CN109608938A - A kind of surface modification technology of ink mill base - Google Patents
A kind of surface modification technology of ink mill base Download PDFInfo
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- CN109608938A CN109608938A CN201811456568.9A CN201811456568A CN109608938A CN 109608938 A CN109608938 A CN 109608938A CN 201811456568 A CN201811456568 A CN 201811456568A CN 109608938 A CN109608938 A CN 109608938A
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- mill base
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- surface modification
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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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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Inks, Pencil-Leads, Or Crayons (AREA)
Abstract
The invention discloses a kind of surface modification technology of ink mill base, include the following steps: for wetting agent, leuco dye and emulsifier to be add to deionized water and be stirred and heat, and color developing agent is added, gets a uniform mixture；High speed shearing emulsification is carried out with mulser, makes up to ideal partial size, partial size is D90≤300nm, obtains standby color paste；Standby color paste is poured into reaction kettle, is heated at 55~65 DEG C, surface is carried out and is modified, obtains modified mill base.The present invention has good matching with used medium, improves the quality of mill base by making it have good dispersibility and higher hydrophily to mill base progress surface is modified.By the modified working process in a variety of surfaces and matched auxiliary agent, produces application performance and meet enhanced water resistance, different types of ink of chemical-resistant reagent requirement or the special cargo of printing coatings.
Description
Technical field
The invention belongs to be used to prepare the mill base preparation technical field of ink more particularly to a kind of surface of ink mill base to change
Property technique.
Background technique
The suspension of Neutral writing ink system pigment particle, since solid pigment density is significantly greater than fluid density, thus it is neutral black
Water actually belongs to Unstable Systems, and the external product shelf-life is only 1 year or so at present.In order to improve the stability of Neutral writing ink,
Added with aqueous polymer resin in existing formula, such as polyacrylic acid water-base resin (United States Patent (USP) technology, US2002/
0071709A1, added with the acrylic resin of the molecular weight ranges 5000-10000 of 2wt.% in formula), increase to a certain extent
Added the resting period of ink, but as introduced fluoropolymer resin itself or with organic solvent existing for system be easy to produce
Raw polymerization and crosslinking, resin molecular weight are continuously increased with the increase of storage life, and ink viscosity is caused to improve, and mobility is deteriorated,
It is long placed in rear out of ink unsmooth, or even can not normally write so as to cause gel ink pen.
In ink production, existing mill base particle is big, and particle diameter distribution is uneven, is difficult to improve mill base quality.In colored ink
Pigment particle size, surface tension, viscosity, stability all require strictly.
Summary of the invention
Big for mill base feed particles in solution ink production, particle diameter distribution is uneven, surface tension is big, viscosity is big, stablizes
The bad problem of property, the present invention provides a kind of surface modification technology of ink mill base, for improving the quality of mill base, to promote ink
The quality of water finished product.Specific technical solution is as described below:
A kind of surface modification technology of ink mill base, includes the following steps:
Wetting agent, leuco dye and emulsifier are add to deionized water and are stirred and heat, and be added by the first step
Color developing agent gets a uniform mixture；
Second step carries out high speed shearing emulsification with mulser, makes up to ideal partial size, and partial size is D90≤300nm,
Obtain standby color paste；
Third step pours into standby color paste in reaction kettle, heats at 55~65 DEG C, carries out surface and is modified, and obtains modified color
Slurry.
And be modified in mill base backward and thickener is added, and be filtered, the operation such as vacuum outgas, ink products is made.
Preferably, wetting agent described in the first step is selected from ammonium polyacrylate salt, polyacrylic acid sodium salt, di-2-ethylhexylphosphine oxide first naphthalene sulphur
Sour sodium, benzyl naphthalenesulfonate formaldehyde condensation compound, naphthalenesulfonic acid-formaldehyde condensate, sulfocarbolate formaldehyde condensation products, phenolic aldehyde polyoxy second
One of alkene ether, polyoxyethylene ether, derivative of fatty acid, polyacrylate, alkyl sulfate and alkylsulfonate compound.
The emulsifier is nonionic surfactant, is selected from nonylphenol polyoxyethylene ether, octyl phenol polyoxyethylene ether, ten
One or more of polyglycerol monooleate, glycerin monostearate.
The third step surface modification technology includes that dispersing agent is added while stirring, then stirs while surface-active is added
Agent finally adjusts pH value with pH adjusting agent after stirring 2 hours.
Preferably, the dispersing agent is selected from polyethylene glycol 200, polyethylene glycol 400, Sodium Polyacrylate, dispersing agent N, sulfonic acid
One of salt (R-SO3Na), enuatrol, carboxylate or two kinds of mixture, the dispersing agent additional amount range is with mill base
Quality is calculated as 3%-10%；
Preferably, the surfactant is selected from sodium n-alkylbenzenesulfonate (LAS), sodium sulfate of polyethenoxy ether of fatty alcohol
(AES), fatty alcohol polyoxyethylene ether ammonium sulfate (AESA), sldium lauryl sulfate (K12 or SDS), lauroyl glutamate, nonyl
Base phenol polyethenoxy (10) ether (TX-10), paregal O, diglycollic amide (6501) glycerol stearate monoesters, lignin sulfonic acid
Salt, heavy alkylbenzene sulfonate, alkylsulfonate (petroleum sulfonate), dispersing agent NNO, dispersing agent MF, (PO-EO is total for alkyl, polyether
Polymers), the mixture of one or both of aliphatic alcohol polyethenoxy (3) ether (AEO-3), additional amount range is in terms of mill base quality
For 0.5%-5%；
Preferably, the pH adjusting agent is selected from one of triethanolamine, ethylenediamine, 2 hydroxy ethylamine or two kinds of mixing
Modified mill base is adjusted pH value to 7.0~9.0 by object, and pH adjusting agent additional amount range is calculated as 0.1%- with mill base quality
1%；
The color developing agent is water-soluble R- hydroxy-pheny-derivatives of isobenzofaranone or R- hydroxy-phenylene-
Derivatives of isobenzofaranone.It has been draped over one's shoulders in publication " ink and preparation method thereof " (application number: CN201410313003.0)
The type of color developing agent is revealed, color developing agent can for one of red color developing agent, blue colouration agent and purple color developing agent or at least
Two kinds of combination.Red color developing agent are as follows: the different benzofuranone up and down of bis- (the 2- hydroxy phenyls) -1 (3H)-of 3,3-；The blue is aobvious
Toner are as follows: 3,3- bis- [2- hydroxy-4-methyl -5- (1- methyl) phenyl] -1 (3H) -2- benzo [C] furanone；The purple is aobvious
Toner are as follows: N, N '-[(5- oxo -1 (3H)-isobenzofuran-base subunit] bis- [(6- hydroxyl -3,1- phenylene) methylene] double
[N- (carboxymethyl group) glycine].
The thickener is the mixture of one or both of hydroxyethyl cellulose or hydroxypropyl cellulose.
It is the gap of raw particles to be infiltrated through, in grain by its wetting action and osmosis that dispersing agent, which is added, in the present invention
Oriented attachment occurs for the surface of son, to change the surface property of solids, and charges particle surface, forms double electricity
Layer, prevents the aggregation of particle, and pigment dispersion system is made to form stabilization.
By different piece in molecule respectively for the affine of two-phase, two-phase is made to be regarded as the ingredient of this phase, molecule
Arrangement between the two phases, is equivalent to the surface of two-phase and is transferred to intramolecule.To reduce surface tension.Since two-phase is all by it
A component for regarding this phase as, is equivalent to two phases and surfactant molecule does not all form interface, is equivalent to pass through
The elimination of this mode part interface of two phases, reduces surface tension and surface free energy, just so as to improve mill base
Hydrophily.
The invention enables mill bases obtained to have good compatibility, is because good compatibility can be such that coating manufactures
Quotient's production is used for the dispersion of a variety of different classes of naval stores.Pigment concentration can be improved in polymeric dispersant, not only increases
Add yield, and improves from mill base until medium incompatibility problem potential in final products.So especially with high phase
Under conditions of capacitive resin, polymeric dispersant expands the use scope of basic coating.This is non-to mixing pigmented finiss production
It is often important.More high pigment levels can be improved using dispersing agent, keep particle fragmentation rapider, while preventing viscosity from increasing, point
Powder increases more tiny particle encounter stability, does not flocculate, thus give full play in it tinctorial strength.
Surface is modified to make it have good dispersibility and higher hydrophily to the present invention by carrying out to mill base, and used
Medium has good matching, improves the quality of mill base.Pass through the modified working process in a variety of surfaces and matched auxiliary agent, system
Produce the extraordinary quotient that application performance meets enhanced water resistance, different types of ink of chemical-resistant reagent requirement or printing coatings
Product.
The auxiliary agent includes the conventional use of fungicide for ink production, wetting agent, thickener, resin etc..
This technology is different from being in place of the prior art, in ink production process, change to the mill base of intermediate products
Property processing, so as to avoid process is modified again after producing ink, the beneficial effect of this change is: 1. are used as ink
Intermediate raw material, the usage amount of mill base is modified dispersing agent, table used in processing to mill base far fewer than the quantum of output of ink
The dosage that face activating agent and other reagent consumptions comparison ink are modified processing is few, reduces production cost；2. this technology
Heating is carried out to mill base in early period and cooling is handled, is then prepared into ink, compared to being modified processing again after having prepared ink,
Ink property obtained by this technology is more stable.
Detailed description of the invention
The Figure of description for constituting a part of the invention is used to provide further understanding of the present invention, and of the invention shows
Examples and descriptions thereof are used to explain the present invention for meaning property, does not constitute improper limitations of the present invention.
Fig. 1 is a kind of schematic diagram of the surface modification technology of ink mill base provided by the invention.
Specific embodiment
It is noted that described further below be all exemplary, it is intended to provide further instruction to the present invention.Unless another
It indicates, all technical and scientific terms used herein has usual with general technical staff of the technical field of the invention
The identical meanings of understanding.
It should be noted that term used herein above is merely to describe specific embodiment, and be not intended to restricted root
According to exemplary embodiments of the present invention.As used herein, unless the context clearly indicates otherwise, otherwise singular
Also it is intended to include plural form, additionally, it should be understood that, when in the present specification using term "comprising" and/or " packet
Include " when, indicate existing characteristics, step, operation, device, component and/or their combination.
Embodiment 1:
The preparation of ink: the first step, by 0.2g wetting agent polyacrylate, 0.1g leuco dye and 0.2g monostearate
Glyceride is added in 100ml deionized water and is stirred and heats, and 0.05g color developing agent 3, the bis- [2- hydroxyl -4- of 3- are added
Methyl -5- (1- methyl) phenyl] -1 (3H) -2- benzo [C] furanone, it gets a uniform mixture；
Second step carries out high speed shearing emulsification with mulser, until partial size is D90≤300nm, obtains standby color paste；
Third step pours into standby color paste in reaction kettle, heats at about 55 DEG C, carries out surface and is modified, is added while stirring
3g dispersing agent polyethylene glycol 200 then stirs while being added surfactant 0.6gSDS and finally uses second two after stirring 2 hours
Amine adjusts pH to 7.5, obtains modified mill base.
And be modified in mill base backward and hydroxyethyl cellulose be added, and be filtered, the operation such as vacuum outgas, be made ink at
Product.
Embodiment 2:
The preparation of ink: the first step, by 0.2g wetting agent polyacrylate, 0.1g leuco dye and 0.2g monostearate
Glyceride is added in 100ml deionized water and is stirred and heats, and 0.05g color developing agent 3, the bis- [2- hydroxyl -4- of 3- are added
Methyl -5- (1- methyl) phenyl] -1 (3H) -2- benzo [C] furanone, it gets a uniform mixture；
Second step carries out high speed shearing emulsification with mulser, until partial size is D90≤300nm, obtains standby color paste；
Third step pours into standby color paste in reaction kettle, heats at about 65 DEG C, carries out surface and is modified, is added while stirring
10g dispersing agent enuatrol then stirs while being added surfactant 5g lauroyl glutamate and finally uses after stirring 2 hours
Ethylenediamine adjusts pH to 8.7, obtains modified mill base.
And be modified in mill base backward and hydroxyethyl cellulose be added, and be filtered, the operation such as vacuum outgas, be made ink at
Product.
Embodiment 3:
The preparation of ink: the first step, by 0.3g wetting agent polyacrylate, 0.3g leuco dye and 0.1g monostearate
Glyceride is added in 100ml deionized water and is stirred and heats, and 0.1g color developing agent R- hydroxy-phenylene-different benzene is added
And furanone derivatives, it gets a uniform mixture；
Second step carries out high speed shearing emulsification with mulser, until partial size is D90≤300nm, obtains standby color paste；
Third step pours into standby color paste in reaction kettle, heats at about 60 DEG C, carries out surface and is modified, is added while stirring
10g dispersing agent Sodium Polyacrylate then stirs while being added surfactant 5g sodium sulfate of polyethenoxy ether of fatty alcohol (AES),
After stirring 2 hours, pH to 8.1 finally is adjusted with ethylenediamine, obtains modified mill base.
And be modified in mill base backward and hydroxyethyl cellulose be added, and be filtered, the operation such as vacuum outgas, be made ink at
Product.
Comparative example:
Sodium Polyacrylate 0.5g: (1) being dissolved in 10g deionized water by conventional inks preparation process first, and stirring keeps its molten
Solution prepares thickener soln to fully transparent；(2) glycerine solvent 15g is hybridly prepared into solvent with 10g deionized water and mixes
Object；(3) by dispersible pigment color paste 25g, common unmodified polypropylene yogurt liquid 20g, 25g solvent mixture, stearic acid 0.5g, benzo
Triazole 0.5g, potassium sorbate 0.5g, Laurate alcohol ester phenylacetate defoaming agent (Aldrich) 0.1g, deionized water 15.9g are stirred
It mixes uniformly；(4) prepared ink slurry is placed in mulser high speed (revolving speed is 1000 revs/min) emulsification 15 minutes, so
It is placed in sand mill and is sanded 60 minutes.(5) thickener of (1) step preparation, triethanolamine 2g, stirring 30 are added after being sanded
After minute, by gained thick liquid with 1um filter element filtering, packaging, it is prepared into Neutral writing ink finished product.
Pen core is made in the ink prepared in Examples 1 to 3 and comparative example, and detects the performance indicator result of the pen core such as
Under:
Wherein, viscosity is measured referring to standard GB/T/T14624.5-93 " the ink viscosity method of inspection ".
Situation, high/low temperature stability test method are write referring to People's Republic of China's light industry standard QB/T2625-
2003 " gel pen and pen cores " are detected.
The above results show to carry out surface to mill base using provided by the invention that modified to prepare ink properties good
Good, internal stability is good within 12 months.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field
For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, made any to repair
Change, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (7)
1. a kind of surface modification technology of ink mill base, which comprises the steps of:
Wetting agent, leuco dye and emulsifier are add to deionized water and are stirred and heat, and colour developing is added by the first step
Agent gets a uniform mixture；
Second step carries out high speed shearing emulsification with mulser, makes up to ideal partial size, and partial size is D90≤300nm, obtains
Standby color paste；
Third step pours into standby color paste in reaction kettle, heats at 55~65 DEG C, carries out surface and is modified, and obtains modified mill base.
2. a kind of surface modification technology of ink mill base according to claim 1, which is characterized in that the choosing of wetting agent described in the first step
From for ammonium polyacrylate salt, polyacrylic acid sodium salt, di-2-ethylhexylphosphine oxide first sodium naphthalene sulfonate, benzyl naphthalenesulfonate formaldehyde condensation compound, naphthalene sulphur
Sour sodium formaldehyde condensation product, sulfocarbolate formaldehyde condensation products, phenolic aldehyde polyoxyethylene ether, polyoxyethylene ether, derivative of fatty acid, poly- third
One of olefin(e) acid ester, alkyl sulfate and alkylsulfonate compound.
3. a kind of surface modification technology of ink mill base according to claim 1, which is characterized in that the emulsifier is nonionic table
Face activating agent is selected from nonylphenol polyoxyethylene ether, octyl phenol polyoxyethylene ether, ten polyglycerol monooleates, glycerol monostearate
One or more of ester.
4. a kind of surface modification technology of ink mill base according to claim 1, which is characterized in that the modified work in the third step surface
Skill includes that dispersing agent is added while stirring, then stirs while being added surfactant and finally adjusted with pH after stirring 2 hours
Agent adjusts pH value.
5. a kind of surface modification technology of ink mill base according to claim 1, which is characterized in that the dispersing agent is selected from poly- second two
One of alcohol 200, polyethylene glycol 400, Sodium Polyacrylate, dispersing agent N, sulfonate (R-SO3Na), enuatrol, carboxylate or
The mixture that two kinds of person, the dispersing agent additional amount range are calculated as 3%-10% with mill base quality.
6. a kind of surface modification technology of ink mill base according to claim 1, which is characterized in that the surfactant is selected from straight
Alkyl group benzene sulfonic acid sodium salt, sodium sulfate of polyethenoxy ether of fatty alcohol, fatty alcohol polyoxyethylene ether ammonium sulfate, sldium lauryl sulfate, the moon
Osmanthus acyl glutamic acid, nonylphenol polyoxyethylene ether, paregal O, diglycollic amide glycerol stearate monoesters, lignosulfonates,
Heavy alkylbenzene sulfonate, alkylsulfonate, dispersing agent NNO, dispersing agent MF, alkyl, polyether, one in fatty alcohol polyoxyethylene ether
Kind or two kinds of mixture, additional amount range are calculated as 0.5%-5% with mill base quality.
7. a kind of surface modification technology of ink mill base according to claim 1, which is characterized in that the pH adjusting agent is selected from three second
One of hydramine, ethylenediamine, 2 hydroxy ethylamine or two kinds of mixtures, by modified mill base adjust pH value to 7.0~
9.0。
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201811456568.9A CN109608938A (en) | 2018-11-30 | 2018-11-30 | A kind of surface modification technology of ink mill base |
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| CN201811456568.9A CN109608938A (en) | 2018-11-30 | 2018-11-30 | A kind of surface modification technology of ink mill base |
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| CN109608938A true CN109608938A (en) | 2019-04-12 |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113648841A (en) * | 2021-08-05 | 2021-11-16 | 苏州中色德源环保科技有限公司 | Dry-state preservation method for hollow fiber membrane |
| CN113736317A (en) * | 2021-06-17 | 2021-12-03 | 山东掘色新材料科技有限公司 | Thermosensitive color-changing pen ink |
-
2018
- 2018-11-30 CN CN201811456568.9A patent/CN109608938A/en not_active Withdrawn
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113736317A (en) * | 2021-06-17 | 2021-12-03 | 山东掘色新材料科技有限公司 | Thermosensitive color-changing pen ink |
| CN115124884A (en) * | 2021-06-17 | 2022-09-30 | 山东掘色新材料科技有限公司 | Thermosensitive color-changing watercolor pen ink |
| CN113648841A (en) * | 2021-08-05 | 2021-11-16 | 苏州中色德源环保科技有限公司 | Dry-state preservation method for hollow fiber membrane |
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Application publication date: 20190412 |
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