CN105214603B - A kind of preparation method of ink-jet printing media compound adsorbent - Google Patents
A kind of preparation method of ink-jet printing media compound adsorbent Download PDFInfo
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Abstract
The invention belongs to ink-jet printing media absorbent fields.A kind of preparation method of ink-jet printing media compound adsorbent, it is comprised the following steps：(1) liquid is matched somebody with somebody：Sodium silicate aqueous solution, aluminum sulfate solution（2）Reaction；（3）Polyol is added, is crushed（4）Cocurrent（5）Heating（6）Washing（7）Mashing（8）Dry, obtain finished product.Present invention process is simple, raw material is cheap, and finished product is not only with the big advantage of silica adsorbance but also with the oil loving feature of aluminum oxide, and the image color that prints is gorgeous, saturation degree is high, glossiness is good, has higher stereovision.
Description
Technical field
The invention belongs to inkjet technology field, specifically a kind of preparation side of color inkjet printing medium adsorbent
Method.
Technical background
The critical material of color ink jet printer paper is that one layer of porous type with absorbency coated in paper surface adsorbs
Agent, its absorption and infiltration to ink on paper, and printing density, colour gamut, lines acutance etc. important.
The development of color ink jet printing and ink-jet printing ink is closely bound up, and marking ink includes dye ink and paint ink.
Dye ink has the advantage that vividness is high, color rendition degree is high, but photostability and water proofing property are poor, and paint ink light is stable
Property and water proofing property are poor, but it has the defects of thick granularity, color rendition degree difference.Exploitation all has to dye ink and paint ink
The adsorbent for having preferable absorption property is developing direction.
Ink-jet printing media adsorbent mainly includes two kinds of silicon systems and aluminium system.Simple silica adsorbent is due to surface
Abundant hydroxyl is its advantage for water-based dye ink absorption, but because lipophile difference is poor for paint ink adsorptivity.
Oxidation aluminium surface is organophilic, there is stronger adsorptivity for pigment, but current nano aluminium oxide largely relies on import,
It is expensive, hinder it and further apply.
Chinese patent CN101570338B is disclosed with the composition of raw materials of high ink absorption nano-alumina and preparation side
Method, the nano aluminium oxide with high ink absorption is made, but its raw material organo-aluminium used is expensive.
The content of the invention
It is both big with silica adsorbance it is an object of the invention to provide a kind of ink-jet printing media compound adsorbent
Advantage there is the oil loving feature of aluminum oxide again so that the image color reduction degree of printing is high, stereovision is strong, it is stronger to have
Sun-proof and water-fast function.
A kind of preparation method of ink-jet printing media compound adsorbent, it is comprised the following steps：
(1) sodium metasilicate is configured to A grams of the sodium silicate aqueous solution of the 5-10%wt in terms of silica, weighs 18 water sulfuric acid
B grams of aluminium, water is added to be configured to the aluminum sulfate solution that alumina content is 5-10%wt, wherein silica：Aluminum oxide=(3-9)：
1, sulfuric acid adds water to be configured to 10-20%wt aqueous sulfuric acid, and ammoniacal liquor is configured to 10-20%wt ammonia spirit；
(2) A grams of sodium silicate aqueous solution is added into reactor, starts stirring, at normal temperatures, added and walked with 50-100ml/min
Suddenly the aqueous sulfuric acid that (1) prepares stirs 30-40 minutes, adds aqueous sulfuric acid adjustment PH7-8, be warming up to PH8-9
80-90 DEG C, it is incubated 1-2 hours；
(3) by step (2) slurry, 30-40 DEG C is cooled to, adds polyol, its dosage is the 1- of silica
3%wt, silica is crushed to 40-50nm using grinder, polyol include glycerine, propane diols one kind or
Two kinds；
(4) aluminum sulfate solution while the addition of cocurrent equivalent that step (1) is prepared are added with 100-120ml/min speed
The ammonia spirit that step (1) is prepared, keep bottom liquid PH7-8 constant；
(5) slurry of step (4) is warming up to 60-65 DEG C, is incubated 3-4 hours；
(6) slurry of step (5) is washed, below the μ s/cm of wash water electrical conductivity 100 obtain silicoaluminate (butt)
C grams；
(7) filter cake after step (6) is washed is added beater and is carried out being beaten while adding nano-calcium carbonate with 2500 revs/min
Calcium carries out surface modification, and its addition is silicoaluminate (butt) 3-5%wt, adds water to adjust solid content 20-25%wt, mashing
40-60 minutes；
(8) n-butanol is added to step (7) slurry, moisture is removed using azeotropic distillation, and done under nitrogen protection
It is dry, obtain finished product；
Present invention process is simple, raw material is cheap, and finished product is not only with the big advantage of silica adsorbance but also with aluminum oxide
Oil loving feature, the image color that prints is gorgeous, saturation degree is high, glossiness is good, has higher stereovision.
Embodiment
With reference to embodiment, the present invention is described further.
Embodiment one
(1) sodium metasilicate is configured to 1000 grams of the sodium silicate aqueous solution of the 5%wt in terms of silica, weighs 18 water sulfuric acid
108 grams of aluminium, water is added to be configured to 165.24 grams of the aluminum sulfate solution that alumina content is 10%wt, sulfuric acid adds water to be configured to 10%wt
Aqueous sulfuric acid, ammoniacal liquor is configured to 10%wt ammonia spirit；
(2) 1000 grams of 5%wt sodium silicate aqueous solutions are added into reactors, start stirring, at normal temperatures, with 50ml/min plus
Entering aqueous sulfuric acid to PH8-9, the stirring 30-40 minutes that step (1) prepares forms colloidal sol, adds aqueous sulfuric acid and adjusts
PH7-8. 80 DEG C are warming up to, is incubated 1 hour；
(3) by step (2) slurry, 30-40 DEG C is cooled to, adds more 0.5 gram of glycerine, using grinder by silica
To 40-50nm；
(4) 165.24 grams of aluminum sulfate solution for adding step (1) preparation with 100ml/min speed into step (3) is same
The ammonia spirit that Shi Bingliu equivalents add, keep bottom liquid PH7-8 constant；
(5) slurry of step (4) is warming up to 60 DEG C, is incubated 3 hours；
(6) slurry of step (5) is washed, below the μ s/cm of wash water electrical conductivity 100 obtain silicoaluminate (butt)
56.5 grams；
(7) filter cake after step (6) is washed is added beater and is carried out being beaten while adding 2 grams of nanometers with 2500 revs/min
Calcium carbonate, it is 20%wt to add water adjustment solid content, is beaten 40 minutes；
(8) add n-butanol to step (7) slurry and use azeotropic distillation, remove moisture, and done under nitrogen protection
It is dry, obtain finished product.
Embodiment two
(1) sodium metasilicate is configured to 1000 grams of the sodium silicate aqueous solution of the 10%wt in terms of silica, weighs 18 water sulphur
Sour 218 grams of aluminium, it is 333.33 grams of 10wt% aluminum sulfate solutions to add water to be assigned into alumina content, and sulfuric acid adds water to be configured to 15%wt
Aqueous sulfuric acid, ammoniacal liquor is configured to 10%wt ammonia spirit；
(2) 1000 grams of 10%wt sodium silicate aqueous solutions are added into reactor, stirring is started, at normal temperatures, with 75ml/min
Add aqueous sulfuric acid to PH8-9, the stirring that step (1) prepares and form colloidal sol in 30 minutes, add aqueous sulfuric acid adjustment
PH7-8. 85 DEG C are warming up to, is incubated 1 hour；
(3) by step (2) slurry, 30 DEG C are cooled to, adds 2 grams of propane diols, using grinder by silica to 40-
50nm；
(4) the 333.33 grams of solution of aluminum sulfate for adding step (1) preparation with 100ml/min speed into step (3) are same
Shi Bingliu equivalents add the ammonia spirit that step (1) is prepared, and keep bottom liquid PH7-8 constant；
(5) slurry of step (4) is warming up to 60-65 DEG C, is incubated 3-4 hours；
(6) slurry of step (5) is washed, below the μ s/cm of wash water electrical conductivity 100 obtain silicoaluminate (butt)
133 grams；
(7) filter cake after step (6) is washed is added beater and is carried out being beaten while adding nano-calcium carbonate with 2500 revs/min
6 grams of calcium, adjustment solid content 20% is added, is beaten 40-60 minutes；
(8) add n-butanol to step (7) slurry and use azeotropic distillation, remove moisture, and done under nitrogen protection
It is dry, obtain finished product.
Embodiment three
(1) sodium metasilicate is configured to 1000 grams of the sodium silicate aqueous solution of the 10%wt in terms of silica, weighs 18 water sulphur
Sour 72 grams of aluminium, it is 220.32 grams of 5%wt aluminum sulfate solutions to add water to be assigned into alumina content, and sulfuric acid adds water to be configured to 20%wt's
Aqueous sulfuric acid, ammoniacal liquor are configured to 20%wt ammonia spirit；
(2) 1000 grams of 10%wt sodium silicate aqueous solutions are added into reactor, stirring is started, at normal temperatures, with 100ml/min
Add aqueous sulfuric acid to PH8-9, the stirring that step (1) prepares and form colloidal sol in 30 minutes, add aqueous sulfuric acid adjustment
PH7-8. 85 DEG C are warming up to, is incubated 1 hour；
(3) by step (2) slurry, 30 DEG C are cooled to, adds 3 grams of propane diols, using grinder by silica to 40nm；
(4) 220.32 grams of aluminum sulfate solution for adding step (1) preparation with 150ml/min speed into step (3) is same
Shi Bingliu equivalents add the ammonia spirit that step (1) is prepared, and keep bottom liquid PH7-8 constant；
(5) slurry of step (4) is warming up to 65 DEG C, is incubated 4 hours；
(6) slurry of step (5) is washed, below the μ s/cm of wash water electrical conductivity 100 obtain silicoaluminate (butt)
111 grams；
(7) filter cake after step (6) is washed is added beater and is carried out being beaten while adding nano-calcium carbonate with 2500 revs/min
4.5 grams of calcium, adjustment solid content 20% is added, is beaten 50 minutes；
(8) add n-butanol to step (7) slurry and use azeotropic distillation, remove moisture, and done under nitrogen protection
It is dry, obtain finished product；
Example IV
(1) sodium metasilicate is configured to 2000 grams of the sodium silicate aqueous solution of the 8%wt in terms of silica, weighs 18 water sulfuric acid
209 grams of aluminium, it is 640 grams of 5wt% aluminum sulfate solutions to add water to be configured to alumina content, and sulfuric acid adds water to be configured to 10-20%wt's
Aqueous sulfuric acid, ammoniacal liquor are configured to 10-20%wt ammonia spirit；
(2) 2000 grams of 8%wt sodium silicate aqueous solutions are added into reactors, start stirring, at normal temperatures, with 50ml/min plus
Enter aqueous sulfuric acid to PH8-9, the stirring that step (1) prepares and form colloidal sol in 40 minutes, add aqueous sulfuric acid adjustment PH7-
8. being warming up to 80-90 DEG C, 1-2 hours are incubated；
(3) by step (2) slurry, be cooled to 30-40 DEG C, add 4.8 grams of glycerine, using grinder by silica extremely
40-50nm；
(4) 640 grams of aqueous solution of aluminum sulfate of step (1) preparation are added simultaneously with 120ml/min speed into step (3)
Cocurrent equivalent adds the ammonia spirit that step (1) is prepared, and keeps bottom liquid PH7-8 constant；
(5) slurry of step (4) is warming up to 60-65 DEG C, is incubated 3-4 hours；
(6) slurry of step (5) is washed, below the μ s/cm of wash water electrical conductivity 100 obtain silicoaluminate (butt)
192 grams；
(7) filter cake after step (6) is washed is added beater and is carried out being beaten while adding 9 grams of nanometers with 2500 revs/min
Calcium carbonate, add water to adjust solid content 25%wt, be beaten 60 minutes；
(8) add n-butanol to step (7) slurry and use azeotropic distillation, remove moisture, and done under nitrogen protection
It is dry, obtain finished product.
Performance test
The measure of pore volume specific surface area is measured using BET nitrogen adsorptions, and the pore property of test specimen is：Pore volume 2.0-
2.2ml/g, specific surface area 200-250m2/g
| Embodiment | Pore volume ml/g | Specific surface area m2/g |
| 1 | 2.05 | 230 |
| 2 | 2.18 | 220 |
| 3 | 2.15 | 231 |
| 4 | 2.18 | 243 |
Application performance determines
The absorption property of the present invention is measured in the following way：
Application process, prepare pre-coating solution:
50g deionized waters are taken, add the adsorbent that 15g is obtained by preparation method of the present invention, stir 30min, 20g is added and gathers
Glycohol solution (solid content：9%), continue to stir 30min, stand defoaming, above-mentioned coating liquid is applied on RC paper substrates, 50 DEG C
Drying.
Method of testing：Print performance is tested：Ink-jet printing media obtained by the embodiment of the present invention, uses Epson respectively
STYLUS R800 (pigment inks) and Epson STYLUS R230 (dye ink), carry out print performance test.For evaluation printing property
Can, ink absorption, printing color density, printing water proofing property are evaluated respectively.
1st, ink absorption：Epson STYLUS R800 (pigment inks) and Epson STYLUS R230 (dyestuffs are used respectively
Ink) printing test figure, ink setting effect is observed, evaluation criterion is as follows：
It is excellent：Immediately dry, just print, be wiped repeatedly, white cotton balls does not have ink blok；
In：Place 5~10s to dry, be wiped repeatedly, white cotton balls does not have ink blok；
Difference：Dry, be wiped repeatedly, white cotton balls does not have ink blok after placing 10s.
2nd, color density is printed：Epson STYLUS R800 (pigment inks) and Epson STYLUS R230 (dyestuffs are used respectively
Ink) black (K), blue or green (C), fuchsin (M), yellow (Y), red (R), green (G), blue (B) seven color lump are printed, it is divided light using SpectroEye
Spend instrument measurement reflection of monochromatic light density.
3rd, water proofing property is printed：Printed using Epson STYLUS R230, bath test was carried out in 30 seconds.First will drop
Water receptacle drips runoff investigation to 3 drops/sec, and the medium after printing color lump then is put in into water drenching 50 seconds under drip container in 60 °,
After taking-up is dried, visual assessment surface degree, evaluation criterion is as follows：
It is excellent：The substantially inkless current of color lump lose；
It is good：Only black is slightly lost in, and other color lumps are substantially without loss；
Difference：Color lump ink is lost in heavier.
| Ink absorption | Color density | Water proofing property | |
| Embodiment 1 | It is excellent | 2.02 | It is excellent |
| Embodiment 2 | It is excellent | 1.98 | It is excellent |
| Embodiment 3 | It is excellent | 2.05 | It is excellent |
| Embodiment 4 | It is excellent | 1.99 | It is excellent |
Claims (1)
1. a kind of preparation method of ink-jet printing media compound adsorbent, it is comprised the following steps：
（1）Sodium metasilicate is configured to the sodium silicate aqueous solution of the 5-10wt% in terms of silica, aluminum sulfate octadecahydrate is weighed and adds water to match somebody with somebody
The aluminum sulfate solution that alumina content is 5-10wt%, wherein silica is made：Aluminum oxide=（3-9）：1, sulfuric acid adds water to prepare
Into 10-20wt% aqueous sulfuric acid, ammoniacal liquor is configured to 10-20wt% ammonia spirit；
（2）Sodium silicate aqueous solution is added into reactor, starts stirring, at normal temperatures, it is water-soluble that sulfuric acid is added with 50-100ml/min
Liquid stirs 30-40 minutes, adds aqueous sulfuric acid adjustment pH7-8, be warming up to 80-90 DEG C, be incubated 1-2 hours to pH8-9；
（3）30-40 DEG C is cooled to, adds polyol, its dosage is the 1-3wt% of silica, and silica is crushed
To 40-50nm；
Polyol is glycerine and/or propane diols;
（4）Aluminum sulfate solution cocurrent equivalent ammonia spirit simultaneously is added with 100-120ml/min speed, keeps bottom liquid pH7-
8 is constant；
（5）60-65 DEG C is warming up to, is incubated 3-4 hours；
（6）Washing, below the μ s/cm of wash water electrical conductivity 100；
（7）By step（6）Filter cake after washing is added beater and is beaten with 2500 revs/min, while adds silicoaluminate
Butt 3-5wt% nano-calcium carbonate, add water to adjust solid content 20-25wt%, be beaten 40-60 minutes；
（8）To step（7）Slurry adds n-butanol, and moisture is removed using azeotropic distillation, and is dried under nitrogen protection, obtains
To finished product.
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| CN1344764A (en) * | 2000-09-30 | 2002-04-17 | 德古萨公司 | Adulterated precipitated silicate |
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