CN108017953A - A kind of preparation method of heat-resisting hydrophobic type water-based ink binder - Google Patents
A kind of preparation method of heat-resisting hydrophobic type water-based ink binder Download PDFInfo
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- CN108017953A CN108017953A CN201711489125.5A CN201711489125A CN108017953A CN 108017953 A CN108017953 A CN 108017953A CN 201711489125 A CN201711489125 A CN 201711489125A CN 108017953 A CN108017953 A CN 108017953A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/10—Printing inks based on artificial resins
- C09D11/106—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- C09D11/107—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds from unsaturated acids or derivatives thereof
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
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Abstract
The present invention relates to field of polymer material preparing technology, and in particular to a kind of preparation method of heat-resisting hydrophobic type water-based ink binder.The present invention is using modified acrylic acid emulsion as base material, modified carbon nano tube pipe powder and modified boron mud powder are as accelerating agent, and it is aided with poloxalkol and potassium peroxydisulfate etc. and heat-resisting hydrophobic type water-based ink binder is prepared, acrylic resin is modified first, acrylic resin is effectively filled in inside water-based ink binder, be conducive to the heat resistance of water-based ink binder, adhesive force and hydrophobicity are improved, steam distillation is recycled to extract plants essential oil from roseleaf, by modified carbon nanotube powder and plants essential oil and Yoghourt blending fermentation, improve the compatibility of carbon nanotube powder and base material, continue with boron mud powder and self-control dispersion liquid reaction, further improve the heat resistance of water-based ink binder, it is with a wide range of applications.
Description
Technical field
The present invention relates to field of polymer material preparing technology, and in particular to a kind of heat-resisting hydrophobic type water-based ink binder
Preparation method.
Background technology
Ink is the important materials for printing, it is shown pattern, word on stock by printing.Ink is general
It is made of pigment, binder, solvent and auxiliary agent etc., these components equably mix and form a kind of stickiness glue through repeat-rolling
Fluid.Ink is widely used in the various printings such as books and periodicals, packing and decorating, building decoration, as social demand increases, ink kind and
Yield also respective extension and growth.
Ink adhesive is the important component for printing ink, is the fluid section of ink.The rheological characteristic of printing ink,
Viscosity, drying property, film forming and printing performance, depend primarily upon binder.Solid constituent in ink is by binder
Wetting action can be finely ground in the fabrication process, by its viscosity complete printing process transmission shift, on printed matter according to
By link stuff drying and forming-film make trace formed gloss fastness ink film and protect pigment.Transmission of the link stuff to ink
Property, brightness, the printability such as fixed speed and printing effect have a significant impact, therefore, it is to ensure print to select suitable binder
One of good key is brushed, the composition of link stuff can be adjusted at any time with matching somebody with somebody according to the difference of packaging material, print request etc.
Than.
In recent years, people are higher and higher to the demand of packages printing security, and water-based ink is by low VOC, non-combustible, nothing
The environmentally friendly feature such as poison and free from extraneous odour, the just mainstream and trend as ink industry development.Waterborne binder is a kind of hydrophilic
High molecular material, can dissolve or be swollen and form solution or dispersion liquid in water.The quality of waterborne binder quality, directly affects
The performance of water-based ink.The water-based ink binder of early stage is mainly made of rosin and maleic acid modified resin, its performance
It is poor.
At present, the binder of general water-based ink is waterborne polyurethane resin and water-based acrylic resin etc., due to poly- ammonia
Ester molecule has " Scalability ", in conjunction with new modification and synthesis technique, can by effectively control water-based ink structure and
Composition, enables resistance to high bottom warm nature, wearability, intensity, pliability and levelability of ink film etc. to have and largely carries
Height, aqueous polyurethane binder have become the research hotspot of current ink area.In addition, it can also reduce flammable solvent
And the fire hazard caused by electrostatic, the residual smell on printing surface is eliminated, is most potential binder tree used for water color ink
Fat.
Since the water imbibition of waterborne polyurethane resin is stronger, it is unfavorable for the disengaging of moisture.If water-based ink drying is too slow,
Printed matter underdry can be caused, ink is adhered on dancing roll, and printed matter tarnishes, and can also influence double exposure effect, causes to print
Brush quality problem；Water-based ink drying it is too fast, easily in printing process ink also not in printable fabric surface penetration just
It has been done that, cause ink to be suspended in printable fabric surface, adhesive force is deteriorated.Therefore water-based ink is spread out in printing process just
During to printable fabric surface, rate of drying will soon, but it is dry to a certain extent when, it is necessary to slow down rate of drying, in favor of water
Property ink has time enough to penetrate into printable fabric.In addition, water-based polyurethane ink binder also generally existing
It is low solid content, the shortcomings of poor water resistance, hydrolytic resistance are poor, resistance to blocking is poor, boiling resistance is poor, need to further improve.
Therefore, developing a kind of water-based ink binder that can solve above-mentioned performance issue is highly desirable.
The content of the invention
The technical problems to be solved by the invention：It is stronger for the water imbibition of current common water borne ink adhesive, it is unfavorable
In the disengaging of moisture, if water-based ink drying is too slow, printed matter underdry can be caused, and water-based ink drying is too fast, holds
Easily cause ink and be suspended in printable fabric surface, adhesive force is deteriorated, additionally there are poor heat resistance and poor water resistance, can not meet
A kind of the defects of market demands, there is provided preparation method of heat-resisting hydrophobic type water-based ink binder.
In order to solve the above technical problems, the present invention is using technical solution as described below：
A kind of preparation method of heat-resisting hydrophobic type water-based ink binder, it is characterised in that specifically preparation process is：
（1）Roseleaf and deionized water are mixed and are placed in the four-hole boiling flask equipped with thermometer, condenser and blender, Xiang Si
Mouthful flask is passed through vapor, first with the low temperature for evaporating fast distillation, controlling condensed water, then with height evaporates fast distillation, heat temperature raising, obtains
Emulsion, the sodium chloride mixing vibration of emulsion quality 7% is added into emulsion, pours into stand in separatory funnel after vibration and divides
Layer, discharges lower water phase after layering, finally draw remaining water with anhydrous sodium sulfate, and still aging, filtering removes solid sulphuric acid
Sodium, takes out filtrate, is Rosa Damascana；
（2）Weigh 20~24g carbon nanotubes and pour into ball milling in ball mill, obtain carbon nanotube powder, then to carbon nanotube powder
The Yoghourt of the middle Rosa Damascana and carbon nanotube powder quality 0.8% for adding carbon nanotube powder quality 9%, is fitted into fermentation tank,
It is sealed by fermentation, after fermentation, takes out tunning, is separated by filtration to obtain fermentation filter residue, is modified carbon nano tube pipe powder；
（3）Bisphenol A type epoxy resin, methyl methacrylate, butyl acrylate and acrylic acid are mixed to be placed in beaker and stirred,
Hybrid resin is obtained, then deionized water, lauryl sodium sulfate, stearoyl lactate and sodium acid carbonate are mixed and are placed on four mouthfuls
Stirring and dissolving in flask, obtains self-control emulsion, continues hybrid resin, self-control emulsion and ammonium persulfate mixing being placed in stirring
Reaction is stirred in machine, cooling discharging, obtains modified acrylic acid emulsion；
（4）100 mesh sieves are crossed after weighing the grinding of 16~20g boron muds, collect sieving boron mud powder, then weigh 4~6g dodecyl sulphur
Sour sodium is poured into the beaker with 42~46mL deionized waters, is placed in ultrasonic disperse in ultrasonic wave separating apparatus, obtains self-control point
Dispersion liquid, sieving boron mud powder and self-control dispersion liquid are mixed, and obtain modified boron mud powder；
（5）Count in parts by weight, weigh respectively 30~40 parts of modified acrylic acid emulsions, 12~16 parts of modified carbon nano tube pipe powders,
10~12 parts of modified boron mud powder, 4~6 parts of Pluronic F68s, 2~4 parts of stearyl lactate, 1~3 part
Ethylenediamine and 2~4 parts of potassium peroxydisulfates, first mix modified acrylic acid emulsion, modified carbon nano tube pipe powder and modified boron mud powder
It is placed in mixer and stirs, then adds Pluronic F68, stearyl lactate, ethylenediamine and potassium peroxydisulfate,
Continue to be mixed and cure, cooling discharging, barrelling is up to heat-resisting hydrophobic type water-based ink binder.
Step（1）The roseleaf and the mass ratio of deionized water are 1：5, the low speed that evaporates is 90~100L/h, low
It is 1~3h to evaporate fast distillation time, and the temperature for controlling condensed water is 35~40 DEG C, and it is 110~125L/h that height, which evaporates speed, and height evaporates fast steaming
It is 45~60min to evaporate the time, and heat temperature raising temperature is 36~42 DEG C, and the stratification time is 2~4min, and the still aging time is
1~2 day.
Step（2）The rotational speed of ball-mill is 85~95r/min, and Ball-milling Time is 45~60min, fermentation temperature for 28~
32 DEG C, fermentation time is 12~16h.
Step（3）The bisphenol A type epoxy resin, methyl methacrylate, the quality of butyl acrylate and acrylic acid
Than for 3：1：1：2, whipping temp is 45~55 DEG C, and mixing time be 12~16min, deionized water, lauryl sodium sulfate, firmly
The mass ratio of acyl sodium lactate and sodium acid carbonate is 5：1：2：1, the stirring and dissolving time is 20~24min, and hybrid resin, self-control are newborn
The mass ratio for changing liquid and ammonium persulfate is 2：3：1, stirring reaction temperature is 75~80 DEG C, and stirring reaction rotating speed is 320~360r/
Min, stirring reaction time are 1~2h.
Step（4）The milling time is 8~10min, and the ultrasonic disperse time is 24~32min, and sieve boron mud powder
Mass ratio with self-control dispersion liquid is 1：3, mixing time is 16~20min.
Step（5）The whipping temp is 35~45 DEG C, and mixing time is 20~30min, and stirring solidification temperature is 75
~85 DEG C, stirring hardening time is 1~3h.
Compared with other methods, advantageous effects are the present invention：
The present invention using modified acrylic acid emulsion as base material, modified carbon nano tube pipe powder and modified boron mud powder as accelerating agent, and
It is aided with Pluronic F68 and potassium peroxydisulfate etc. and heat-resisting hydrophobic type water-based ink binder is prepared, first
Acrylic resin is modified using bisphenol A type epoxy resin, its epoxy resin has very strong cohesive force, and with cause
Close polyhydroxy molecular structure, allows it to be grafted on as macromolecular chain extender in acrylic resin strand, is formed three-dimensional
Cross-linked structure, and the certain heat resistance of acrylic resin, adhesive strength and water resistance are assigned, by acrylic resin effectively
It is filled in inside water-based ink binder, heat resistance, adhesive force and the hydrophobicity for being conducive to water-based ink binder are improved,
Steam distillation is recycled to extract plants essential oil from roseleaf, will then by being modified to carbon nanotube powder
Itself and plants essential oil and Yoghourt blending ferment, and decompose Activities of Some Plants essential oil using microorganism and produce lipophile ester group,
So that ester group is grafted to carbon nanotube powder surface, so as to improve carbon nanotube powder and base material under the self-crosslinking of microorganism
Compatibility, wherein plants essential oil is high hydrophobic, high volatile aromatic substance, and carbon nanotubes has heat resistance, utilizes carbon
Nanotube powder effectively fills water-based ink binder internal void, is conducive to the heat-resisting of water-based ink binder
Property, hydrophobicity and first dryness be improved, continue to mix in boron mud powder and self-control dispersion liquid containing lauryl sodium sulfate,
Boron mud powder is set to be dispersed in substrate surface, since sodium oxide molybdena in boron mud and boron oxide have the characteristic of vitrifying tendency,
In reaction process, the scope of melting base material setting temperature can be substantially reduced, further improves the heat resistance of water-based ink binder,
It is with a wide range of applications.
Embodiment
It is 1 in mass ratio：5 are placed in roseleaf and deionized water mixing equipped with thermometer, condenser and blender
In four-hole boiling flask, vapor is passed through to four-hole boiling flask, first speed 1~3h of distillation is evaporated with the low of 90~100L/h, controls condensed water
Temperature evaporates speed 45~60min of distillation at 35~40 DEG C, then with the height of 110~125L/h, is heated to 36~42 DEG C, obtains breast
Turbid, the sodium chloride mixing vibration of emulsion quality 7% is added into emulsion, stratification 2 in separatory funnel are poured into after vibration
~4min, discharges lower water phase after layering, finally draw remaining water with anhydrous sodium sulfate, still aging 1~2 day, filter off
Except solid sodium sulfate, filtrate is taken out, is Rosa Damascana；Weigh 20~24g carbon nanotubes to pour into ball mill, be 85 in rotating speed
45~60min of ball milling under conditions of~95r/min, obtains carbon nanotube powder, then carbon nanometer is added into carbon nanotube powder
The Rosa Damascana of pipe powder quality 9% and the Yoghourt of carbon nanotube powder quality 0.8%, are fitted into fermentation tank, temperature for 28~
12~16h is sealed by fermentation under conditions of 32 DEG C, after fermentation, takes out tunning, is separated by filtration to obtain fermentation filter residue, is
Modified carbon nano tube pipe powder；It is 3 in mass ratio：1：1：2 by bisphenol A type epoxy resin, methyl methacrylate, butyl acrylate
With acrylic acid mixing be placed in beaker, temperature be 45~55 DEG C at stir 12~16min, obtain hybrid resin, then will go from
Sub- water, lauryl sodium sulfate, stearoyl lactate and sodium acid carbonate are 5 in mass ratio：1：2：1 mixing is placed on four-hole boiling flask
Middle 20~24min of stirring and dissolving, obtains self-control emulsion, continues hybrid resin, self-control emulsion and ammonium persulfate by quality
Than for 2：3：1 mixing is placed in mixer, is stirred under conditions of temperature is 75~80 DEG C, rotating speed is 320~360r/min anti-
1~2h is answered, cooling discharging, obtains modified acrylic acid emulsion；Weigh after 16~20g boron muds grind 8~10min and cross 100 mesh sieves, receive
Collection sieving boron mud powder, then weigh 4~6g lauryl sodium sulfate and pour into the beaker with 42~46mL deionized waters, juxtaposition
24~32min of ultrasonic disperse in ultrasonic wave separating apparatus, obtains self-control dispersion liquid, is in mass ratio 1：3 will sieving boron mud powder
16~20min is mixed with self-control dispersion liquid, obtains modified boron mud powder；Count in parts by weight, weigh 30~40 parts respectively
Modified acrylic acid emulsion, 12~16 parts of modified carbon nano tube pipe powders, 10~12 parts of modified boron mud powder, 4~6 parts of polyoxyethylene-
Poiyoxypropylene copolymer, 2~4 parts of stearyl lactate, 1~3 part of ethylenediamine and 2~4 parts of potassium peroxydisulfates, first by modified acroleic acid
Lotion, modified carbon nano tube pipe powder and modified boron mud powder mixing are placed in mixer, and 20 are stirred at being 35~45 DEG C in temperature
~30min, then Pluronic F68, stearyl lactate, ethylenediamine and potassium peroxydisulfate are added, it is in temperature
Continue to be mixed at 75~85 DEG C and cure 1~3h, cooling discharging, barrelling is up to heat-resisting hydrophobic type water-based ink binder.
Example 1
It is 1 in mass ratio：5 mix roseleaf and deionized water four mouthfuls be placed in equipped with thermometer, condenser and blender
In flask, vapor is passed through to four-hole boiling flask, first speed distillation 1h is evaporated with the low of 90L/h, controls the temperature of condensed water at 35 DEG C, then
Speed distillation 45min is evaporated with the height of 110L/h, 36 DEG C is heated to, obtains emulsion, emulsion quality is added into emulsion
7% sodium chloride mixing vibration, pours into stratification 2min in separatory funnel, lower water phase is discharged after layering, is finally used after vibration
Anhydrous sodium sulfate draws remaining water, and still aging 1 day, filtering removed solid sodium sulfate, took out filtrate, is Rosa Damascana；
Weigh 20g carbon nanotubes to pour into ball mill, the ball milling 45min under conditions of rotating speed is 85r/min, obtains carbon nanotube powders
End, then add into carbon nanotube powder the Rosa Damascana and carbon nanotube powder quality 0.8% of carbon nanotube powder quality 9%
Yoghourt, is fitted into fermentation tank, is sealed by fermentation 12h under conditions of being 28 DEG C in temperature, after fermentation, takes out tunning, mistake
Isolated fermentation filter residue is filtered, is modified carbon nano tube pipe powder；It is 3 in mass ratio：1：1：2 by bisphenol A type epoxy resin, first
Base methyl acrylate, butyl acrylate and acrylic acid mixing are placed in beaker, are stirred 12min at being 45 DEG C in temperature, are mixed
Resin, then by deionized water, lauryl sodium sulfate, stearoyl lactate and sodium acid carbonate in mass ratio be 5：1：2：1 is mixed
Conjunction is placed on stirring and dissolving 20min in four-hole boiling flask, obtains self-control emulsion, continues hybrid resin, self-control emulsion and mistake
Ammonium sulfate is 2 in mass ratio：3：1 mixing is placed in mixer, is stirred under conditions of temperature is 75 DEG C, rotating speed is 320r/min
1h is reacted, cooling discharging, obtains modified acrylic acid emulsion；100 mesh sieves are crossed after weighing 16g boron muds grinding 8min, collect sieving boron
Mud powder, then weigh 4g lauryl sodium sulfate and pour into the beaker with 42mL deionized waters, it is placed in ultrasonic wave separating apparatus
Middle ultrasonic disperse 24min, obtains self-control dispersion liquid, is in mass ratio 1：Sieving boron mud powder and self-control dispersion liquid are mixed and stirred by 3
16min is mixed, obtains modified boron mud powder；Count in parts by weight, weigh 30 parts of modified acrylic acid emulsions respectively, 12 parts of carbon modifieds are received
Mitron powder, 10 parts of modified boron mud powder, 4 parts of Pluronic F68s, 2 parts of stearyl lactate, 1 part of second two
Amine and 2 parts of potassium peroxydisulfates, modified acrylic acid emulsion, modified carbon nano tube pipe powder and modified boron mud powder first mixed and be placed in stirring
In machine, 20min is stirred at being 35 DEG C in temperature, then add Pluronic F68, stearyl lactate, second two
Amine and potassium peroxydisulfate, continue to be mixed and cure 1h at being 75 DEG C in temperature, and cooling discharging, barrelling is water-based up to heat-resisting hydrophobic type
Ink adhesive.
Example 2
It is 1 in mass ratio：5 mix roseleaf and deionized water four mouthfuls be placed in equipped with thermometer, condenser and blender
In flask, vapor is passed through to four-hole boiling flask, first speed distillation 2h is evaporated with the low of 95L/h, controls the temperature of condensed water at 38 DEG C, then
Speed distillation 53min is evaporated with the height of 119L/h, 39 DEG C is heated to, obtains emulsion, emulsion quality is added into emulsion
7% sodium chloride mixing vibration, pours into stratification 3min in separatory funnel, lower water phase is discharged after layering, is finally used after vibration
Anhydrous sodium sulfate draws remaining water, and still aging 1.5 days, filtering removed solid sodium sulfate, took out filtrate, is rhodamine toner
Oil；Weigh 22g carbon nanotubes to pour into ball mill, the ball milling 53min under conditions of rotating speed is 90r/min, obtains carbon nanotubes
Powder, then add into carbon nanotube powder the Rosa Damascana and carbon nanotube powder quality 0.8% of carbon nanotube powder quality 9%
Yoghourt, be fitted into fermentation tank, temperature be 30 DEG C under conditions of be sealed by fermentation 14h, after fermentation, take out tunning,
It is separated by filtration to obtain fermentation filter residue, is modified carbon nano tube pipe powder；It is 3 in mass ratio：1：1：2 by bisphenol A type epoxy resin,
Methyl methacrylate, butyl acrylate and acrylic acid mixing are placed in beaker, are stirred 14min at being 50 DEG C in temperature, are obtained
Hybrid resin, then by deionized water, lauryl sodium sulfate, stearoyl lactate and sodium acid carbonate in mass ratio be 5：1：2：1
Mixing be placed on stirring and dissolving 22min in four-hole boiling flask, obtain self-control emulsion, continue by hybrid resin, self-control emulsion and
Ammonium persulfate is 2 in mass ratio：3：1 mixing is placed in mixer, is stirred under conditions of temperature is 78 DEG C, rotating speed is 340r/min
Reaction 1.5h is mixed, cooling discharging, obtains modified acrylic acid emulsion；100 mesh sieves are crossed after weighing 18g boron muds grinding 9min, were collected
Boron mud powder is sieved, then weighs 5g lauryl sodium sulfate and pours into the beaker with 44mL deionized waters, is placed in ultrasonic wavelength-division
Ultrasonic disperse 28min in instrument is dissipated, self-control dispersion liquid is obtained, is in mass ratio 1：3 mix sieving boron mud powder and self-control dispersion liquid
Stirring 18min is closed, obtains modified boron mud powder；Count in parts by weight, weigh 35 parts of modified acrylic acid emulsions, 14 parts of modifications respectively
Carbon nanotube powder, 11 parts of modified boron mud powder, 5 parts of Pluronic F68s, 3 parts of stearyl lactate, 2 parts
Ethylenediamine and 2 parts of potassium peroxydisulfates, modified acrylic acid emulsion, modified carbon nano tube pipe powder and modified boron mud powder first mixed and be placed in
In mixer, temperature be 40 DEG C at stir 25min, then add Pluronic F68, stearyl lactate,
Ethylenediamine and potassium peroxydisulfate, continue that curing 2h is mixed, cooling discharging, barrelling is up to heat-resisting hydrophobic type at being 80 DEG C in temperature
Water-based ink binder.
Example 3
It is 1 in mass ratio：5 mix roseleaf and deionized water four mouthfuls be placed in equipped with thermometer, condenser and blender
In flask, vapor is passed through to four-hole boiling flask, first speed distillation 3h is evaporated with the low of 100L/h, controls the temperature of condensed water at 40 DEG C,
Speed distillation 60min is evaporated with the height of 125L/h again, 42 DEG C is heated to, obtains emulsion, emulsion matter is added into emulsion
The sodium chloride mixing vibration of amount 7%, pours into stratification 4min in separatory funnel, lower water phase is discharged after layering, finally after vibration
Remaining water is drawn with anhydrous sodium sulfate, still aging 2 days, filtering removed solid sodium sulfate, took out filtrate, was rhodamine toner
Oil；Weigh 24g carbon nanotubes to pour into ball mill, the ball milling 60min under conditions of rotating speed is 85~95r/min, obtains carbon and receive
Mitron powder, then add into carbon nanotube powder the Rosa Damascana and carbon nanotube powder quality of carbon nanotube powder quality 9%
0.8% Yoghourt, is fitted into fermentation tank, and 16h is sealed by fermentation under conditions of being 32 DEG C in temperature, after fermentation, takes out fermentation production
Thing, is separated by filtration to obtain fermentation filter residue, is modified carbon nano tube pipe powder；It is 3 in mass ratio：1：1：2 by bisphenol type epoxy tree
Fat, methyl methacrylate, butyl acrylate and acrylic acid mixing are placed in beaker, are stirred 16min at being 55 DEG C in temperature, are obtained
It is 5 in mass ratio to hybrid resin, then by deionized water, lauryl sodium sulfate, stearoyl lactate and sodium acid carbonate：1：2：
1 mixing be placed on stirring and dissolving 24min in four-hole boiling flask, obtain self-control emulsion, continue by hybrid resin, self-control emulsion and
Ammonium persulfate is 2 in mass ratio：3：1 mixing is placed in mixer, is stirred under conditions of temperature is 80 DEG C, rotating speed is 360r/min
Reaction 2h is mixed, cooling discharging, obtains modified acrylic acid emulsion；100 mesh sieves are crossed after weighing 20g boron muds grinding 10min, collect sieving
Boron mud powder, then weigh 6g lauryl sodium sulfate and pour into the beaker with 46mL deionized waters, it is placed in ultrasonic wave and disperses
Ultrasonic disperse 32min in instrument, obtains self-control dispersion liquid, is in mass ratio 1：3 will sieving boron mud powder and self-control dispersion liquid mixing
20min is stirred, obtains modified boron mud powder；Count in parts by weight, weigh 40 parts of modified acrylic acid emulsions, 16 parts of carbon modifieds respectively
Nanotube powder, 12 parts of modified boron mud powder, 6 parts of Pluronic F68s, 4 parts of stearyl lactate, 3 parts of second
Diamines and 4 parts of potassium peroxydisulfates, modified acrylic acid emulsion, modified carbon nano tube pipe powder and modified boron mud powder first mixed to be placed in and stirred
Mix in machine, stir 30min at being 45 DEG C in temperature, then add Pluronic F68, stearyl lactate, second
Diamines and potassium peroxydisulfate, continue that curing 3h is mixed, cooling discharging, barrelling is up to heat-resisting hydrophobic type water at being 85 DEG C in temperature
Property ink adhesive.
Comparative example
With the water-based ink binder of Guangzhou company production as a comparison case
Water-based ink binder in heat-resisting hydrophobic type water-based ink binder produced by the present invention and comparative example is detected,
Testing result is as shown in table 1：
1st, solid content is tested
First prepare a roll of tinfoil（About 100mm × 100mm tinfoil pieces）, weight under scale, is calculated as M on electronic balance1.After peeling,
The ink to be measured is poured into, is calculated as M2.Place into 103 DEG C of ovens, when baking 2 is small, takes out rear weighing, be calculated as M3。
Solid content calculation formula=（M3- M1）/M2×100%
2nd, water absorption rate test
Example 1~3 and the water-based ink binder of comparative example prepared by the present invention is added in ink, spare, and ink is applied
It is overlying on polyfluortetraethylene plate, places at room temperature one week and spontaneously dry film forming, it is 30mm × 30mm test blocks to be cut into size,
Claim its quality to be denoted as a, immerse in pure water, taken out after 24h, naturally dry surface moisture weighs it and is denoted as quality b at normal temperatures.
Water absorption rate=(b-a)/a × 100%.
3rd, elongation at break is tested
Example 1~3 and the water-based ink binder of comparative example prepared by the present invention is added in ink, spare, and ink is applied
It is overlying on polyfluortetraethylene plate, places at room temperature one week and spontaneously dry film forming, coated film sample is made to the length of 10mm × 60mm
Bar, after sample is balanced 24h under the conditions of constant temperature and humidity, measures on tensile strength test instrument, absolute long when record is broken
Degree.
4th, resistance to blocking is tested
By the sample after single side dried coating film, coated surface is opposite two-by-two, is stacked together, and stacks the pressure of after-applied 500g/cm
Power, is placed on 5h in climatic chamber.
5th, stability test
Example 1~3 and comparative example product prepared by the present invention is positioned in colorimetric cylinder, is kept in dark place at room temperature 6 months.
6th, pencil hardness test
Using pencil hardness test.Example 1~3 and the water-based ink binder of comparative example prepared by the present invention is added to ink
In, it is spare, by ink coated on polyfluortetraethylene plate, place at room temperature, until film forming is spontaneously dried, after dried coating film,
With 1 kilogram of strength of pressure at right angle, 45 degree of oblique angles draw 3cm length in film, draw 5 times, film does not have cut, and the pencil rank is hard
Degree is hardness of film.
7th, adhesive force is tested
Tested according to standard GB/T9286.0 grade preferably, and 1 grade is taken second place.
8th, water resistance test
Tested according to standard GB/T1733-193.
9th, humidity resistance is tested
Tested according to standard GB/T1740-79.
1 performance measurement result of table
From the data in table 1, it can be seen that when heat-resisting hydrophobic type water-based ink binder produced by the present invention is used in ink, ink can be made
Water resistance, humidity resistance, adhesive force and stability etc. be improved, and the preparation process of the present invention is simple, operation control
System is convenient, stable quality, and production efficiency is high, can large-scale industrial production.Hence it is evident that being better than comparative example product, have wide
Wealthy prospect of the application.
Claims (6)
1. a kind of preparation method of heat-resisting hydrophobic type water-based ink binder, it is characterised in that specifically preparation process is：
（1）Roseleaf and deionized water are mixed and are placed in the four-hole boiling flask equipped with thermometer, condenser and blender, Xiang Si
Mouthful flask is passed through vapor, first with the low temperature for evaporating fast distillation, controlling condensed water, then with height evaporates fast distillation, heat temperature raising, obtains
Emulsion, the sodium chloride mixing vibration of emulsion quality 7% is added into emulsion, pours into stand in separatory funnel after vibration and divides
Layer, discharges lower water phase after layering, finally draw remaining water with anhydrous sodium sulfate, and still aging, filtering removes solid sulphuric acid
Sodium, takes out filtrate, is Rosa Damascana；
（2）Weigh 20~24g carbon nanotubes and pour into ball milling in ball mill, obtain carbon nanotube powder, then to carbon nanotube powder
The Yoghourt of the middle Rosa Damascana and carbon nanotube powder quality 0.8% for adding carbon nanotube powder quality 9%, is fitted into fermentation tank,
It is sealed by fermentation, after fermentation, takes out tunning, is separated by filtration to obtain fermentation filter residue, is modified carbon nano tube pipe powder；
（3）Bisphenol A type epoxy resin, methyl methacrylate, butyl acrylate and acrylic acid are mixed to be placed in beaker and stirred,
Hybrid resin is obtained, then deionized water, lauryl sodium sulfate, stearoyl lactate and sodium acid carbonate are mixed and are placed on four mouthfuls
Stirring and dissolving in flask, obtains self-control emulsion, continues hybrid resin, self-control emulsion and ammonium persulfate mixing being placed in stirring
Reaction is stirred in machine, cooling discharging, obtains modified acrylic acid emulsion；
（4）100 mesh sieves are crossed after weighing the grinding of 16~20g boron muds, collect sieving boron mud powder, then weigh 4~6g dodecyl sulphur
Sour sodium is poured into the beaker with 42~46mL deionized waters, is placed in ultrasonic disperse in ultrasonic wave separating apparatus, obtains self-control point
Dispersion liquid, sieving boron mud powder and self-control dispersion liquid are mixed, and obtain modified boron mud powder；
（5）Count in parts by weight, weigh respectively 30~40 parts of modified acrylic acid emulsions, 12~16 parts of modified carbon nano tube pipe powders,
10~12 parts of modified boron mud powder, 4~6 parts of Pluronic F68s, 2~4 parts of stearyl lactate, 1~3 part
Ethylenediamine and 2~4 parts of potassium peroxydisulfates, first mix modified acrylic acid emulsion, modified carbon nano tube pipe powder and modified boron mud powder
It is placed in mixer and stirs, then adds Pluronic F68, stearyl lactate, ethylenediamine and potassium peroxydisulfate,
Continue to be mixed and cure, cooling discharging, barrelling is up to heat-resisting hydrophobic type water-based ink binder.
A kind of 2. preparation method of heat-resisting hydrophobic type water-based ink binder according to claim 1, it is characterised in that：Step
Suddenly（1）The roseleaf and the mass ratio of deionized water are 1：5, the low speed that evaporates is 90~100L/h, it is low evaporate speed distillation when
Between be 1~3h, the temperature for controlling condensed water is 35~40 DEG C, and it be 110~125L/h that height, which evaporates speed, and it is 45 that height, which evaporates fast distillation time,
~60min, heat temperature raising temperature are 36~42 DEG C, and the stratification time is 2~4min, and the still aging time is 1~2 day.
A kind of 3. preparation method of heat-resisting hydrophobic type water-based ink binder according to claim 1, it is characterised in that：Step
Suddenly（2）The rotational speed of ball-mill is 85~95r/min, and Ball-milling Time is 45~60min, and fermentation temperature is 28~32 DEG C, fermentation
Time is 12~16h.
A kind of 4. preparation method of heat-resisting hydrophobic type water-based ink binder according to claim 1, it is characterised in that：Step
Suddenly（3）The bisphenol A type epoxy resin, methyl methacrylate, the mass ratio of butyl acrylate and acrylic acid are 3：1：1：
2, whipping temp is 45~55 DEG C, and mixing time is 12~16min, deionized water, lauryl sodium sulfate, stearoyl lactate
Mass ratio with sodium acid carbonate is 5：1：2：1, the stirring and dissolving time is 20~24min, and hybrid resin, make emulsion and over cure by oneself
The mass ratio of sour ammonium is 2：3：1, stirring reaction temperature is 75~80 DEG C, and stirring reaction rotating speed is 320~360r/min, and stirring is anti-
It is 1~2h between seasonable.
A kind of 5. preparation method of heat-resisting hydrophobic type water-based ink binder according to claim 1, it is characterised in that：Step
Suddenly（4）The milling time is 8~10min, and the ultrasonic disperse time is 24~32min, and sieving boron mud powder and self-control are scattered
The mass ratio of liquid is 1：3, mixing time is 16~20min.
A kind of 6. preparation method of heat-resisting hydrophobic type water-based ink binder according to claim 1, it is characterised in that：Step
Suddenly（5）The whipping temp is 35~45 DEG C, and mixing time is 20~30min, and stirring solidification temperature is 75~85 DEG C, stirring
Hardening time is 1~3h.
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| CN109457466A (en) * | 2018-11-15 | 2019-03-12 | 李宁 | Functionalized carbon nano-tube and its application in antistatic antibiotic fabric finishing liquor |
| CN109468844A (en) * | 2018-11-15 | 2019-03-15 | 李宁 | Antibacterial fabric and its production technology |
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Application publication date: 20180511 |