CN107502063A

CN107502063A - A kind of preparation method of composite water soluble ink jet ink for printing

Info

Publication number: CN107502063A
Application number: CN201710774142.7A
Authority: CN
Inventors: 张欢
Original assignee: Chengdu Qi Fang Biotechnology Co Ltd
Current assignee: Chengdu Qi Fang Biotechnology Co Ltd
Priority date: 2017-08-31
Filing date: 2017-08-31
Publication date: 2017-12-22

Abstract

The invention discloses a kind of preparation method of composite water soluble ink jet ink for printing, including step once：It is first according to mass fraction and calculates take 3 5% water-soluble dye, 15 25% organic solvent, 0.8 1.5% trialkyl phosphates, 0.5 1.5% potassium dihydrogen phosphate, 0.2 0.4% diethylene-triamine pentaacetic acid and 70 85% deionized water and be used as the raw material of composite water soluble ink and individually placed standby；Then ready water-soluble dye and organic solvent are put into stirred tank and stirred, it is mixed for solvent orange 2 A；Trialkyl phosphates are added respectively into the solvent orange 2 A to have stirred and diethylene-triamine pentaacetic acid is stirred for, and the rear potassium dihydrogen phosphate that adds adjusts its pH value formation solvent B；Slowly filling deionized water and stirring are to obtain ink crude product in most backward solvent B；The processing of obtained ink crude product high frequency ultrasound is carried out into multiple times of filtration again to finally give ink product and encapsulate preservation.The method of the present invention can effectively improve the production efficiency of the water-base ink, and improve ink quality and performance.

Description

A kind of preparation method of composite water soluble ink jet ink for printing

Technical field

The present invention relates to a kind of preparation method of composite water soluble ink jet ink for printing.

Background technology

With the popularization of computer applications, colour print market becomes increasingly prosperous.Especially color inkjet printer, it can be carried The figure of high quality is printed for the text printing and can of high quality.In recent years, color inkjet printer is swashed with it close to colored The print quality of optical printer and be only the part of color laser printer ten low price, and increasingly by user's Favor, is particularly subject to the welcome of domestic consumer.

But its supporting ink-jet printing ink, it is still unsatisfactory at present in performance and price.From price See, several special print cartridges are equivalent to the price of a low-end ink jet printer；From it is fast light, water-fast, save-resistant angularly, mesh The preceding type of dye ink used, even if the expensive special-purpose ink that factory is supporting, it can not meet to require.Therefore, state The interior development to ink-jet printing ink, substantial amounts of work has been done in recent years.But a kind of ink product is set to meet not in performance The same requirement even to differ greatly, and it is cheap, it is difficult to.The demand of user should be carried out appropriate thin Point, meet the needs of user from multiple directions.

The content of the invention

For the problem of ink for printing performance indications are poor in the prior art, impurity is more and manufacturing cost is higher, this hair Bright offer is a kind of by that can improve the composite water soluble ink jet ink for printing of existing ink performance added with special additive Preparation method.

The present invention is achieved through the following technical solutions：A kind of preparation method of composite water soluble ink jet ink for printing, including Step once：

S1. it is first according to mass fraction calculating and takes 3-5% water-soluble dye, 15-25% organic solvent, 0.8- 1.5% trialkyl phosphates, 0.5-1.5% potassium dihydrogen phosphate, 0.2-0.4% diethylene-triamine pentaacetic acid and 70- 85% deionized water is used as the raw material of composite water soluble ink and individually placed standby；

S2. and then ready water-soluble dye and organic solvent are put into and 45-70 DEG C of temperature is heated in stirred tank In the range of stir 10-15min, it is mixed for solvent orange 2 A；

S3. trialkyl phosphates and diethylene-triamine pentaacetic acid are added respectively into the solvent orange 2 A to have stirred, often It must be kept stirring for when adding a kind of additive, then it is stirred for adding potassium dihydrogen phosphate after 5-10min adjusts its pH value and formed Solvent B；

S4. deionized water is slowly filled in most backward solvent B and stirs 20-30min and obtains ink crude product；

S5. obtained ink crude product is placed in ultrasonic processing equipment and 120- is handled with 1040kHz high frequency ultrasounds 180h, then detect its indices；

S6. the ink crude product after being ultrasonically treated carries out multiple times of filtration and finally gives ink product and encapsulate guarantor Deposit.

Further, described organic solvent is the mixture of glycerine and tetrahydrofuran, glycerine and tetrahydrofuran it is mixed Composition and division in a proportion is 4：3.

Further, in step sl with mass fraction than 4：3 take glycerine and tetrahydrofuran is put into stirred tank and carried out Mixing 10-15min makes it mix to obtain organic solvent and deposited standby.

Further, the step S6 is comprised the following steps that：

S61. filter plant is ready to first, the filter plant includes standing pond, multi-layer filter paper filter and poly- four PVF filter cloth filtering machine；

S62. the ink crude product after being ultrasonically treated, which is passed through to stand, carries out cooling and standings precipitation in pond, during standing A length of 30-50min；

S63. and then by the ink crude product stood in pond multi-bed filter and polytetrafluoroethylene (PTFE) filter-cloth filtering are passed through successively Filtered in machine, by the small particle contaminant filter in ink crude product；

S64. the ink product most come out at last from polytetrafluoroethylene (PTFE) filter cloth filtering machine is stored in macromolecule storage barrel Row storage.

Further, 5-7 layer polypropylene cotton filter layers, the polytetrafluoroethylene (PTFE) filter-cloth filtering are provided with the multi-bed filter 3-5 strata tetrafluoroethene filter clothes are provided with machine.

Ink has a variety of sorting techniques, wherein can be divided into water-based and organic solvent type according to type of solvent, and it is of the invention It is a kind of water-based ink-jet printing ink, then its dyestuff used adds ionized water as solvent for water-soluble dye, appropriate to increase Some organic solvents are added to improve compatible degree, and described organic solvent is a kind of hydrophilic organic solvent, can be dissolved in water In.Requirement of the ink-jet printing ink on print performance mainly has:Image clearly, color are true to nature, have well water-fast, fast light Fastness and optical density, rate of drying is fast, be not easy to stain, is not easy to be formed that duricrust, storage ability are good, should in spray nozzle front end There are chemical change or precipitation generation etc..And surfactant, buffer and the diethylene-triamine pentaacetic acid added in the present invention It is the additive for improving the indices of ink.

Wherein, described surfactant refers to add can make the interface state of its solution system that significant change occur on a small quantity Material.With fixed hydrophilic lipophilic group, aligned in the surface energy of solution.The molecular structure of surfactant has It is amphipathic：One end is hydrophilic radical, and the other end is hydrophobic grouping；Hydrophilic radical is often polar group, as carboxylic acid, sulfonic acid, sulfuric acid, Amino or amido and its salt, hydroxyl, amide groups, ehter bond etc. can also be used as polar hydrophilic group；And hydrophobic grouping is often to be nonpolar Hydrocarbon chain, such as 8 carbon atom above hydrocarbon chains.Surfactant is divided into ionic surfactant (including cationic surfactant With anion surfactant), nonionic surface active agent, amphoteric surfactant, compound surfactant, other surfaces Activating agent etc..And described buffer is primarily used to adjust the solvent of pH value, usually salt, as strong acid weak base or weak acid are strong Alkali salt class, the acid in salt or alkali are gradually disengaged in reaction or preservation to keep stable pH-value.Described diethylidene three Triamine pentaacetic acid is a kind of metal-chelator, and another important indicator for evaluating ink performance is conductivity value.Conductivity values are For reflecting the height of wherein salt content.The two ionic factors of salt and dyestuff of the parameter in by ink are influenceed, although The ionic of dyestuff will not cause damage as salt to print cartridge, but the salt (such as sodium chloride) in ink can damage print cartridge or even make Print cartridge fails.It need to add metal-chelator during ink formulation sometimes for this.

Further, the surfactant is trialkyl phosphates.Described trialkyl phosphates are that a kind of surface is lived Property agent, synthetic reaction is mainly carried out by POCl3 and excessive alcohol at low temperature, passes through what is generated in vacuum discharge reaction Hydrogen chloride, excessive alcohol is then reclaimed, is then neutralized with alkali, be finally evaporated under reduced pressure and obtain finished product.And the trialkyl in the present invention Phosphate is directly commercially to purchase matured product, and its specific preparation method is prior art, therefore be will not be described in detail herein.

The surfactant is pine-seed oil.Described pine-seed oil is a kind of natural surfactant, not only cost compared with To be cheap, and it is more green.And pine-seed oil is spread with certain dividing and defoaming effect, in the difference of ink manufacture Stage adds pine-seed oil as anti-foaming agent or defoamer to control foaming degree.

The buffer is potassium dihydrogen phosphate.Potassium dihydrogen phosphate, it is colourless tetragonal crystal or white crystalline powder.Relatively Density 2.338.252.6 DEG C of fusing point.Soluble in water, at 90 DEG C, solubility is 83.5g/100ml water, and the aqueous solution is in acidity, 1% The pH value of potassium dihydrogen phosphate is 4.6.Potassium dihydrogen phosphate is usually industrially used as buffer, not only with preferable water Dissolubility, and be easy to adjust its pH value.

Further, also added with the ultraviolet radiation absorption for being used for improving light fastness in terms of mass fraction in formula materials Agent 0.8-2.1%, described ultra-violet absorber are BP-4.Common dye ink exists Under dayligth effect, dyestuff absorbs luminous energy, and molecule, which is in, to be intensified state and become extremely unstable, it is easy to some chemical reactions are produced, Decompose dyestuff to fade, cause print pattern to produce obviously discolouration phenomena after Exposure to Sunlight.And common dye ink because The rate of decay of different colours is different and causes to print works " discoloration ".The problem of in order to overcome its light resistance poor, so as to logical Crossing the ultra-violet absorber of addition increases its light fastness.Described BP-4 is a kind of White or buff powder, be a kind of broad spectrum ultraviolet light absorbent, have absorption efficiency it is high, it is nontoxic, without teratogenesis side effect, it is right The advantages that light, heat endurance are good, it is not easy corruption, service life length；Good water solubility, it is in high transparency liquid to be dissolved in after water；It can improve The stability of various materials in water-based system.In general ultra-violet absorber it is water-soluble poor, it is impossible to be dissolved in aqueous ink In water, and BP-4 has preferably water solubility, so as to the energy after multiple times of filtration finished product It is enough to maintain higher content, avoid reducing light resistance because filtering out active ingredient when producing ink.

Further, described organic solvent is the mixture of glycerine and tetrahydrofuran, glycerine and tetrahydrofuran Mixing ratio is 4：3.The organic solvent being wherein added with is mixture, and described glycerine and tetrahydrofuran are high-dissolvability Organic solvent, and can are dissolved each other, and can dissolve the additive that part is slightly soluble in water, so as to improve the performance of whole ink.

Further, also it is added with formula materials in terms of mass fraction for improving the propylene of dimethyl two of color fastness to water Ammonium chloride 0.9-1.2%.

The present invention compared with prior art, has the advantage that and had the beneficial effect that：The present invention in order to meet printing requirement, When preparing ink-jet printing ink, the various additives that are added with and the colouring agent selected according to the ratio of optimization are so as to carrying comprehensively The performance of high ink, improve stability；Also to be added as needed on solvent, cosolvent, surfactant, buffer and water in addition Deng so that ink makes great progress in terms of water-fast, fast light, sunlight fastness and image definition.The side of the present invention Method can effectively improve the production efficiency of the water-base ink, and improve ink quality and performance.

Embodiment

The present invention is described in further detail with reference to embodiment, but the implementation of the present invention is not limited to this, Without departing from the idea case in the present invention described above, according to ordinary skill knowledge and customary means, various replace is made Change and change, all should be included within the scope of the invention.

Embodiment 1：

Present embodiment discloses a kind of composite water soluble ink jet ink for printing formula, the formula materials are included with quality point Count the water-soluble dye 3-5% counted, organic solvent 15-25%, surfactant 0.8-1.5%, buffer 0.5-1.5%, two Ethylenetriamine pentacetic acid 0.2-0.4%, dimethyl-dipropenyl ammonium chloride 0.9-1.2%, 2- hydroxyl -4- methoxyl group hexichol first Ketone -5- sulfonic acid 0.8-2.1% and deionized water 70-85%.Its making step is as follows：

1st, it is first according to mass fraction calculating and takes following material：

5% water-soluble dye

19% organic solvent

1.2% trialkyl phosphates

1.5% potassium dihydrogen phosphate

0.3% diethylene-triamine pentaacetic acid

0.9% dimethyl-dipropenyl ammonium chloride

1% BP-4

71.1% deionized water

Will be above-mentioned individually placed standby as raw material, wherein with mass fraction than 4：3 take glycerine and tetrahydrofuran Be put into stirred tank carry out mix 12min make it mix to obtain organic solvent and deposit standby；Then by ready water solubility Dyestuff and organic solvent are put into stirred tank be heated to 60 DEG C within the temperature range of stir 12min, it is mixed for solvent orange 2 A.

2nd, trialkyl phosphates and diethylene-triamine pentaacetic acid are added respectively into the solvent orange 2 A to have stirred, often It must be kept stirring for when adding a kind of additive, addition potassium dihydrogen phosphate adjusts its pH value formation solvent then it is stirred for 8min after B。

3rd, deionized water is slowly filled in most backward solvent B and stirs 30min and obtains ink crude product；The ink that will be obtained Water crude product is placed in ultrasonic processing equipment handles 150h with 1040kHz high frequency ultrasounds, then detects its indices.

4th, filter plant is ready to, the filter plant includes standing pond, multi-layer filter paper filter and polytetrafluoroethylene (PTFE) Filter cloth filtering machine；Ink crude product after being ultrasonically treated, which is passed through to stand, carries out cooling and standings precipitation in pond, during standing A length of 30min.

5 then by stand pond in ink crude product be passed through multi-bed filter and polytetrafluoroethylene (PTFE) filter cloth filtering machine successively In filtered, by the small particle contaminant filter in ink crude product；Most come out at last from polytetrafluoroethylene (PTFE) filter cloth filtering machine Ink product is stored in macromolecule storage barrel and stored.5 layer polypropylene cotton filter layers, institute are provided with the multi-bed filter State in polytetrafluoroethylene (PTFE) filter cloth filtering machine and be provided with 6 strata tetrafluoroethene filter clothes.

Described trialkyl phosphates are a kind of surfactants, mainly by POCl3 and excessive alcohol at low temperature Synthetic reaction is carried out, by the hydrogen chloride generated in vacuum discharge reaction, excessive alcohol is then reclaimed, is then neutralized with alkali, most It is evaporated under reduced pressure afterwards and obtains finished product.And the trialkyl phosphates in the present invention are directly commercially to purchase matured product, its is specific Preparation method be prior art, therefore will not be described in detail herein.

And potassium dihydrogen phosphate, it is colourless tetragonal crystal or white crystalline powder.Relative density 2.338.Fusing point 252.6 ℃.Soluble in water, at 90 DEG C, solubility is 83.5g/100ml water, and the aqueous solution is in acidity, the pH value of 1% potassium dihydrogen phosphate For 4.6.It is industrial usually to use potassium dihydrogen phosphate that not only there is preferably water solubility, and be easy to adjust it as buffer PH value.

And common dye ink is under dayligth effect, dyestuff absorbs luminous energy, and molecule, which is in, to be intensified state and become extremely unstable, It is easy to produce some chemical reactions, decomposes dyestuff and fade, cause print pattern to be produced after Exposure to Sunlight and obviously fade Phenomenon.And common dye ink causes to print works " discoloration " because the rate of decay of different colours is different.In order to overcome it The problem of light resistance is poor, so as to increase its light fastness by the ultra-violet absorber of addition.Described 2- hydroxyl -4- methoxies Base benzophenone -5- sulfonic acid is a kind of white or buff powder, is a kind of broad spectrum ultraviolet light absorbent, has absorption efficiency It is high, nontoxic, without teratogenesis side effect, to light, heat endurance is good the advantages that, be not easy corruption, service life length；Good water solubility, it is molten Yu Shuihou is in high transparency liquid；The stability of various materials in water-based system can be improved.In general ultra-violet absorber it is water-soluble Property it is poor, it is impossible to be dissolved in water-base ink, and BP-4 have preferably it is water-soluble Property, so as to being able to maintain that higher content after multiple times of filtration finished product, avoid when producing ink because filtering out active ingredient and Reduce light resistance.

Further, described organic solvent is the mixture of glycerine and tetrahydrofuran, glycerine and tetrahydrofuran Mixing ratio is 4：3.The organic solvent being wherein added with is mixture, and described glycerine and tetrahydrofuran are high-dissolvability Organic solvent, and can are dissolved each other, and can dissolve the additive that part is slightly soluble in water, so as to improve the performance of whole ink.Match somebody with somebody Also it is added with square bar material in terms of mass fraction for improving the dimethyl-dipropenyl ammonium chloride 0.9-1.2% of color fastness to water.

Embodiment 2：

According to the preparation method in embodiment 1, the organic solvent in raw material is removed, and adds 19% plasma water As replacement, be made contrast groups 1 test it is standby.

Embodiment 3：

According to the preparation method in embodiment 1, the trialkyl phosphates in raw material are removed, and the mass fraction such as addition Plasma water as replacing, be made contrast groups 2 test it is standby.

Embodiment 4：

According to the preparation method in embodiment 1, the diethylene-triamine pentaacetic acid in raw material is removed, and the matter such as addition The plasma water of fraction is measured as replacing, be made contrast groups 3 test it is standby.

Embodiment 5：

According to the preparation method in embodiment 1, the dimethyl-dipropenyl ammonium chloride in raw material is removed, and add etc. The plasma water of mass fraction as replacing, be made contrast groups 4 test it is standby.

Embodiment 6：

According to the preparation method in embodiment 1, the BP-4 in raw material is gone Fall, and the plasma water of mass fraction such as add as replacing, be made contrast groups 5 test it is standby.

Embodiment 7：

According to the preparation method in embodiment 1, the supersonic treatment in former preparation method is removed, the ink that will be obtained Water crude product be directly filtrated to get final products contrast groups 6 the most test it is standby.

Sample in above-mentioned contrast groups and embodiment 1 is subjected to unified test, what deserves to be explained is, all contrast groups are equal Including 10-15 group samples, then using the results averaged that every group of contrast groups are tested as final measured value.

The index wherein to be tested is including stability test, water resistance test, alkali resistance is tested, optical density is tested, dry Dry time and the test of colourity.

Wherein described water resistance experimental method is that the ink-jet printing ink (including standard sample) that will be prepared uniformly applies Smear on a plastic film, make the consistency of thickness of different samples as far as possible, wiped after drying in mixture of ice and water, record is just The number that sample can be wiped out, performance comparison is carried out with standard sample.Alkali resistance method of testing and water resistance testing method phase Together, alkali lye selection mass fraction for 3% sodium hydroxide solution.

And the phenomenon of clear liquid precipitation can occur during standing for the unstable ink of described system, that is, it is existing that sedimentation occurs As ink layer height declines.In experiment, tested ink is poured into the graduated graduated cylinder of tool, tests the liquid of its precipitation With the situation that moves down at the solids interface of sinking, drafting liquid level moves down the relation curve with standing time, scattered steady as system Qualitatively characterize, and contrasted with standard sample.

And described drying time is then that every group of sample is dipped into some inks (about 0.01ml) to general with glass bar On logical printing paper, its colourity and drying time are observed.

Test result such as following table：

According to above-mentioned test data analyzer, all indexs of the sample in embodiment 1 are optimal, and lack corresponding function Additive will have certain index and decline, and wherein all remove organic solvent in contrast groups 1, cause many additives without Method is fully compatible with water, then various aspects of performance index has decline.And wherein for eliminating metal-chelator in contrast groups 3, Show that wherein salt content is higher using single conductivity test, the extent of corrosion highest to caused by print cartridge.

It is described above, be only presently preferred embodiments of the present invention, any formal limitation not done to the present invention, it is every according to Any simply modification, the equivalent variations made according to the technical spirit of the present invention to above example, each fall within the protection of the present invention Within the scope of.

Claims

A kind of 1. preparation method of composite water soluble ink jet ink for printing, it is characterised in that：Including step once：

S1. it is first according to mass fraction calculating and takes 3-5% water-soluble dye, 15-25% organic solvent, the three of 0.8-1.5% Alkyl phosphate, 0.5-1.5% potassium dihydrogen phosphate, 0.2-0.4% diethylene-triamine pentaacetic acid and 70-85% deionization Water is used as the raw material of composite water soluble ink and individually placed standby；

S2. and then ready water-soluble dye and organic solvent are put into and 45-70 DEG C of temperature range is heated in stirred tank Interior stirring 10-15min, it is set to mix for solvent orange 2 A；

S3. trialkyl phosphates and diethylene-triamine pentaacetic acid are added respectively into the solvent orange 2 A to have stirred, are often added It must be kept stirring for during a kind of additive, addition potassium dihydrogen phosphate adjusts its pH value formation solvent then it is stirred for 5-10min after B；

S4. deionized water is slowly filled in most backward solvent B and stirs 20-30min and obtains ink crude product；

S5. obtained ink crude product is placed in ultrasonic processing equipment and 120-180h is handled with 1040kHz high frequency ultrasounds, so After detect its indices；

S6. the ink crude product after being ultrasonically treated carries out multiple times of filtration and finally gives ink product and encapsulate preservation.
A kind of 2. preparation method of composite water soluble ink jet ink for printing according to claim 1, it is characterised in that：It is described Organic solvent be the mixture of glycerine and tetrahydrofuran, the mixing ratio of glycerine and tetrahydrofuran is 4：3.
A kind of 3. preparation method of composite water soluble ink jet ink for printing according to claim 1, it is characterised in that：In step With mass fraction than 4 in rapid S1：3 take glycerine and tetrahydrofuran is put into stirred tank to carry out mixing 10-15min and it is mixed Obtain organic solvent and deposit standby.
A kind of 4. preparation method of composite water soluble ink jet ink for printing according to claim 1, it is characterised in that：It is described Step S6's comprises the following steps that：

S61. filter plant is ready to first, the filter plant includes standing pond, multi-layer filter paper filter and polytetrafluoroethyl-ne Alkene filter cloth filtering machine；

S62. the ink crude product after being ultrasonically treated, which is passed through to stand, carries out cooling and standings precipitation in pond, a length of during standing 30-50min；

S63. and then by the ink crude product stood in pond it is passed through successively in multi-bed filter and polytetrafluoroethylene (PTFE) filter cloth filtering machine Filtered, by the small particle contaminant filter in ink crude product；

S64. the ink product most come out at last from polytetrafluoroethylene (PTFE) filter cloth filtering machine, which is stored in macromolecule storage barrel, to be stored up Deposit.
A kind of 5. preparation method of composite water soluble ink jet ink for printing according to claim 1, it is characterised in that：It is described 5-7 layer polypropylene cotton filter layers are provided with multi-bed filter, 3-5 strata tetrafluoros are provided with the polytetrafluoroethylene (PTFE) filter cloth filtering machine Ethene filter cloth.