CN104761926B - A kind of preparation method of acid ink-jet dye - Google Patents
A kind of preparation method of acid ink-jet dye Download PDFInfo
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- CN104761926B CN104761926B CN201510039260.4A CN201510039260A CN104761926B CN 104761926 B CN104761926 B CN 104761926B CN 201510039260 A CN201510039260 A CN 201510039260A CN 104761926 B CN104761926 B CN 104761926B
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Abstract
The present invention relates to the preparation method of acid stain.The preparation method of a kind of acid ink-jet dye, is first dissolved as the aqueous solution of 2 5% by dyestuff, through pressure filter coarse filtration, then filters through micropore filter element, removes the impurity in dye solution;Then carry out desalination with low salt reverse osmosis membrane, the chloride ion in dye solution and sulfate ion are controlled at below 200ppm, be then concentrated into 20 30% solid contents;Then the hydrochloric acid adding about 10 20% in dyestuff carries out acid out, the dyestuff of precipitation is pressed into filter cake through membrane pressure filter, obtain the acid stain filter cake of acid, this filter cake is pressed in pure water the concentration making beating of 2 3% again, and it is gradually added the organic base of respective amount, stirring heats up until dyestuff is completely dissolved, the pH regulator of dye solution is to 46 the most at last, filter through micropore filter element again, then with reverse osmosis membrane desalination to chloride ion and sulfate ion at below 100ppm, 20 30% solid contents finally it are concentrated into;Finally it is spray-dried and obtains ink-jet dye.
Description
Technical field
The present invention relates to the preparation method of acid stain, be specifically related to a kind of for digital ink-jet printed acid
The preparation method of property dyestuff.
Background technology
Along with development and the extension of inkjet technology, digital ink-jet printed the rapidest
Development, the performance requirement as ink-jet printed ink is more and more higher.And ink performance is risen decisive
Impact, be the quality of dyestuff, the quality of dyestuff directly determine ink-jet ink bin stability and
Spray printing fluency, this just proposes high requirement to ink-jet dye.
The dissolubility of acid stain is far short of what is expected for reactive dye, even if by the salinity in dyestuff
After heavy metals removal, its dissolubility does not the most obtain improvement substantially, and dyestuff is being configured to ink
After water, it is easy to separate out under conditions of low temperature, affect bin stability, have a strong impact on printing fluency,
Also can block shower nozzle, even damage printer.
The Chinese patent of Patent No. CN102618082A is mentioned with organic base quaternary ammonium cation replacing acid
Property dye solution in sodium ion, dissolubility and the bin stability of acid stain can be significantly improved, should
The substitution technique taked in patent is to be directly added into by organic base in the dye solution containing a large amount of sodium ion, then
It is intended to remove sodium ion by embrane method, and retains the organic base quaternary ammonium cation of addition simultaneously.But it is actual
If using such method upper, the exchange degree of dye solution cationic is difficult to improve to more than 70%,
This patent is not mentioned the actual exchange degree of dyestuff cationic yet.And the height of actual exchange degree is right
In improving acid stain dissolubility and stability, play conclusive effect.
Summary of the invention
It is an object of the invention to provide the preparation method of a kind of acid ink-jet dye, to solve above-mentioned technology
Problem.
Technical problem solved by the invention can realize by the following technical solutions:
The preparation method of a kind of acid ink-jet dye, it is characterised in that first dyestuff is dissolved as 2-5%'s
Aqueous solution, through pressure filter coarse filtration, then filters through micropore filter element, removes the impurity in dye solution;
Then carry out desalination, by the chloride ion in dye solution and sulfate radical with low salt reverse osmosis membrane
Ionic control, at below 200ppm, is then concentrated into the solid content of 20-30%;
Then the hydrochloric acid adding about 10-20% in dyestuff carries out acid out, by the dyestuff of precipitation through diaphragm type
Pressure filter is pressed into filter cake, obtains the acid stain filter cake of acid, then this filter cake is pressed in pure water 2-3%
Concentration making beating, and be gradually added the organic base of respective amount, stirring heats up until dyestuff is completely dissolved,
The pH regulator of dye solution is to 4-6 at last, then filters through micropore filter element, then uses reverse osmosis membrane desalination
To chloride ion and sulfate ion at below 100ppm, finally it is concentrated into 20-30% solid content;
Finally it is spray-dried and obtains ink-jet dye.
By the method, the cation exchange degree in acid stain solution can reach more than 90%.
Described pressure filter is plate and frame filter cloth pressure filter.Described membrane pressure filter is plate and frame membrane filter pressing
Machine.
The membrane material of described micropore filter element is polypropylene, politef, Kynoar, nylon or poly-
Ether sulfone material.The multistage filtering precision of described micropore filter element is divided into 50 microns, 10 microns, 1 micron and 0.2
Micron.
Described low salt reverse osmosis membrane is 10-50% for the rejection of sodium chloride, retains magnesium sulfate
Rate is 20-70%.Described desalination operating temperature is 30-65 DEG C, and pressure is 2.0~3.0Mpa.
Described organic base is diethanolamine, triethanolamine, tripropanol amine and isomer thereof.Described organic base is excellent
Elect diethanolamine as.
Described spray drying uses spray drying tower, and baking temperature controls as 110-195 DEG C.
Preferred version 1: Indian yellow 79 (C.I.Acid Yellow 79) structural formula is as follows:
In formula, M is H, Na, ethanolamine, diethanolamine or triethanolamine;
In 1000 parts of pure water, add 30 parts of Indian yellow 79 dry powder, be warming up to 65 DEG C, after dissolving completely,
Add 10 parts of kieselguhr to stir 30 minutes, filter pressing;Filtrate, through the filter element filtering of 10 microns, enters anti-
Permeable membrane system carries out desalting processing, temperature 45 C, and pressure 2.0Mpa, when chloride ion, sulfate ion
After concentration is respectively less than 200ppm (calculating by dyestuff powder body), being concentrated into solid content is 20%, is subsequently adding
100 parts of hydrochloric acid (10%), press dry through membrane pressure filter after separating out completely to dyestuff, obtain dyestuff filter-cakes
50 parts, then dyestuff filter-cakes is put into making beating dispersion in 1000 parts of pure water, it is warming up to 45 DEG C, adds 10
Part diethanolamine regulation pH to 4, until after dyestuff is completely dissolved, continuing desalination to chloride ion, sulfate radical
Ion concentration is respectively less than 100ppm (calculating by dyestuff powder body), continues to be concentrated into 120 parts, sprays
It is dried, obtains ink-jet dye 25 parts.
Preferred version 2: Xylene Red 52 (C.I.Acid Red 52)
In formula, M is H, Na, ethanolamine, diethanolamine or triethanolamine;
In 1000 parts of pure water, add 70 parts of Xylene Red 52 dry powder, be warming up to 40 DEG C, after dissolving completely,
Add 10 parts of kieselguhr to stir 30 minutes, filter pressing;Filtrate, through the filter element filtering of 10 microns, enters anti-
Permeable membrane system carries out desalting processing, temperature 35 DEG C, and pressure 2.0Mpa, when chloride ion, sulfate ion
After concentration is respectively less than 200ppm (calculating by dyestuff powder body), being concentrated into solid content is 20%, is subsequently adding
150 parts of hydrochloric acid (10%), press dry through membrane pressure filter after separating out completely to dyestuff, obtain dyestuff filter-cakes
100 parts, then dyestuff filter-cakes is put into making beating dispersion in 1000 parts of pure water, it is warming up to 30 DEG C, adds 20
Part diethanolamine regulation pH to 5.5, until after dyestuff is completely dissolved, continuing desalination to chloride ion, sulphuric acid
Ion concentration is respectively less than 100ppm (calculating by dyestuff powder body), continues to be concentrated into 200 parts, sprays
Mist is dried, and obtains ink-jet dye 50 parts.
Preferred version 3: acid blue 260 (C.I.Acid Blue 260)
In formula, M is H, Na, ethanolamine, diethanolamine or triethanolamine;
In 1000 parts of pure water, add 30 parts of acid blue 260 dry powder, be warming up to 60 DEG C, after dissolving completely,
Add 10 parts of kieselguhr to stir 30 minutes, filter pressing;Filtrate, through the filter element filtering of 10 microns, enters anti-
Permeable membrane system carries out desalting processing, temperature 40 DEG C, and pressure 2.0Mpa, when chloride ion, sulfate ion
After concentration is respectively less than 300ppm (calculating by dyestuff powder body), being concentrated into solid content is 16%, is subsequently adding
160 parts of hydrochloric acid (10%), press dry through membrane pressure filter after separating out completely to dyestuff, obtain dyestuff filter-cakes
50 parts, then dyestuff filter-cakes is put into making beating dispersion in 1000 parts of pure water, it is warming up to 40 DEG C, adds 8
Part diethanolamine regulation pH to 5, until after dyestuff is completely dissolved, continuing desalination to chloride ion, sulfate radical
Ion concentration is respectively less than 150ppm (calculating by dyestuff powder body), continues to be concentrated into 100 parts, sprays
It is dried, obtains ink-jet dye 20 parts.
Preferred version 4: acid black 1 94 (C.I.Acid Black 194)
In formula, M is H, Na, ethanolamine, diethanolamine or triethanolamine;
In 1000 parts of pure water, add 60 parts of acid black 1 94 dry powder, be warming up to 55 DEG C, after dissolving completely,
Add 10 parts of kieselguhr to stir 30 minutes, filter pressing;Filtrate, through the filter element filtering of 10 microns, enters anti-
Permeable membrane system carries out desalting processing, temperature 45 C, and pressure 2.0Mpa, when chloride ion, sulfate ion
After concentration is respectively less than 200ppm (calculating by dyestuff powder body), being concentrated into solid content is 20%, is subsequently adding
13 parts of hydrochloric acid (10%), press dry through membrane pressure filter after separating out completely to dyestuff, obtain dyestuff filter-cakes 95
Part, then dyestuff filter-cakes is put into making beating dispersion in 1000 parts of pure water, it is warming up to 40 DEG C, adds 15 parts
Diethanolamine regulation pH to 4.5, until after dyestuff is completely dissolved, continuing desalination to chloride ion, sulfate radical
Ion concentration is respectively less than 100ppm (calculating by dyestuff powder body), continues to be concentrated into 180 parts, sprays
It is dried, obtains ink-jet dye 50 parts.
Detailed description of the invention
For the technological means making the present invention realize, creation characteristic, reach purpose and effect and be readily apparent from
Solve, the present invention is further elucidated below.
The preparation method of a kind of acid ink-jet dye, is first dissolved as dyestuff the aqueous solution of 2-5%, passes through
Pressure filter coarse filtration, then filter through micropore filter element, remove the impurity in dye solution;Then use low desalination
The reverse osmosis membrane of property carries out desalination, controls the chloride ion in dye solution and sulfate ion at 200ppm
Hereinafter, 20-30% solid content then it is concentrated into;Then the hydrochloric acid adding about 10-20% in dyestuff carries out acid
Analysis, is pressed into filter cake by the dyestuff of precipitation through membrane pressure filter, obtains the acid stain filter cake of acid,
The concentration that this filter cake is pressed in pure water 2-3% again is pulled an oar, and is gradually added the organic base of respective amount, stirring
Heating up until dyestuff is completely dissolved, the pH regulator of dye solution is to 4-6 the most at last, then through micropore filter element
Filter, then with reverse osmosis membrane desalination to chloride ion and sulfate ion at below 100ppm, finally concentrate
To 20-30% content;Finally it is spray-dried and obtains ink-jet dye.
Described pressure filter is plate and frame filter cloth pressure filter;Described membrane pressure filter is plate and frame membrane filter pressing
Machine;The membrane material of described micropore filter element is polypropylene, politef, Kynoar, nylon or poly-
Ether sulfone material;The multistage filtering precision of described micropore filter element is divided into 50 microns, 10 microns, 1 micron and 0.2
Micron;Described low salt reverse osmosis membrane is 10-50% for the rejection of sodium chloride, cuts magnesium sulfate
Staying rate is 20-70%;Described desalination operating temperature is 30-65 DEG C, and pressure is 2.0~3.0Mpa;Described have
Machine alkali is diethanolamine, triethanolamine, tripropanol amine and isomer thereof;Described organic base is preferably diethyl
Hydramine;Described spray drying uses spray drying tower, and baking temperature controls as 110-195 DEG C.
Detailed description of the invention
Embodiment 1: Indian yellow 79 (C.I.Acid Yellow 79) structural formula is as follows:
In formula, M is H, Na, ethanolamine, diethanolamine or triethanolamine;
In 1000 parts of pure water, add 30 parts of Indian yellow 79 dry powder, be warming up to 65 DEG C, after dissolving completely,
Add 10 parts of kieselguhr to stir 30 minutes, filter pressing;Filtrate, through the filter element filtering of 10 microns, enters anti-
Permeable membrane system carries out desalting processing, temperature 45 C, and pressure 2.0Mpa, when chloride ion, sulfate ion
After concentration is respectively less than 200ppm (calculating by dyestuff powder body), being concentrated into solid content is 20%, is subsequently adding
100 parts of hydrochloric acid (10%), press dry through membrane pressure filter after separating out completely to dyestuff, obtain dyestuff filter-cakes
50 parts, then dyestuff filter-cakes is put into making beating dispersion in 1000 parts of pure water, it is warming up to 45 DEG C, adds 10
Part diethanolamine regulation pH to 4, until after dyestuff is completely dissolved, continuing desalination to chloride ion, sulfate radical
Ion concentration is respectively less than 100ppm (calculating by dyestuff powder body), continues to be concentrated into 120 parts, sprays
It is dried, obtains ink-jet dye 25 parts.
Embodiment 2: Xylene Red 52 (C.I.Acid Red 52)
In formula, M is H, Na, ethanolamine, diethanolamine or triethanolamine;
In 1000 parts of pure water, add 70 parts of Xylene Red 52 dry powder, be warming up to 40 DEG C, after dissolving completely,
Add 10 parts of kieselguhr to stir 30 minutes, filter pressing;Filtrate, through the filter element filtering of 10 microns, enters anti-
Permeable membrane system carries out desalting processing, temperature 35 DEG C, and pressure 2.0Mpa, when chloride ion, sulfate ion
After concentration is respectively less than 200ppm (calculating by dyestuff powder body), being concentrated into solid content is 20%, is subsequently adding
150 parts of hydrochloric acid (10%), press dry through membrane pressure filter after separating out completely to dyestuff, obtain dyestuff filter-cakes
100 parts, then dyestuff filter-cakes is put into making beating dispersion in 1000 parts of pure water, it is warming up to 30 DEG C, adds 20
Part diethanolamine regulation pH to 5.5, until after dyestuff is completely dissolved, continuing desalination to chloride ion, sulphuric acid
Ion concentration is respectively less than 100ppm (calculating by dyestuff powder body), continues to be concentrated into 200 parts, sprays
Mist is dried, and obtains ink-jet dye 50 parts.
Embodiment 3: acid blue 260 (C.I.Acid Blue 260)
In formula, M is H, Na, ethanolamine, diethanolamine or triethanolamine;
In 1000 parts of pure water, add 30 parts of acid blue 260 dry powder, be warming up to 60 DEG C, after dissolving completely,
Add 10 parts of kieselguhr to stir 30 minutes, filter pressing;Filtrate, through the filter element filtering of 10 microns, enters anti-
Permeable membrane system carries out desalting processing, temperature 40 DEG C, and pressure 2.0Mpa, when chloride ion, sulfate ion
After concentration is respectively less than 300ppm (calculating by dyestuff powder body), being concentrated into solid content is 16%, is subsequently adding
160 parts of hydrochloric acid (10%), press dry through membrane pressure filter after separating out completely to dyestuff, obtain dyestuff filter-cakes
50 parts, then dyestuff filter-cakes is put into making beating dispersion in 1000 parts of pure water, it is warming up to 40 DEG C, adds 8
Part diethanolamine regulation pH to 5, until after dyestuff is completely dissolved, continuing desalination to chloride ion, sulfate radical
Ion concentration is respectively less than 150ppm (calculating by dyestuff powder body), continues to be concentrated into 100 parts, sprays
It is dried, obtains ink-jet dye 20 parts.
Embodiment 4: acid black 1 94 (C.I.Acid Black 194)
In formula, M is H, Na, ethanolamine, diethanolamine or triethanolamine;
In 1000 parts of pure water, add 60 parts of acid black 1 94 dry powder, be warming up to 55 DEG C, after dissolving completely,
Add 10 parts of kieselguhr to stir 30 minutes, filter pressing;Filtrate, through the filter element filtering of 10 microns, enters anti-
Permeable membrane system carries out desalting processing, temperature 45 C, and pressure 2.0Mpa, when chloride ion, sulfate ion
After concentration is respectively less than 200ppm (calculating by dyestuff powder body), being concentrated into solid content is 20%, is subsequently adding
13 parts of hydrochloric acid (10%), press dry through membrane pressure filter after separating out completely to dyestuff, obtain dyestuff filter-cakes 95
Part, then dyestuff filter-cakes is put into making beating dispersion in 1000 parts of pure water, it is warming up to 40 DEG C, adds 15 parts
Diethanolamine regulation pH to 4.5, until after dyestuff is completely dissolved, continuing desalination to chloride ion, sulfate radical
Ion concentration is respectively less than 100ppm (calculating by dyestuff powder body), continues to be concentrated into 180 parts, sprays
It is dried, obtains ink-jet dye 50 parts.
The cation exchange degree of table 1 distinct methods and impact thereof
Note: 1, method one is the method for this patent, method two is the method for patent CN102618082A;
2, the content during Na content is dyestuff dry powder in table;
3, observe after liquid dyes low-temperature stability is 0-5 DEG C of cold preservation 7 days;
From the experimental result of table 1, this method can make the exchange degree of dyestuff cationic improve to 90%
Above, and higher exchange degree can be greatly improved dyestuff dissolubility in water and low-temperature stability.
The ultimate principle of the present invention and principal character and advantages of the present invention have more than been shown and described.This
Skilled person will appreciate that of industry, the present invention is not restricted to the described embodiments, above-described embodiment and saying
The principle that the present invention is simply described described in bright book, without departing from the spirit and scope of the present invention,
The present invention also has various changes and modifications, and these changes and improvements both fall within claimed invention model
In enclosing.Claimed scope is defined by appending claims and equivalent thereof.
Claims (10)
1. the preparation method of an acid ink-jet dye, it is characterised in that first dyestuff is dissolved as 2-5%
Aqueous solution, through pressure filter coarse filtration, then filter through micropore filter element, remove the impurity in dye solution;
Then carry out desalination, by the chloride ion in dye solution and sulfate radical with low salt reverse osmosis membrane
Ionic control, at below 200ppm, is then concentrated into 20-30% solid content;
Then the hydrochloric acid adding 10-20% in dyestuff carries out acid out, by the dyestuff of precipitation through diaphragm type pressure
Filter is pressed into filter cake, obtains the acid stain filter cake of acid, then this filter cake is pressed in pure water 2-3%'s
Concentration is pulled an oar, and is gradually added the organic base of respective amount, and stirring heats up until dyestuff is completely dissolved, finally
By the pH regulator of dye solution to 5-7.5, then filter through micropore filter element, then use reverse osmosis membrane desalination
To chloride ion and sulfate ion at below 100ppm, finally it is concentrated into 20-30% content;
Finally it is spray-dried and obtains ink-jet dye.
The preparation method of a kind of acid ink-jet dye the most according to claim 1, it is characterised in that: institute
Stating pressure filter is plate and frame filter cloth pressure filter.
The preparation method of a kind of acid ink-jet dye the most according to claim 1, it is characterised in that: institute
Stating membrane pressure filter is plate and frame diaphragm filter press.
The preparation method of a kind of acid ink-jet dye the most according to claim 1, it is characterised in that: institute
The membrane material stating micropore filter element is polypropylene, politef, Kynoar, nylon or polyether sulfone material
Matter.
The preparation method of a kind of acid ink-jet dye the most according to claim 1, it is characterised in that: institute
The multistage filtering precision stating micropore filter element is divided into 50 microns, 10 microns, 1 micron and 0.2 micron.
The preparation method of a kind of acid ink-jet dye the most according to claim 1, it is characterised in that: institute
Stating low salt reverse osmosis membrane for the rejection of sodium chloride is 10-50%, to the rejection of magnesium sulfate is
20-70%.
The preparation method of a kind of acid ink-jet dye the most according to claim 1, it is characterised in that: institute
Stating desalination operating temperature and be 30-65 DEG C, pressure is 2.0~3.0Mpa.
The preparation method of a kind of acid ink-jet dye the most according to claim 1, it is characterised in that: institute
Stating organic base is diethanolamine, triethanolamine, tripropanol amine and isomer thereof.
The preparation method of a kind of acid ink-jet dye the most according to claim 1, it is characterised in that: institute
Stating spray drying and use spray drying tower, baking temperature controls as 110-195 DEG C.
The preparation method of a kind of acid ink-jet dye the most according to claim 1, it is characterised in that: described
Dyestuff is Indian yellow 79 (C.I.Acid Yellow 79)
In formula, M is Na;
Xylene Red 52 (C.I.Acid Red 52)
In formula, M is Na;
Acid blue 260 (C.I.Acid Blue 260)
In formula, M is Na;
Or, acid black 1 94 (C.I.Acid Black 194)
In formula, M is Na.
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JP4466987B2 (en) * | 2001-05-09 | 2010-05-26 | 日本化薬株式会社 | Anthrapyridone compound, aqueous magenta ink composition, and ink jet recording method |
CN102618082B (en) * | 2012-03-16 | 2014-03-12 | 金华双宏化工有限公司 | Method for preparing water-soluble ink jet dye |
CN102942808A (en) * | 2012-08-03 | 2013-02-27 | 上海色如丹染料化工有限公司 | Liquid dye desalination purification preparation method |
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