the center tube can dodge under the spacing of groove at the sleeve pipe tip, and can be under the tensile force effect of extension spring, to the inside shrink of sleeve pipe, until the joint at the sleeve pipe tip, avoid the center tube shrink to go into inside the sleeve pipe, guarantee center tube and bushing's stability.

When the ball mill is used, the outer pipe sleeve is additionally arranged on the side wall of the branch pipe of the wet ball mill and used for shielding the end part of the branch pipe, parts such as the sleeve pipe and the like at the end part of the branch pipe are protected and installed, the handle bolt is installed on the side wall of the outer pipe sleeve, the handle bolt is screwed up, the outer pipe sleeve can be fixed on the outer side of the branch pipe, and the stability of the position of an outer pipe sleeve assembly is maintained.

Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that 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

1. The neutral erasable ink composition is characterized by comprising the following raw materials in percentage by mass:

2-10% of alcohol-soluble dye;

25-35% of film-forming agent;

0.5-1% of lubricant;

0.5-1% of surfactant;

0.5 to 1 percent of stabilizer;

1-2% of a thickening agent;

10-15% of a dispersant;

30-45% of a solvent;

3-5% of a wetting agent;

0.5 to 1 percent of flatting agent;

0.05 to 0.5 percent of defoaming agent;

the stabilizer is one or more of sodium alginate and ethanolamine;

2. A method of making a neutral erasable ink composition, comprising the steps of:

s1, preprocessing alcohol-soluble dye, placing different color-based pigments in a wet ball mill for ball milling, and sieving;

s2, preparing a mixed solution, mixing the stabilizer and the dispersant in parts by weight in a wet ball mill according to a proportion, grinding and sieving the mixture, then adding the thickener and the flatting agent in parts by weight again, adjusting the stirring speed and keeping the mixture for a certain time to prepare the mixed solution;

s3, centrifuging and washing the mixed solution, adjusting the pH value of the mixed solution by using an ammonium acetate buffer solution, stirring, standing for a certain time, placing the mixture in a centrifuge for centrifugal treatment, collecting precipitates, and washing and purifying for multiple times;

s4, preparing a pigment aggregate, blowing and drying the obtained precipitate by nitrogen to obtain a dry dispersed pigment, flatly paving the pigment, and atomizing a solvent to disperse the pigment on the surface of pigment powder to form the pigment aggregate; softening the pigment aggregates, atomizing the wetting agent to disperse the wetting agent on the outer surface of the pigment powder, and softening the pigment aggregates;

s5, placing the pigment aggregate in a closed container, adding acrylic emulsion and polyester ethylene emulsion in parts by mass, adjusting the pressure in the container, keeping the pressure for a certain time, reducing the pressure to normal pressure, removing the upper suspension, transferring the suspension to a high-speed dispersion machine, adding a film-forming agent, and shearing and dispersing until the particle size is sub-nanometer;

and S6, defoaming, namely adding a defoaming agent into the pigment aggregate after high-speed shearing and dispersing, defoaming by using a defoaming screen, filtering, and repeating the steps for multiple times to prepare the ink composition.

3. The method of preparing a neutral erasable ink composition of claim 2, wherein the steps of preparing and softening the pigment aggregates are as follows:

4. The method of claim 3, wherein the step of ball milling further comprises: the spiral feeder through inside grafting of wet ball mill inlet pipe assists the barrel feeding, maintains the stability of feeding, opens drive assembly, drives the barrel and rotates, grinds crushing work, and the material that the ball-milling was accomplished is discharged from the discharging pipe of the barrel other end.

5. The method of claim 4, wherein the ball milling step is performed by:

(1) the method comprises the following steps of (1) guiding, namely connecting a wet ball mill with a power supply, placing color-based pigments of different alcohol-soluble dyes in a cylinder body in the ball mill through a feeding pipe, maintaining the stability of feeding, and sequentially introducing a thickening agent, a flatting agent, a stabilizing agent and a dispersing agent after grinding;

(2) grinding, namely switching on a power supply of the driving assembly to enable the cylinder to rotate, and grinding and crushing the inner plate with the through hole in cooperation with the inner plate with the through hole arranged in the cylinder to prepare a mixed solution;

(3) discharging, namely discharging the completely ground and crushed materials through a discharge pipe connected to the other end of the barrel;

(4) and (4) cleaning, namely extending the liquid supply pipeline into the cylinder from the access hole on the side wall of the cylinder to perform spraying and cleaning work.

6. The method of claim 5, wherein the grinding step is performed by:

the bearing seat (5) is connected with the base (2) through the supporting seat (4), the height of the supporting seat (4) is adjusted, and the installation of the cylinders (1) with different specifications can be adapted;

drive assembly (3) of installation in base (2) upper end are used for driving barrel (1) to rotate through ring gear (7) of master gear (6) cooperation barrel (1) lateral wall installation, the power of switch-on drive assembly (3), drive assembly (3) can drive master gear (6) and rotate, master gear 6 and then can drive ring gear (7) and drive barrel (1) of installing on bearing frame (5) and rotate, the cooperation is smashed the work, barrel (1) internally mounted has inner panel (8) of through-hole (9), be used for the cooperation to grind crushing work.

7. The method of claim 6, wherein the washing step is performed by:

a support table (13) assembly is arranged at the upper end of a support (12) in the middle of a base (2), a liquid supply pipeline (17) arranged on the support table (13) extends into the cylinder (1) from an access hole in the side wall of the cylinder (1), the liquid supply pipeline (17) is arranged on a sliding block (15) assembly through a pipe clamp (16), the sliding block (15) is moved along a sliding rail (14), and the liquid supply pipeline (17) assembly can be moved and sent into the cylinder (1);

when the ball mill is stopped, cleaning liquid is conveyed to the liquid supply pipeline (17), a branch pipe (19) assembly is installed at the end part of the liquid supply pipeline (17) through a fixing plate (18), when the cleaning liquid enters the branch pipe (19) from the liquid supply pipeline (17), the internal pressure of the branch pipe (19) is increased, the sleeve (20) is stressed and extends out of the end part of the branch pipe (19), a drain hole (21) in the side wall of the sleeve (20) is exposed, and the liquid is sprayed into the barrel (1) from the drain hole (21) to perform spraying and cleaning work.

8. The method for preparing a neutral erasable ink composition according to claim 7, wherein the wet ball mill comprises a cylinder (1), a base (2) and a driving assembly (3), wherein the driving assembly (3) is connected to one side of the upper end of the base (2) through a bolt, the other side of the upper end of the base (2) is connected with a supporting seat (4) through a bolt, the upper end of the supporting seat (4) is connected with a bearing seat (5) through a bolt, the end of the cylinder (1) is clamped in the middle of the bearing seat (5), the main shaft end of the driving assembly (3) is connected with a main gear (6) through a shaft coupling, the side wall of the end of the cylinder (1) is connected with a gear ring (7) through a bolt, and the main gear (6) is meshed with the gear.