CN110229557A - Neutral writing ink and preparation method thereof, application - Google Patents
Neutral writing ink and preparation method thereof, application Download PDFInfo
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- CN110229557A CN110229557A CN201910576906.0A CN201910576906A CN110229557A CN 110229557 A CN110229557 A CN 110229557A CN 201910576906 A CN201910576906 A CN 201910576906A CN 110229557 A CN110229557 A CN 110229557A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/16—Writing inks
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/16—Writing inks
- C09D11/17—Writing inks characterised by colouring agents
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/16—Writing inks
- C09D11/18—Writing inks specially adapted for ball-point writing instruments
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- Inks, Pencil-Leads, Or Crayons (AREA)
Abstract
This application discloses a kind of Neutral writing ink and preparation methods, application.Contain urushiol-based emulsifier in the Neutral writing ink.Neutral writing ink provided herein uses laccol agent emulsifier for pigment anti-settling agent, effectively prevent settling between pigment particles because of reunion, and has excellent high temperature resistant storage stability, freeze-resistant stable storing energy.
Description
Technical field
This application involves a kind of Neutral writing inks and preparation method thereof, application, belong to technical field of fine.
Background technique
It is more comfortable, smooth that gel ink pen writes feel, ink marks convergence is strong, can persistence, be a kind of to like by people
Writing implement.The core technology of Neutral writing ink is mainly monopolized by Japan, Germany, the U.S. and South Korea, and China's high quality is neutral
Ink still largely relies on import.Gel ink pen prepared by the prior art is easily made with Neutral writing ink through thermmal storage or stored frozen
It precipitates and cannot use at pigment.Common Neutral writing ink stability problem is mainly shown as that ink is deposited for a long time in high temperature or low temperature
Occur during putting pigment return slightly with flocculation, and phenomena such as the pigment precipitating eventually led to is thickened with system.Chinese patent CN
105400289A discloses a kind of neutral ink composition, carries out using including hybrid resin and the swollen acrylic emulsion component of alkali soluble
Rationally cooperation, makes pigment be uniformly dispersed, and flocculation of reuniting does not occur, obtained Neutral writing ink stability is good, mildew resistance is good, raises one's hat
Time is long, thixotropy with higher, writes that feel is fluent, svelteness；CN 105385238A discloses one kind with carbon black
The Carbon black gel ink and preparation method of the high stability of raw material.CN 105348916A discloses a kind of polymolecularity high thixotropic
Neutral writing ink and preparation method thereof is used as composite dispersing agent using alcohol ether carboxylate and polyethylene glycol -200, and propylene glycol is hydrotropy
Agent, and using triethanolamine as pH adjusting agent, prepare the good aqueous color paste of dispersion stabilization；Again using aqueous color paste as parent,
Diethylene glycol (DEG) and other organic additives is added, obtains the Neutral writing ink for having both polymolecularity and high thixotropic；CN 101649137B is public
A kind of gel ink with high stability has been opened, has used graphite lotion as colorant, using Tween 80 as surfactant, simultaneously
Joined one kind can prevent calcium, magnesium, the crystallization of iron plasma, the diffusant reunited as stabilizer, so that stability greatly mentions
The high, shelf-life significantly extends, and can substitute similar imported product.
In conclusion storing under high temperature or freezing conditions, pigment precipitating is current Neutral writing ink common problem,
It is also that Neutral writing ink researches and develops one of most formidable bottleneck.
Summary of the invention
According to the one aspect of the application, a kind of Neutral writing ink is provided, it is the resistance to hot storage stability of the Neutral writing ink, cold-resistant
It is splendid to freeze storage stability, is a kind of high stable Neutral writing ink.
A kind of Neutral writing ink contains urushiol-based emulsifier in the Neutral writing ink.
In the application, by adding urushiol-based emulsifier, stability of the ink in hot-cool environment is improved.
Optionally, the granularity of the Neutral writing ink is 65~78nm.
Optionally, weight percentage of the urushiol-based emulsifier in the Neutral writing ink be 0.05~
8.0wt%.
Optionally, the urushiol-based emulsifier is selected from least one of the compound with structural formula shown in formula I；
Wherein, R01Selected from straight chain C15One of alkyl；
R02, R03, R04Independently selected from one of hydrogen, alkyl；
N is integer, value range 4≤n≤50 of n.
Preferably, R02, R03, R04For hydrogen.
Optionally, the alkyl is C1~C4Alkyl.
Preferably, R01Selected from straight chain C15Alkyl, straight chain C15One of alkenyl.
It is further preferred that R in the urushiol-based emulsifier01Selected from formula (a) structural formula group, have formula
(b) group of structural formula shown in, the group with structural formula shown in formula (c), appointing in the group with structural formula shown in formula (d)
It is a kind of:
In a specific example, the urushiol-based emulsifier is in the compound with structural formula shown in formula I -1
At least one；
Wherein, R02, R03, R04For hydrogen；
R01Selected from the group with formula (a) structural formula, the group with structural formula shown in formula (b), there is formula (c) institute
Show any one of the group of structural formula, the group with structural formula shown in formula (d):
The integer that n is 4 to 50.
In the application, urushiol-based emulsifier can be prepared by suitable method in the prior art.Be described below it is a kind of compared with
Good preparation method, the urushiol-based emulsifier are prepared in the following manner:
(1) laccol and epoxy chlorine is added in the four-hole boiling flask equipped with blender, reflux condensing tube, thermometer, dropping funel
Propane is heated to 50~60 DEG C, and 1~2h of NaOH solution is added dropwise dropwise under stiring, after being added dropwise, is warming up to 60~70
DEG C, and isothermal reaction 4h, obtain laccol shrink drier oil ether.Dimethylbenzene and water washing are added into laccol glycidol ether, stands
Layering overnight removes water layer inorganic matter, and until no chloride ion, vacuum distillation obtains laccol glycidol ether for washing repeatedly.
(2) laccol obtained in (1) is added in the three-necked flask equipped with blender, reflux condensing tube, thermometer to shrink
The polyethylene glycol (PEG) of glycerin ether sum, is heated to 90 DEG C, is added dropwise NaOH solution dropwise under stiring, and reaction is to dissolving in
Water obtains laccol based high molecular emulsifier.Its whole preparation process such as following formula:
The laccol is to extract to obtain from natural raw lacquer through dimethylbenzene, acetone or alcohol；The natural raw lacquer is selected from
At least one of safe and comfortable paint, flat interest paint, entrance of the city paint, hair dam paint, Qinling Mountains paint or other raw lacquer.
It optionally, further include dispersible pigment color paste, resin aqueous emulsion, shear shinning agent, surface-active in the Neutral writing ink
Agent, lubricant, wetting agent, moisturizer, preservative, antirust agent, antifreezing agent, pH adjusting agent, solvent.
Optionally, in Neutral writing ink, the content of each component are as follows:
Optionally, in Neutral writing ink, the content of each component are as follows:
Optionally, the dispersible pigment color paste is aqueous carbon black dispersible pigment color paste；
The resin aqueous emulsion is selected from aqueous polyurethane emulsion, water-and acrylate lotion, aqueous alkide resin emulsion
At least one of；
The shear shinning agent is selected from least one of xanthan gum, polyvinyl glue, guar gum；
The surfactant is complexed surfactant, and the complexed surfactant is by anionic surfactant
It is formed with nonionic surface active agent；The anionic surfactant is selected from dodecyl sodium sulfate, dodecyl sulphur
At least one of sour sodium, the nonionic surface active agent is selected from least one in triton x-100, Tween 80
Kind；
Wherein, the ratio of anionic surfactant and nonionic surface active agent is 1:0.2~5；
The lubricant is selected from least one of potassium oleate, enuatrol, potassium stearate, phosphate；
The wetting agent in urea element, sorbitol, Silok-8100, Dick 5840, Bi Ke 154, Bi Ke 191 extremely
Few one kind；
The moisturizer is selected from least one of water-soluble denaturated silicone oil, sucrose, glucose；
The preservative be selected from 2- benzisothiazole-3-ketone and its derivative, imidazole and its derivants, benzimidazole and
At least one of its derivative；
The antirust agent is selected from least one of benzotriazole, tolytriazole；
The antifreezing agent in glycerol, diglycerol, ethylene glycol, diethylene glycol, triethylene glycol, two diethyl acetals at least
It is a kind of；
The pH adjusting agent is selected from least one of monoethanolamine, diethanol amine, triethanolamine；
The solvent is deionized water.
Preferably, resin aqueous emulsion is selected from water-and acrylate lotion, and mass percentage is 20~60wt%.
Preferably, shear shinning agent is xanthan gum.
According to the another aspect of the application, a kind of method for preparing Neutral writing ink described in any of the above embodiments is additionally provided,
Urushiol-based emulsifier is mixed with other components, the Neutral writing ink can be obtained.
Optionally, it at least includes the following steps:
A) mixture I containing shear shinning agent, preservative is obtained；
B) mixing containing urushiol-based emulsifier, anionic surfactant, lubricant, moisturizer, antirust agent is obtained
Object II；
C) antifreezing agent, wetting agent, nonionic surface active agent, resin aqueous emulsion and dispersible pigment color paste are added to step
B) in the mixtures II obtained, mixture III is obtained；
D) mixing IV containing mixture I and mixture III is obtained, pH is adjusted, the Neutral writing ink can be obtained.
Specifically, a) shear shinning agent, preservative are dissolved in 60~90 DEG C of deionized water, are stirred evenly, mixed
Close object I；
B) urushiol-based emulsifier, anionic surfactant, lubricant, moisturizer, antirust agent are dissolved in 60~90 DEG C
Deionized water in, stirring, dissolution completely after, obtain mixture II；
C) antifreezing agent, wetting agent, nonionic surface active agent, resin aqueous emulsion, pigment are added into mixture II
Mill base stirs evenly, and obtains mixture III；
D) it in the mixture III for obtaining the addition of mixture I obtained in step a) step c), stirs evenly, is mixed
Object IV；PH adjusting agent is added and after grinding distribution, obtains the Neutral writing ink of high stable after mixing evenly.
According to the another aspect of the application, a kind of product is additionally provided, the product includes in described in any of the above embodiments
Property ink, any one of the Neutral writing ink being prepared according to method described above.
Preferably, the product is a based article.
In the application, " alkyl " refers to the group formed by losing any one hydrogen atom on hydrocarbon molecules.
In the application, " alkenyl " refers to by losing any one hydrogen on the hydrocarbon molecules containing at least one C=C
The group that atom is formed.
In the application, " alkyl " refers to the group formed by losing any one hydrogen atom on alkane compound molecule.Alkane
Hydrocarbon compound includes cycloalkane, linear paraffin, branched paraffin.
In the application, C15、C1~C4In subscript indicate the group carbon atom number that is included.For example, C15Alkyl indicates carbon
The alkyl that atomicity is 15.
The beneficial effect that the application can generate includes:
1) Neutral writing ink provided herein uses laccol agent emulsifier for pigment anti-settling agent, effectively prevent pigment grain
It is settled between son because of reunion；
2) high stable Neutral writing ink provided herein and its product have excellent high temperature resistant storage stability, cold-resistant
Freeze stable storing energy；
3) Neutral writing ink provided herein, writes that book feel is fluent, svelteness, and the time of raising one's hat is long；
4) preparation method of Neutral writing ink provided herein, raw material sources are wide, cheap and easily-available, and preparation process letter
It is single, it is easy to industrialized production.
Specific embodiment
The application is described in detail below with reference to embodiment, but the application is not limited to these embodiments.
Unless otherwise instructed, the raw material in embodiments herein is bought by commercial sources.
Analysis method is as follows in embodiments herein:
It is tested referring to QB/T 2625-2011 " Neutral writing ink ball pen and pen core ".
Viscosity test: it is tested using U.S. Brookfield R/S plus RHEMETER rotational rheometer；Rotor model:
C50-1；Revolving speed: 12r/min；Temperature: 25 DEG C.
Testing graininess: it is tested using Britain's Malvern ZETA SIZER Nano series Nano-ZS Particle Size Analyzer.
Surface tension test: it is tested using Germany's KRUSS-K100 surface tension instrument, test temperature: room temperature.
Pen core centrifugal sedimentation test: it is tested using Hunan instrument H-2050R centrifugal separator, test condition: 12000r/min,
15 DEG C, 30min.
PH value test: it is tested using PHB-5 pen type pH meter room temperature.
Hot storage stability test: sample is placed in 70 DEG C of baking ovens, is tested after 10.
Stability test is deposited in freezing: sample being placed in -10 DEG C of ice-water baths, is tested after 10 days.
The preparation of Examples 1 to 4 Neutral writing ink
(1) shear shinning agent, preservative are dissolved in 90 DEG C of 50 parts of deionized waters according to the parts by weight of formula metering,
It stirs evenly, obtains mixture I；
(2) according to the parts by weight of formula metering by urushiol-based emulsifier, anionic surfactant, lubricant, moisturizing
Agent, antirust agent are dissolved in 90 DEG C of balance deionized water (50 parts), after stirring, dissolution completely, obtain mixture II；
(3) antifreezing agent, wetting agent, the nonionic surface active agent, aqueous tree of the parts by weight according to formula metering is added
Fat liquor, dispersible pigment color paste, stir evenly, and obtain mixture III；
Wherein, the dispersible pigment color paste is aqueous carbon black dispersible pigment color paste, is purchased from Suzhou Sunmun Technology Co., Ltd.；
The resin aqueous emulsion is the acrylic acid ester emulsion that mass percentage is 50 ± 1wt%, is purchased from Guangzhou Bai Chuan
Chemical Co., Ltd.；
Wetting agent Silok-8100 is purchased from Guangzhou Si Luoke Chemical Co., Ltd；
(4) it in the mixture for obtaining the addition of mixture obtained in step (1) step (2), stirs evenly, is mixed
Object IV；The pH adjusting agent according to the parts by weight for wanting formula metering is added, after mixing evenly, after grinding distribution, obtains gel ink pen use
Neutral writing ink.
The content of specific each component is shown in Table 1.
Wherein, the acquisition pattern of urushiol-based emulsifier are as follows:
The synthesis of laccol glycidol ether: in four mouthfuls of burnings equipped with blender, reflux condensing tube, thermometer, dropping funel
The laccol of 31.4g and the epoxychloropropane of 55.6g is added in bottle, is heated to 56 DEG C, is added dropwise 20ml's dropwise under stiring
The NaOH solution 1.5h of 10mol/L after being added dropwise, is warming up to 67 DEG C, and isothermal reaction 4h, obtains laccol shrink drier oil ether.
After purified, laccol glycidol ether is obtained.
Urushiol-based emulsifier: it is added in the three-necked flask of the 500ml equipped with blender, reflux condensing tube, thermometer
The laccol glycidol ether of 33.5g and the polyethylene glycol (PEG1000) of 118g, are heated to 90 DEG C, drip dropwise under stiring
Add the NaOH solution of the 1mol/L of 2ml, reaction obtains urushiol-based emulsifier to water-soluble.
Comparative example 1
The preparation method is the same as that of Example 1~and 4, the difference is that, do not contain urushiol-based emulsifier.Specific each component contains
Amount is shown in Table 1.
Comparative example 2
In step (2), charging sequence is different, the same Examples 1 to 4 of preparation process.
(1) shear shinning agent, preservative are dissolved in 90 DEG C of deionized waters according to the parts by weight of formula metering, stirring is equal
It is even；
(2) according to the antifreezing agent of the parts by weight of formula metering, wetting agent, nonionic surface active agent, water-base resin cream
Liquid, dispersible pigment color paste, stir evenly；
(3) be added according to formula metering parts by weight by urushiol-based emulsifier, anionic surfactant, lubricant,
Moisturizer, antirust agent are dissolved in the balance deionized water of heat, and stirring, dissolution are complete；
(4) it in the mixture for obtaining the addition of mixture obtained in step (1) step (3), stirs evenly；Be added according to
The pH adjusting agent of the parts by weight of formula metering is wanted, after mixing evenly, after grinding distribution, obtains gel ink pen Neutral writing ink.
The content of specific each component is shown in Table 1
The formula of 1. embodiment of table and comparative example
Wherein, number is parts by weight in table 1.
2 performance test of embodiment
Respectively to the sample and comparative example 1 and the progress performance parameter test of comparative example 2 in embodiment 1 to 4, test result
It is as shown in table 2:
The test of 2. particular product performance parameters of table
As can be seen from Table 2, made sample all has lesser partial size.
Respectively in embodiment 1 to 4 sample and comparative example 1 and comparative example 2 carry out Modified bitumen test, test knot
Fruit is as shown in table 3:
The test of 3. product Modified bitumen of table
As can be seen from Table 3, the Neutral writing ink of urushiol-based emulsifier is added, pigment particle size has good without significant change
Modified bitumen；Charging sequence has larger impact to the Modified bitumen of Neutral writing ink.
Respectively in embodiment 1 to 4 sample and comparative example 1 and comparative example 2 carry out freezing performance test, test result
It is as shown in table 4:
4. product of table freezes performance test
As can be seen from Table 4, the Neutral writing ink of urushiol-based emulsifier is added, pigment particle size has good without significant change
Frozen for storage performance；Charging sequence has larger impact to the frozen for storage performance of Neutral writing ink.
Respectively by the sample and comparative example 1 and the resulting Neutral writing ink of comparative example 2 in embodiment 1 to 4, carry out in filling
Property pen core, carry out room temperature raise one's hat, heat storage, freezing testing writing performance, test result as shown in table 5 and table 6:
5. product testing writing performance of table
6. comparative example product testing writing performance of table
By the filling gel ink pen of the Neutral writing ink containing urushiol-based emulsifier with good normal it can be seen from table 5 and table 6
Temperature is raised one's hat, heat is stored up, freezes writing quality；Charging sequence has larger impact to Neutral ball-point for ball-point pen writing quality.
By above-mentioned data it is found that addition laccol base emulsified base and charging sequence can influence the stability of product.
The above is only several embodiments of the application, not does any type of limitation to the application, although this Shen
Please disclosed as above with preferred embodiment, however not to limit the application, any person skilled in the art is not taking off
In the range of technical scheme, a little variation or modification are made using the technology contents of the disclosure above and is equal to
Case study on implementation is imitated, is belonged in technical proposal scope.
Claims (10)
1. a kind of Neutral writing ink, which is characterized in that contain urushiol-based emulsifier in the Neutral writing ink.
2. Neutral writing ink according to claim 1, which is characterized in that the urushiol-based emulsifier is in the Neutral writing ink
Weight percentage be 0.05~8.0wt%.
3. Neutral writing ink according to claim 1, the urushiol-based emulsifier is selected from the chemical combination with structural formula shown in formula I
At least one of object；
Wherein, R01Selected from straight chain C15One of alkyl；
R02, R03, R04Independently selected from one of hydrogen, alkyl；
N is integer, value range 4≤n≤50 of n；
Preferably, R in the urushiol-based emulsifier01Selected from formula (a) structural formula group, have formula (b) shown in knot
Any one of the group of structure formula, the group with structural formula shown in formula (c), group with structural formula shown in formula (d):
4. Neutral writing ink according to claim 1, which is characterized in that further include dispersible pigment color paste, water in the Neutral writing ink
Property resin emulsion, shear shinning agent, surfactant, lubricant, wetting agent, moisturizer, preservative, antirust agent, antifreezing agent, pH
Regulator, solvent.
5. Neutral writing ink according to claim 4, which is characterized in that in Neutral writing ink, the content of each component are as follows:
6. Neutral writing ink according to claim 4, which is characterized in that in Neutral writing ink, the content of each component are as follows:
7. Neutral writing ink according to claim 5, which is characterized in that the dispersible pigment color paste is aqueous carbon black dispersible pigment color paste；
The resin aqueous emulsion is in aqueous polyurethane emulsion, water-and acrylate lotion, aqueous alkide resin emulsion
It is at least one；
The shear shinning agent is selected from least one of xanthan gum, polyvinyl glue, guar gum；
The surfactant is complexed surfactant, and the complexed surfactant is by anionic surfactant and non-
Ionic surfactant composition；The anionic surfactant is selected from dodecyl sodium sulfate, lauryl sodium sulfate
At least one of, the nonionic surface active agent is selected from least one of triton x-100, Tween 80；
Wherein, the ratio of anionic surfactant and nonionic surface active agent is 1:0.2~5；
The lubricant is selected from least one of potassium oleate, enuatrol, potassium stearate, phosphate；
The wetting agent is selected from least one of urea element, sorbitol, Silok-8100, Bi Ke 154, Bi Ke 191；
The moisturizer is selected from least one of water-soluble denaturated silicone oil, sucrose, glucose；
The preservative is selected from 2- benzisothiazole-3-ketone and its derivative, imidazole and its derivants, benzimidazole and its spreads out
At least one of biology；
The antirust agent is selected from least one of benzotriazole, tolytriazole；
The antifreezing agent in glycerol, diglycerol, ethylene glycol, diethylene glycol, triethylene glycol, two diethyl acetals at least one
Kind；
The pH adjusting agent is selected from least one of monoethanolamine, diethanol amine, triethanolamine；
The solvent is deionized water.
8. a kind of method for preparing the described in any item Neutral writing inks of claim 1 to 7, which is characterized in that emulsify laccol base
Agent is mixed with other components, and the Neutral writing ink can be obtained.
9. according to the method described in claim 8, it is characterized in that, at least including the following steps:
A) mixture I containing shear shinning agent, preservative is obtained；
B) obtain containing urushiol-based emulsifier, anionic surfactant, lubricant, moisturizer, antirust agent mixture II；
C) antifreezing agent, wetting agent, nonionic surface active agent, resin aqueous emulsion and dispersible pigment color paste step b) is added to obtain
In the mixtures II obtained, mixture III is obtained；
D) mixture IV containing mixture I and mixture III is obtained, pH adjusting agent is added and adjusts pH, the neutrality can be obtained
Ink.
10. a kind of product, which is characterized in that the product includes the described in any item Neutral writing inks of claim 1 to 7, according to
Any one of the Neutral writing ink that claim 8 or 9 the methods are prepared；
Preferably, the product is a based article.
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