CN103897483B - A kind of neutral blue ink and preparation method thereof - Google Patents
A kind of neutral blue ink and preparation method thereof Download PDFInfo
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- CN103897483B CN103897483B CN201410123952.2A CN201410123952A CN103897483B CN 103897483 B CN103897483 B CN 103897483B CN 201410123952 A CN201410123952 A CN 201410123952A CN 103897483 B CN103897483 B CN 103897483B
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- 230000007935 neutral effect Effects 0.000 title claims abstract description 57
- 238000002360 preparation method Methods 0.000 title claims abstract description 35
- NIXOWILDQLNWCW-UHFFFAOYSA-N Acrylic acid Chemical compound OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 66
- 229920002125 Sokalan® Polymers 0.000 claims abstract description 64
- 229960001631 carbomer Drugs 0.000 claims abstract description 64
- 239000011159 matrix material Substances 0.000 claims abstract description 28
- 230000008719 thickening Effects 0.000 claims abstract description 28
- 239000006185 dispersion Substances 0.000 claims abstract description 22
- -1 oligose Substances 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 11
- 239000008367 deionised water Substances 0.000 claims abstract description 11
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 11
- 238000000518 rheometry Methods 0.000 claims abstract description 11
- 239000003002 pH adjusting agent Substances 0.000 claims abstract description 9
- XCJYREBRNVKWGJ-UHFFFAOYSA-N copper(II) phthalocyanine Chemical compound [Cu+2].C12=CC=CC=C2C(N=C2[N-]C(C3=CC=CC=C32)=N2)=NC1=NC([C]1C=CC=CC1=1)=NC=1N=C1[C]3C=CC=CC3=C2[N-]1 XCJYREBRNVKWGJ-UHFFFAOYSA-N 0.000 claims abstract description 8
- 239000013530 defoamer Substances 0.000 claims abstract description 8
- 230000003449 preventive effect Effects 0.000 claims abstract description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000000203 mixture Substances 0.000 claims description 40
- 238000003756 stirring Methods 0.000 claims description 36
- 238000013019 agitation Methods 0.000 claims description 18
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims description 18
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 15
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 12
- QRUDEWIWKLJBPS-UHFFFAOYSA-N benzotriazole Chemical compound C1=CC=C2N[N][N]C2=C1 QRUDEWIWKLJBPS-UHFFFAOYSA-N 0.000 claims description 10
- 239000012964 benzotriazole Substances 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 10
- 239000002245 particle Substances 0.000 claims description 10
- OWEGMIWEEQEYGQ-UHFFFAOYSA-N 100676-05-9 Natural products OC1C(O)C(O)C(CO)OC1OCC1C(O)C(O)C(O)C(OC2C(OC(O)C(O)C2O)CO)O1 OWEGMIWEEQEYGQ-UHFFFAOYSA-N 0.000 claims description 9
- GUBGYTABKSRVRQ-PICCSMPSSA-N Maltose Natural products O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@@H]1O[C@@H]1[C@@H](CO)OC(O)[C@H](O)[C@H]1O GUBGYTABKSRVRQ-PICCSMPSSA-N 0.000 claims description 9
- 239000004698 Polyethylene Substances 0.000 claims description 9
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 9
- 229920000573 polyethylene Polymers 0.000 claims description 9
- 239000000839 emulsion Substances 0.000 claims description 8
- 235000010228 ethyl p-hydroxybenzoate Nutrition 0.000 claims description 7
- 239000004403 ethyl p-hydroxybenzoate Substances 0.000 claims description 7
- 229940043351 ethyl-p-hydroxybenzoate Drugs 0.000 claims description 7
- NUVBSKCKDOMJSU-UHFFFAOYSA-N ethylparaben Chemical compound CCOC(=O)C1=CC=C(O)C=C1 NUVBSKCKDOMJSU-UHFFFAOYSA-N 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 7
- CZMRCDWAGMRECN-UGDNZRGBSA-N Sucrose Chemical compound O[C@H]1[C@H](O)[C@@H](CO)O[C@@]1(CO)O[C@@H]1[C@H](O)[C@@H](O)[C@H](O)[C@@H](CO)O1 CZMRCDWAGMRECN-UGDNZRGBSA-N 0.000 claims description 6
- 229930006000 Sucrose Natural products 0.000 claims description 6
- 239000003094 microcapsule Substances 0.000 claims description 6
- 239000005720 sucrose Substances 0.000 claims description 6
- MEIRRNXMZYDVDW-MQQKCMAXSA-N (2E,4E)-2,4-hexadien-1-ol Chemical compound C\C=C\C=C\CO MEIRRNXMZYDVDW-MQQKCMAXSA-N 0.000 claims description 5
- ZNQVEEAIQZEUHB-UHFFFAOYSA-N 2-ethoxyethanol Chemical compound CCOCCO ZNQVEEAIQZEUHB-UHFFFAOYSA-N 0.000 claims description 5
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 5
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 claims description 5
- 239000008103 glucose Substances 0.000 claims description 5
- DURPTKYDGMDSBL-UHFFFAOYSA-N 1-butoxybutane Chemical compound CCCCOCCCC DURPTKYDGMDSBL-UHFFFAOYSA-N 0.000 claims description 4
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 claims description 4
- 239000005977 Ethylene Substances 0.000 claims description 4
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 4
- ZBCBWPMODOFKDW-UHFFFAOYSA-N diethanolamine Chemical compound OCCNCCO ZBCBWPMODOFKDW-UHFFFAOYSA-N 0.000 claims description 4
- 238000006116 polymerization reaction Methods 0.000 claims description 4
- POAOYUHQDCAZBD-UHFFFAOYSA-N 2-butoxyethanol Chemical compound CCCCOCCO POAOYUHQDCAZBD-UHFFFAOYSA-N 0.000 claims description 3
- KGWDUNBJIMUFAP-KVVVOXFISA-N Ethanolamine Oleate Chemical compound NCCO.CCCCCCCC\C=C/CCCCCCCC(O)=O KGWDUNBJIMUFAP-KVVVOXFISA-N 0.000 claims description 3
- 239000004743 Polypropylene Substances 0.000 claims description 3
- GSEJCLTVZPLZKY-UHFFFAOYSA-N Triethanolamine Chemical compound OCCN(CCO)CCO GSEJCLTVZPLZKY-UHFFFAOYSA-N 0.000 claims description 3
- 239000003112 inhibitor Substances 0.000 claims description 3
- 235000010270 methyl p-hydroxybenzoate Nutrition 0.000 claims description 3
- 239000004292 methyl p-hydroxybenzoate Substances 0.000 claims description 3
- LXCFILQKKLGQFO-UHFFFAOYSA-N methylparaben Chemical compound COC(=O)C1=CC=C(O)C=C1 LXCFILQKKLGQFO-UHFFFAOYSA-N 0.000 claims description 3
- 239000005543 nano-size silicon particle Substances 0.000 claims description 3
- 229920001155 polypropylene Polymers 0.000 claims description 3
- 230000008569 process Effects 0.000 claims description 3
- 229960004418 trolamine Drugs 0.000 claims description 3
- 239000000976 ink Substances 0.000 abstract description 60
- 230000008901 benefit Effects 0.000 abstract description 4
- 238000007639 printing Methods 0.000 abstract description 3
- 239000000080 wetting agent Substances 0.000 abstract description 3
- 238000005538 encapsulation Methods 0.000 abstract description 2
- 238000005189 flocculation Methods 0.000 abstract description 2
- 230000016615 flocculation Effects 0.000 abstract description 2
- 150000004676 glycans Chemical class 0.000 abstract description 2
- 229920001282 polysaccharide Polymers 0.000 abstract description 2
- 239000005017 polysaccharide Substances 0.000 abstract description 2
- 239000007864 aqueous solution Substances 0.000 abstract 1
- 239000000243 solution Substances 0.000 description 23
- 238000012360 testing method Methods 0.000 description 10
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- 238000001914 filtration Methods 0.000 description 8
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- 230000000052 comparative effect Effects 0.000 description 7
- 238000001879 gelation Methods 0.000 description 7
- 239000007788 liquid Substances 0.000 description 7
- 229920001285 xanthan gum Polymers 0.000 description 7
- 239000000230 xanthan gum Substances 0.000 description 7
- 229940082509 xanthan gum Drugs 0.000 description 7
- 235000010493 xanthan gum Nutrition 0.000 description 7
- DNIAPMSPPWPWGF-UHFFFAOYSA-N Propylene glycol Chemical compound CC(O)CO DNIAPMSPPWPWGF-UHFFFAOYSA-N 0.000 description 4
- GUBGYTABKSRVRQ-QUYVBRFLSA-N beta-maltose Chemical compound OC[C@H]1O[C@H](O[C@H]2[C@H](O)[C@@H](O)[C@H](O)O[C@@H]2CO)[C@H](O)[C@@H](O)[C@@H]1O GUBGYTABKSRVRQ-QUYVBRFLSA-N 0.000 description 4
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
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- 238000010008 shearing Methods 0.000 description 2
- 230000009471 action Effects 0.000 description 1
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- 239000003607 modifier Substances 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
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Abstract
The invention discloses a kind of neutral blue ink and preparation method thereof.This neutral blue ink is made up of blue mill base, carbomer, rheology control agent, lower alcohol, oligose, Antisepticize and mildew preventive, pH adjusting agent, defoamer, deionized water.Its preparation process comprises: prepare the carbomer aqueous solution, adds wetting Agent for Printing Inks, rheology control agent, oligose, pH adjusting agent wherein, obtains carbomer gel; Add Antisepticize and mildew preventive, defoamer again, obtain thickening thixotroping matrix; Add blue mill base again, obtain neutral blue ink.Advantage of the present invention is that employing comprises carbomer, polysaccharide, rheology control agent and micro encapsulation CuPc mill base component and carries out reasonable coordination, make colo(u)rant dispersion even, there is not flocculation of reuniting, obtained Neutral writing ink good stability, mildew resistance are good, the time of raising one's hat is long, have higher thixotropy, write that feel is fluent, svelteness.
Description
Technical field
The present invention relates to a kind of neutral blue ink and preparation method thereof, belong to technical field of ink.
Background technology
Ballpoint pen, as a kind of writing implement, has carried out writing of writing etc. by nib by the ink transfer in ballpoint pen to writing medium.A kind of ballpoint pen of high-quality requires that it all should not drip ink, not trickling when writing or do not write, and have to require when writing out of ink evenly, the advantage such as writing line weight is even, color is suitable, sticking power is good, antifriction.Therefore, on the basis of oiliness ballpoint pen and aqueous ballpoint pen, people, in conjunction with the advantage of the two, develop a kind of neutral ballpoint pen, and what it not only had a water-base ink writes lubrication fluency, and has the feature of good antitrickle.Compared with traditional writing implement, neutral ballpoint pen obviously more meets the requirement of human consumer, liking more by everybody.
The ink used in neutral ballpoint pen is called Neutral writing ink.Neutral writing ink has unique rheological property, and namely when not shearing under External Force Acting, viscosity is very large, can guarantee that ballpoint pen does not drip ink, do not trickle; Writing under shear action, the viscosity of ink is lower and less with shearing force change, thus when can ensure to write, lubrication does not break and amount out of ink is even.The rheologic behavio(u)r of Neutral writing ink is not only relevant with the factor such as concentration, electrolyte strength, pH value, temperature of the kind of its thickening material, solvent, solution, and with the dispersible pigment color paste, the various auxiliary agent such as also close relation such as surface tension modifier, pH adjusting agent, sanitas and wetting Agent for Printing Inks that use in ink modulation process.Consistency above between these processing parameters, component and cooperation technique etc. can not only change the rheological property of ink, and directly affect stability and the integrated application performance of ink.In other words, ink set technology is the key determining Neutral writing ink over-all properties.
Neutral writing ink water-based system safety and environmental protection, excellent durability, fluent writing, occupy dominant contribution that is domestic and ballpoint pen market, Asia.But China studies with the Neutral writing ink thixotropy manufactured low now, and rheological property is poor, and poor stability, these all cause manufactured product time of raising one's hat short, and the storage time is short, writing quality is poor, so that China's ball pen ink is all rely on import to solve at present.
Summary of the invention
The object of the invention is to provide a kind of neutral blue ink and preparation method thereof, and this ink has that the time of raising one's hat is long, thixotropy is high, the feature of good stability, and preparation process is simple, easily realizes suitability for industrialized production.
The present invention is realized by the following technical programs: a kind of neutral blue ink, is characterized in that, this neutral blue ink is made up of following component and mass percentage:
Blue mill base, 30%-50%; Carbomer, 0.3%-0.6%; Rheology control agent, 2%-8%; Lower alcohol, 15%-30%; Oligose, 1%-4%; Antisepticize and mildew preventive 0.4%-0.6%, pH adjusting agent 0.6%-1.7%, defoamer 0.2%-0.4%, all the other are deionized water, and the mass percentage sum of above-mentioned each component is 100%.
Blue mill base in said components is at 80-600nm containing particle diameter, the CuPc microcapsule aqueous color paste that mass percentage forms at the CuPc microcapsule of 15%-45%, CuPc surface of microcapsule contains non-ionic hydrophilic group, and zeta current potential is 35-70mV.
Carbomer in said components is carbomer series, is Acritamer 940, Acritamer 940 L, carbomer 2020, Carpobol 956 or carbomer 970.
Rheology control agent in said components to be massfraction be 10% nano silicon, or for the massfraction formed by polyethylene, oxidic polyethylene or polypropylene be the nano-scale dispersion emulsion one wherein of 30%.
Lower alcohol in said components is two or more the mixture in 1,2-PD, glycerol, sorbyl alcohol, ethylene glycol, ethylene glycol ethyl ether, diethylene glycol ether, butyl glycol ether and diglycol ethylene butyl ether.
The oligopolymer that oligose in said components is molecular-weight average one or both or three kinds of sugar polymerizations are formed in the maltose of 200-2000, sucrose, glucose.
Antisepticize and mildew preventive in said components is one or both in benzotriazole, mould inhibitor 253, AF251, ethyl p-hydroxybenzoate and methyl p-hydroxybenzoate; Defoamer in said components is one or both in SE-47, SD-670 and JS-5115.
PH adjusting agent in said components is the one in ammoniacal liquor, sodium hydroxide, thanomin, diethanolamine and trolamine.
The preparation method of the neutral blue ink of said structure, is characterized in that comprising following process:
Get carbomer aqueous dispersions 20-40 part that mass concentration is 1.07%-1.6% by mass, under agitation add 15-30 part wetting Agent for Printing Inks wherein, 2-8 part rheology control agent, with 1-4 part oligose, degassed after fully mixing at 40-45 DEG C, add 0.6-1.7 part pH adjusting agent in 10min while stirring, obtain carbomer gel; In this gel, add Antisepticize and mildew preventive 0.4-0.6 part again, defoamer 0.2-0.4 part, filter after stirring in 10min and obtain thickening thixotroping matrix; Under agitation, in this matrix, slowly add the blue mill base of 30-50 part, mix rear degassed, obtain that pH is 7-8, thixotropy index is the neutral blue ink of 4.0-7.
The present invention compared with prior art has the following advantages, the present invention's employing comprises carbomer, polysaccharide, rheology control agent and CuPc micro encapsulation mill base component and carries out reasonable coordination, make colo(u)rant dispersion even, there is not flocculation of reuniting, obtained Neutral writing ink good stability, mildew resistance are good, the time of raising one's hat is long, have higher thixotropy, write that feel is fluent, svelteness.
Embodiment
Following examples are described in further detail the present invention, and do not mean that the restriction to protection scope of the present invention.
Embodiment 1
A. carbomer gel preparation
0.5g Acritamer 940 is dissolved in deionized water and obtains carbomer aqueous dispersions 30g, stir 2h, rear standing 2h.In this carbomer dispersion liquid, under agitation add that 25g mass ratio is 5:4:1 1,2-propylene glycol, the mixture of 70% sorbyl alcohol and ethylene glycol ethyl ether, 30% polyethylene emulsion of 8g is added again in this solution, the oligose of 1g maltose, degassed after fully mixing at 40-45 DEG C, in 10min, 30% sodium hydroxide adding 1.2g while stirring in this solution makes carbomer solution gelation;
B. thickening thixotroping matrix preparation
Be benzotriazole and the mould inhibitor 253(Shenzhen Haichuan Chemical Technology Co., Ltd of 1:1 by 0.6g mass ratio), Chemical Industry Science Co., Ltd is contained in 0.4gJS-349(Qingdao nine) mix and stir; This mixed solution is joined in above-mentioned carbomer gel and stirs 10min, fully mix rear filtration and obtain 60g thickening thixotroping matrix;
C. Neutral writing ink preparation
The 60g carbomer thickening thixotroping matrix prepared slowly is added under agitation the blue mill base of particle diameter at 80-600nm of 20% of 40g, fully mix rear degassed, obtain 100g neutral blue ink.
Senior rotational rheometer (Sweden) is adopted to test its apparent viscosity 47.2cPa to obtained neutral blue ink; Adopt viscosity during NDJ-1 rotary viscosity measurement 6r/min and 60r/min, and calculate its ratio, obtain thixotropy index 7.0; BZY series surface tension instrument is adopted to test its surface tension 36.0mN/m.
Embodiment 2
A. carbomer gel preparation
0.4g carbomer 970 is dissolved in deionized water and obtains carbomer aqueous dispersions 25g, stir 2h, rear standing 2h.Under agitation in this carbomer dispersion liquid, adding 20g mass ratio is the ethylene glycol of 10:1 and the mixture of diethylene glycol ether, 30% polyethylene emulsion of 2.3g is added again in this solution, the oligose of 4g maltose and sucrose polymerization, degassed after fully mixing at 40-45 DEG C, in 10min, the ammoniacal liquor adding 30% of 0.9g while stirring in this solution makes carbomer solution gelation;
B. thickening thixotroping matrix preparation
Be benzotriazole and the ethyl p-hydroxybenzoate of 1:1 by 0.5g mass ratio, Chemical Industry Science Co., Ltd is contained in the JS-5115(Qingdao nine of 0.3g) mix and stir, this mixed solution is joined in above-mentioned carbomer gel and stirs 10min, fully mix rear filtration and obtain 53g thickening thixotroping matrix;
C. Neutral writing ink preparation
The particle diameter 53g carbomer thickening thixotroping matrix prepared slowly being added under agitation 15% of 47g, at the blue mill base of 80-600nm, fully mixes rear degassed, obtains 100g neutral blue ink.
Obtained neutral blue ink apparent viscosity, thixotropy index and capillary test data are as shown in table 1.
Embodiment 3
A. carbomer gel preparation
0.3g carbomer 2020 is dissolved in deionized water and obtains carbomer aqueous dispersions 20g, stir 2h, rear standing 2h.In this carbomer dispersion liquid, under agitation add the mixture of the glycerol that 30g mass ratio is 15:1 and diglycol ethylene butyl ether, 30% oxidic polyethylene emulsion of 5.6g is added again in this solution, the oligose of 3g maltose, sucrose and glucose polymerisation, degassed after fully mixing at 40-45 DEG C, in 10min, 30% diethanolamine adding 0.6g while stirring in this solution makes carbomer solution gelation;
B. thickening thixotroping matrix preparation
Be the benzotriazole of 1:1 and ethyl p-hydroxybenzoate mixture, 0.2gSE-47(Shenzhen Haichuan Chemical Technology Co., Ltd by 0.6g mass ratio), mix and stir, this mixed solution is joined in above-mentioned carbomer gel and stirs 10min, fully mix rear filtration and obtain 60g thickening thixotroping matrix;
C. Neutral writing ink preparation
The 60g carbomer thickening thixotroping matrix prepared slowly is added under agitation the blue mill base of particle diameter at 80-600nm of 20% of 40g, fully mix rear degassed, obtain 100g neutral blue ink.
Obtained neutral blue ink apparent viscosity, thixotropy index and capillary test data are as shown in table 1.
Embodiment 4
A. carbomer gel preparation
0.3g Carpobol 956 is dissolved in deionized water and obtains carbomer aqueous dispersions 28g, stir 2h, rear standing 2h.Under agitation in this carbomer dispersion liquid, add 70% sorbyl alcohol that 15g mass ratio is 10:1 and ethylene glycol ethyl ethers ether mixture, the 10% nano silicon aqueous dispersions of 2g is added again in this solution, the oligose of 3.5g maltose, sucrose and glucose polymerisation, degassed after fully mixing at 40-45 DEG C, in 10min, 30% trolamine adding 0.6g while stirring in this solution makes carbomer solution gelation;
B. thickening thixotroping matrix preparation
Be benzotriazole and the AF251(Shenzhen Haichuan Chemical Technology Co., Ltd of 1:1 by 0.6g mass ratio) mixture, Chemical Industry Science Co., Ltd is contained in 0.3gJS-5115(Qingdao nine) mix and stir; This mixed solution is joined in above-mentioned carbomer gel and stirs 10min, fully mix rear filtration and obtain 50g thickening thixotroping matrix;
C. Neutral writing ink preparation
The 50g carbomer thickening thixotroping matrix prepared slowly is added under agitation the blue mill base of particle diameter at 80-600nm of 15% of 50g, fully mix rear degassed, obtain 100g neutral blue ink.
Obtained neutral blue ink apparent viscosity, thixotropy index and capillary test data are as shown in table 1.
Embodiment 5
A. carbomer gel preparation
0.6g Acritamer 940 L is dissolved in deionized water and obtains carbomer aqueous dispersions 40g, stir 2h, rear standing 2h.Under agitation in this carbomer dispersion liquid, adding 20g mass ratio is 10:1 glycerol and butyl glycol ether mixture, the 30% polypropylene emulsion of 4g is added again in this solution, the oligose of 3.5g maltose polymerization, degassed after fully mixing at 40-45 DEG C, in 10min, 30% thanomin adding 1.7g while stirring in this solution makes carbomer solution gelation;
B. thickening thixotroping matrix preparation
Be the benzotriazole of 1:1 and methyl p-hydroxybenzoate mixture by 0.4g mass ratio, 0.4gSD-670(Beijing An Tepuna scientific & trading Co., Ltd.) mix and stir; This mixed solution is joined in above-mentioned carbomer gel and stirs 10min, fully mix rear filtration and obtain 70g thickening thixotroping matrix;
C. Neutral writing ink preparation
The 70g carbomer thickening thixotroping matrix prepared slowly is added under agitation the blue mill base of particle diameter at 80-600nm of 45% of 30g, fully mix rear degassed, obtain 100g neutral blue ink.
Obtained neutral blue ink apparent viscosity, thixotropy index and capillary test data are as shown in table 1.
Comparative example 1
Comparative example 1 adopts the method as embodiment 1 to be prepared, and difference is, adopts xanthan gum to replace carbomer in its formula.Concrete preparation method is as follows:
A. the preparation of xanthan gum thickening thixotroping system
0.4g xanthan gum is dissolved in deionized water and obtains xanthan gum aqueous dispersions 30g, add under stirring that 25g mass ratio is 5:4:1 wherein 1,2-propylene glycol, the mixture of 70% sorbyl alcohol and ethylene glycol ethyl ether, 30% polyethylene emulsion of 8g is added again in this solution, the oligose of 1g maltose, degassed after fully mixing at 40-45 DEG C, obtain xanthan gum compound system; Be that Chemical Industry Science Co., Ltd is contained in benzotriazole and ethyl p-hydroxybenzoate mixture, 0.4gJS-5115(Qingdao nine of 1:1 by 0.4g mass ratio) mix and stir; This mixed solution is joined in above-mentioned xanthan gum compound system and stirs 10min, fully mix rear filtration and obtain 65g thickening thixotroping matrix;
B. Neutral writing ink preparation
The 65g xanthan gum thickening thixotroping matrix prepared slowly is added under agitation the blue mill base of particle diameter at 80-600nm of 30% of 35g, fully mix rear degassed, obtain 100g neutral blue ink.
Obtained neutral blue ink apparent viscosity, thixotropy index and capillary test data are as shown in table 1.
Comparative example 2
Comparative example 2 adopts the method as embodiment 2 to be prepared, and difference is, does not add oligose in its formula.Concrete preparation method is as follows:
A. carbomer gel preparation
0.4g carbomer 970 is dissolved in deionized water and obtains carbomer aqueous dispersions 29g, stir 2h, rear standing 2h.Under agitation in this carbomer dispersion liquid, adding 20g mass ratio is the ethylene glycol of 10:1 and the mixture of diethylene glycol ether, 30% polyethylene emulsion of 2.3g is added again in this solution, degassed after fully mixing at 40-45 DEG C, in 10min, the ammoniacal liquor adding 30% of 0.9g while stirring in this solution makes carbomer solution gelation;
B. thickening thixotroping matrix preparation
Be benzotriazole and the ethyl p-hydroxybenzoate of 1:1 by 0.5g mass ratio, Chemical Industry Science Co., Ltd is contained in 0.3gJS-5115(Qingdao nine) mix and stir, this mixed solution is joined in above-mentioned carbomer gel and stirs 10min, fully mix rear filtration and obtain 53g thickening thixotroping matrix;
C. Neutral writing ink preparation
The 53g carbomer thickening thixotroping matrix prepared slowly is added under agitation the blue mill base of particle diameter at 80-600nm of 15% of 47g, fully mix rear degassed, obtain 100g neutral blue ink.
Obtained neutral blue ink apparent viscosity, thixotropy index and capillary test data are as shown in table 1.
Comparative example 3
Comparative example 3 adopts the method as embodiment 3 to be prepared, and difference is, does not add rheology control agent in its formula.Concrete preparation method is as follows:
A. carbomer gel preparation
0.3g carbomer 2020 is dissolved in deionized water and obtains carbomer aqueous dispersions 25g, stir 2h, rear standing 2h.In this carbomer dispersion liquid, under agitation add the mixture of the glycerol that 30g mass ratio is 15:1 and diglycol ethylene butyl ether, the oligose of 3.6g maltose, sucrose and glucose polymerisation is added again in this solution, degassed after fully mixing at 40-45 DEG C, in 10min, 30% diethanolamine adding 0.6g while stirring in this solution makes carbomer solution gelation;
B. thickening thixotroping matrix preparation
Be the benzotriazole of 1:1 and ethyl p-hydroxybenzoate mixture, 0.2gSE-47(Shenzhen Haichuan Chemical Technology Co., Ltd by 0.6g mass ratio), mix and stir, this mixed solution is joined in above-mentioned carbomer gel and stirs 10min, fully mix rear filtration and obtain 60g thickening thixotroping matrix;
C. Neutral writing ink preparation
The 60g carbomer thickening thixotroping matrix prepared slowly is added under agitation the blue mill base of particle diameter at 80-600nm of 20% of 40g, fully mix rear degassed, obtain 100g neutral blue ink.
Obtained neutral blue ink apparent viscosity, thixotropy index and capillary test data are as shown in table 1.
The sample tests of embodiments of the invention and comparative example's gained is as shown in the table:
Table 1
Claims (9)
1. a neutral blue ink, is characterized in that, this neutral blue ink is made up of following component and mass percentage:
Blue mill base, 30%-50%; Carbomer, 0.3%-0.6%; Rheology control agent, 2%-8%; Lower alcohol, 15%-30%; Oligose, 1%-4%; Antisepticize and mildew preventive 0.4%-0.6%, pH adjusting agent 0.6%-1.7%, defoamer 0.2%-0.4%, all the other are deionized water, and the mass percentage sum of above-mentioned each component is 100%.
2. by neutral blue ink according to claim 1, it is characterized in that, blue mill base is at 80-600nm containing particle diameter, the CuPc microcapsule aqueous color paste that mass percentage forms at the CuPc microcapsule of 15%-45%, CuPc surface of microcapsule contains non-ionic hydrophilic group, and zeta current potential is 35-70mV.
3. by neutral blue ink according to claim 1, it is characterized in that, carbomer is carbomer series, is Acritamer 940, Acritamer 940 L, carbomer 2020, Carpobol 956 or carbomer 970.
4. by neutral blue ink according to claim 1, it is characterized in that, rheology control agent to be massfraction be 10% nano silicon, or for the massfraction formed by polyethylene, oxidic polyethylene or polypropylene be the nano-scale dispersion emulsion one wherein of 30%.
5. by neutral blue ink according to claim 1, it is characterized in that, lower alcohol is two or more the mixture in 1,2-PD, glycerol, sorbyl alcohol, ethylene glycol, ethylene glycol ethyl ether, diethylene glycol ether, butyl glycol ether and diglycol ethylene butyl ether.
6. by neutral blue ink according to claim 1, it is characterized in that, the oligopolymer that oligose is molecular-weight average one or both or three kinds of sugar polymerizations are formed in the maltose of 200-2000, sucrose, glucose.
7. by neutral blue ink according to claim 1, it is characterized in that, Antisepticize and mildew preventive is one or both in benzotriazole, mould inhibitor 253, AF251, ethyl p-hydroxybenzoate and methyl p-hydroxybenzoate; Defoamer is one or both in SE-47, SD-670 and JS-5115.
8., by neutral blue ink according to claim 1, it is characterized in that, pH adjusting agent is the one in ammoniacal liquor, sodium hydroxide, thanomin, diethanolamine and trolamine.
9. a preparation method for neutral blue ink, is characterized in that comprising following process:
Get carbomer aqueous dispersions 20-40 part that mass concentration is 1.07%-1.6% by mass, under agitation add the lower alcohol of 15-30 part wherein, the rheology control agent of 2-8 part, with 1-4 part oligose, degassed after fully mixing at 40-45 DEG C, 0.6-1.7 part pH adjusting agent is added while stirring in 10min, obtain carbomer gel, Antisepticize and mildew preventive 0.4-0.6 part is added again in this gel, defoamer 0.2-0.4 part, filter after stirring in 10min and obtain thickening thixotroping matrix, when stirring, the blue mill base of 30-50 part is slowly added again in this matrix, mix rear degassed, obtaining pH is 7-8, thixotropy index is the neutral blue ink of 4.0-7.
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| JPH0741714A (en) * | 1993-07-29 | 1995-02-10 | Shiyachihata Kogyo Kk | Oil-base ink |
| DE102004012479A1 (en) * | 2004-03-15 | 2005-10-06 | Dokumental Gmbh & Co. Schreibfarben | Non-aqueous polar ink composition |
| JP4468162B2 (en) * | 2004-12-28 | 2010-05-26 | 三菱鉛筆株式会社 | Water-based gel ink ballpoint pen |
| CN101100573B (en) * | 2007-08-03 | 2011-04-27 | 上海乐美文具有限公司 | Neutral ink and its preparation method |
| KR20120110565A (en) * | 2011-03-29 | 2012-10-10 | 하진경 | Ink for ball pen and ball pen |
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