CN105348426B - The preparation method of low-temperature fixing chemistry ink powder resin and the method for preparing ink powder - Google Patents
The preparation method of low-temperature fixing chemistry ink powder resin and the method for preparing ink powder Download PDFInfo
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Abstract
The invention belongs to ink powder field, is a kind of preparation method of low-temperature fixing chemistry ink powder resin and the method for preparing ink powder.The preparation method of low-temperature fixing chemistry ink powder resin is：1st, seed emulsion is prepared, 2, prepare low molecule and high-molecular low-temperature is fixed emulsion resin, 3, proportioning is high, bottom molecule low-temperature fixing emulsion resin, and solid content adjusts to 33.0% and obtains low-temperature fixing chemistry ink powder resin.The method for preparing ink powder is：Take low-temperature fixing chemistry ink powder resin 20 50%, colorant 1 5%, CCA dispersion liquids 1 3%, wax emulsion 1 3%, water 40 70%, add dilute sulfuric acid, heat up and keep the temperature 13 it is small when, add sodium hydroxide, adjust PH=6 8, again through heating up, keeping the temperature, cooling down, dry, finished product low-temperature fixing chemistry ink powder.Production technology of the present invention is environment friendly and pollution-free, production cost is low, and suitable for preparing low-temperature fixing chemistry ink powder, and the ink powder prepared is suitable for energy saving laser printing/duplicator of most low-temperature fixings, and fixing effect is good, and transferring rate is high, and color density is excellent, and chargeding performance is excellent.
Description
Technical field
The invention belongs to chemical ink powder field, is a kind of low temperature more particularly, to laser printer or the ink powder of duplicator
The preparation method of fixing chemistry ink powder resin and the method for preparing ink powder.
Background technology
With IT Industry Quick Developments, the requirement of higher, one side printed drawings are proposed to duplicator and printer technology
Piece requires quality exquisite, and another aspect print copying rate request faster, can save time and the energy.The increasing of energy conservation and environmental protection requirement
Add, HP, XEROX Deng Ge major companies are proposed duplicating and the printer of low-temperature fixing one after another, so as to reduce the energy consumption of printer.
The duplicating of low-temperature fixing and printer need corresponding low-temperature photographic fixing powdered ink.It is existing effectively to solve low temperature
Fixing ink powder problem mainly has two approach：First, production adds the physics ink powder of polyester resin；Second, the soft core duricrust knot of production
The chemical ink powder of structure.
Under normal conditions, the way of low-temperature fixing physics ink powder is the low molecular polyester resin using part, so as to drop
The softening point of low hybrid resin, matches low-temperature fixing, and has anticaking capacity, does not influence ambient storage temperature.Polyester resin contains
Carboxyl, hydroxyl, ester bond isoreactivity functional group, hydrogen bond can be formed, this causes more low molecular polyester resin also while possesses
Preferable environmental stability, is not susceptible to be adhered.But the random form of physics ink powder, make its mobility poor, transferring rate
80% generally is extremely difficult to, this can not contend with the transferring rate of chemical ink powder 90% or so.
But polyester resin can not directly lotion be prepared, so the method that general lotion co-agglomeration prepares chemical ink powder is
Prepare the low-temperature fixing chemistry ink powder of core shell structure, internal layer is low molecule low softening point resin, the tree of external sheath high softening-point
Fat.Also there is part company, the polyester resin produced is added into solvent, short grained polyester emulsion is formed by emulsification, then lead to
Cross co-agglomeration and prepare chemical ink powder.The toner particles so formed, transferring rate is high, and anticaking capacity is good, and environmental stability is excellent.So
And chemical ink powder as preparing, production cycle length, to complex process, equipment requirement is very harsh, and domestic equipment is difficult to meet.
If prepare low-temperature fixing chemistry ink powder using traditional co-agglomeration method, the way of general enterprises is to reduce breast
The weight average molecular weight of liquid resin is to 5000-20000, so as to reduce softening point to match the temperature of low-temperature fixing.But it can so go out
The drawbacks of now very big, first, using a large amount of mercaptan type chain transfer agents when preparing low molecule emulsion resin, this can cause follow-up ink
There is stink in powder printing；Second, the resin of low molecular weight be easily adhered in co-agglomeration particle type-approval process, influence ink powder
Form；Third, the ink powder of low molecular weight is also easy to produce glutinous roller phenomenon in fast fixing；Fourth, the ink powder of low molecular weight is unfavorable for ring
Border stores, and causes to fail in builder granule insertion ink powder in course of conveying, ink powder also easily lumps.
For this reason, need to be improved the preparation process of existing low-temperature fixing chemistry ink powder.
The content of the invention
To overcome above-mentioned deficiency, the purpose of the present invention is provide a kind of system of low-temperature fixing chemistry ink powder resin to this area
Preparation Method and the method for preparing ink powder, solve it existing when preparing chemical ink powder resin, using a large amount of mercaptan type chain transfer agents,
Cause the stink subsequently printed, and the chemical ink powder resin of low molecular weight easily occurs to stick in co-agglomeration particle type-approval process excessively
Even, ink powder form is influenced, and the low molecular weight ink powder prepared is also easy to produce glutinous roller phenomenon, the ink powder of low molecular weight in fast fixing
It is unfavorable for ambient storage, causes to fail in builder granule insertion ink powder in course of conveying, the technical problem that ink powder easily lumps.Its
Purpose is achieved by the following technical solution.
The preparation method of the low-temperature fixing chemistry ink powder resin is according to certain ratio by a variety of low-temperature fixing emulsion resins
Example uniformly mixing, is adjusted to certain solid content.The method for preparing low-temperature fixing emulsion resin is to use semi-continuous emulsion polymerizing side
Formula, polymerization system include water, alkenyl unsaturated monomer, initiator, chain-transferring agent and pH buffer, and alkenyl unsaturated monomer includes
The unsaturated function monomer of phenylethylene, esters of acrylic acid and hydroxyl or carboxylic group.It is characterized by preparation method bag
Include following steps：
(1) the seed emulsion stage is prepared.Using alkenyl unsaturated monomer, the mixed mixture gross mass of chain-transferring agent as
100 parts of meters, wherein the mercaptan type chain transfer agent accounts for the 0-1.5% of the mixture gross mass；5-15 parts of mixture is taken, is added
10-35 parts of mass fractions are the emulsifier aqueous solution of 5-10%, and add 100-150 parts of deionized waters and appropriate pH buffer,
PH value is adjusted to 7-9, is uniformly mixed, obtains seed emulsion；It is uniformly added into the initiator that 3-6 parts of mass fractions are 3-6%
Aqueous solution, 20-60min is heated at 80-90 DEG C.
(2) low-temperature fixing emulsion resin is prepared, i.e., the follow-up emulsion polymerization stage.By remaining 85-95 parts of mixture, 15-50
The initiator solution that emulsifier aqueous solution that part mass fraction is 5-10%, 10-25 part mass fractions are 1-3%, respectively
In even addition reaction kettle, 150-200min is reacted, then reaction temperature is raised 2-5 DEG C and maintains stirring reaction 60-120min.Instead
After answering, it is evaporated under reduced pressure at 50-90 DEG C, volatile component is evaporated off, that is, low molecule or high-molecular low-temperature is prepared
Fixing emulsion resin.
(3) the low-temperature fixing chemistry ink powder resin-made stage is prepared.Prepare to obtain low molecule by (1) and (2) stage low
The fixing emulsion resin of temperature and high-molecular low-temperature are fixed emulsion resin, and low, the high-molecular low-temperature of preparation are fixed emulsion resin by one
Certainty ratio uniformly mixes, and wherein low molecule low-temperature fixing emulsion resin accounts for 60-90%, and high-molecular low-temperature is fixed emulsion resin and accounts for
10-40%, is 100% by the sum of both shared mass percents, proportioning obtains mixed emulsion resin, by the mixed emulsion resin
Solid content adjusts to 33.0% and obtains low-temperature fixing chemistry ink powder resin.
The low-temperature fixing chemistry ink powder resin that the above method is prepared, molecular chain conformation can match low-temperature fixing and beat
The softening point of print machine, available for the chemical ink powder for preparing laser printer or duplicator, and obtained chemical ink powder ambient storage
Property is good, will not stick roller.
Above-mentioned low-temperature fixing chemistry ink powder resin is several in the interpolymer latex of polystyrene and acrylic ester of different molecular weight
Kind mixture.
Above-mentioned phenylethylene alkenyl unsaturated monomer is styrene, methyl styrene, vinyltoluene, divinylbenzene
One or more combination；The esters of acrylic acid alkenyl unsaturated monomer is methyl methacrylate, methacrylic acid second
Ester, butyl methacrylate, isooctyl methacrylate, isobornyl methacrylate, lauryl methacrylate, acrylic acid
One kind in methyl esters, ethyl acrylate, n-butyl acrylate, isobutyl acrylate, Isooctyl acrylate monomer, lauryl acrylate or
Several combinations；The function monomer is acrylic acid, methacrylic acid, fumaric acid, itaconic acid, maleic acid, methacrylic acid carboxylic
Ethyl ester, hydroxymethyl acrylamide, hydroxyethyl methacrylate, hydroxy-ethyl acrylate, hydroxypropyl acrylate, methacrylic acid hydroxypropyl
One or more combination in ester.
Above-mentioned mercaptan type chain transfer agent is tert-butyl mercaptan, n-butyl mercaptan, spicy thioalcohol, decyl mercaptan, n- dodecyl mereaptan, uncle ten
One or more combination in two mercaptan, positive tetradecanylthioalcohol, positive 16 mercaptan, mercaptoethanol, thioacetic acid.
Above-mentioned emulsifying agent is anion emulsifier and/or nonionic emulsifier, and anion emulsifier is dodecyl sulphur
Sour sodium, lauryl sodium sulfate, neopelex, fatty alcohol polyoxyethylene ether sulfate, alkyl diphenyl ether sulfonate,
The combination of soap, aliphatic alcohol polyethenoxy ether carboxylate one or more, nonionic emulsifier are octylphenol polyethylene ethylene oxide
Ether, nonylphenol polyoxyethylene ether, polyoxyethylene alkyl-carboxylic acid ether, fatty alcohol polyoxyethylene ether, tween, the one or more of sapn
Combination.
Above-mentioned pH buffer is sodium acid carbonate, ammonium hydrogen carbonate, sodium dihydrogen phosphate, ammonium dihydrogen phosphate, ammonium hydroxide, hydroxide
One or both of sodium, sodium acetate combine.
Above-mentioned initiator is water soluble starter, and initiator is ammonium persulfate, sodium peroxydisulfate, potassium peroxydisulfate, peroxidating
One or two kinds of combinations of hydrogen, tert-butyl hydroperoxide, isopropyl benzene hydroperoxide, azo diisobutyl miaow hydrochloride.
Above-mentioned low molecule low-temperature fixing emulsion resin weight average molecular weight is controlled between 20000-100000, vitrifying temperature
Tg controls are spent at 45-65 DEG C；The high-molecular low-temperature be fixed emulsion resin weight average molecular weight control 100000-300000 it
Between, glass transition temperature Tg is controlled at 50-60 DEG C.Lotion tree is fixed by low molecule low-temperature fixing emulsion resin, high-molecular low-temperature
After fat is mixed in a certain ratio, the low-temperature fixing chemistry ink powder resin of preparation, available for manufacturing low smell, fast fixing, low temperature
Fixing xerography or static dump powder.
The low-temperature fixing chemistry ink powder resin-made is for the method for ink powder：Take the low-temperature fixing chemistry ink powder resin 20-
50 parts, 1-5 parts of colorant, 1-3 parts of charge adjusting agent CCA dispersion liquids, 1-3 parts of wax emulsion, the mixing of 40-70 parts of water, shear agitation is same
When be uniformly added into the dilute sulfuric acid that 5-15 parts of mass fractions are 2-4%, 50-65 DEG C is then heated to, when insulation 1-3 is small；Add 5-
The sodium hydroxide solution of 10 parts of 2-4%, adjusts pH=6-8, is warming up to 110-135 DEG C, when insulation 1-5 is small, then cooling discharge；
By drying after press filtration, then add 1-4 parts of auxiliary agents by every 100 parts of ink powders and obtain finished product low-temperature fixing chemistry ink after mixing
Powder.The applicable most low-temperature fixing laser printers of chemical ink powder of this method preparation, fixing effect are good, and transferring rate is high, and color is close
Spend excellent, chargeding performance is excellent, and production technology is environment friendly and pollution-free, production cost is relatively low, is suitable as production low temperature and determines
The method of shadow chemistry ink powder is applicable in.
In the above-mentioned method for preparing ink powder, the colorant uses following proportioning：Dispersant 5-15%, pigment 30-50%, water
50-75%, the sum of mass percent shared by each component are 100%；The CCA dispersion liquids use following proportioning：Dispersant 5-
15%th, CCA15-35%, water 65-75%, the sum of mass percent shared by each component are 100%；The wax emulsion is using following
Proportioning：Dispersant 5-15%, wax 15-35%, water 65-75%, the sum of mass percent shared by each component are 100%.
Mixing and dispersion technology in the preparation process of above-mentioned low-temperature fixing chemistry ink powder resin and ink powder are stirred including machinery
Mix, the method for high-speed stirred, high-pressure homogeneous, ball milling and/or sand milling.
The present invention has the advantages that：
(1) low-temperature fixing emulsion resin preparation process uses few mercaptan type chain transfer agent, finished product ink powder print procedure without
Peculiar smell；
(2) the low-temperature fixing chemistry ink powder resin is stablized without low molecular weight, ink powder preparation process is crossed, and ink powder drying is without caking
Phenomenon, printing do not stick roller, and print quality is good；
(3) chemical ink powder technological operation can be prepared according to traditional lotion co-agglomeration, technique is relatively easy, the production cycle
It is short, environmental protection and energy saving consumption；
(4) ink powder ambient storage stability is good, and auxiliary agent is not easy to be embedded in, and anticaking capacity is good.
The present invention is suitable as production low-temperature fixing chemistry ink powder resin and the method for the chemical ink powder of production uses, or similar
The improvement of method.
Brief description of the drawings
Fig. 1 is the flow diagram that the present invention prepares low-temperature fixing emulsion resin.
Fig. 2 is the flow diagram that the present invention prepares low-temperature fixing chemistry ink powder.
Embodiment
In conjunction with attached drawing, with specific embodiment, the invention will be further described.Except the present invention it is defined otherwise or explanation with
Outside, all specialties used herein or scientific words are identical with meaning familiar to those skilled in the art.In addition it is any with
The similar or impartial method of described content of the present invention and material all can be applied in the method for the present invention.
Material provided by the present invention can be synthesized by existing marketable material or traditional chemical transform mode.
Embodiment 1：
Configure 5% polyoxyethylene (10) alkyl-carboxylic acid ether aqueous solution of 820.0g mass fractions, and have 840.0g styrene,
The mix monomer of 330.0g n-butyl acrylates, 30.0g hydroxyethyl methacrylates and 6.0g methacrylic acids is (altogether
1206.0g)。
In the tetra- mouthfuls of reaction bulbs of 5000ml for being equipped with stirring motor, reflux condensing tube, thermometer and peristaltic pump, add
1500ml deionized waters, 300.0g polyoxyethylene (10) alkyl-carboxylic acid ether aqueous solution (mass fraction 5%), add 120.0g mixing
Monomer, starts stirring, and it is 8.2-8.6 to adjust pH value with ammonium hydroxide, heats the mixture to 82 DEG C, being uniformly added into 40.0g concentration is
3.5% ammonium persulfate aqueous solution, reacts 60min, and seed emulsion is prepared at 85 DEG C in maintenance system.Then it is residue is mixed
Monomer 1086.0g is closed, polyoxyethylene (10) alkyl-carboxylic acid ether aqueous solution (mass fraction 5%) 520.0g, 200.0g concentration is
2.0% ammonium persulfate aqueous solution, while reaction kettle is uniformly added into, maintain 85-86 DEG C and stir, time for adding is respectively
180min, 180min, 200min.After being added dropwise to complete, temperature is increased to 87 DEG C, the reaction was continued 120min.Carry out after reaction
Vacuum distillation, stops after distilling 60min at 20kPa, 87 DEG C.Reactant is cooled down, after filtering, obtained low-temperature fixing lotion
Resin (hereinafter referred to as emulsion resin) is denoted as A.This emulsion resin weight average molecular weight (is surveyed for 242300 with gel permeation chromatography
It is fixed), the glass transition temperature of polymer is determined as 49.0 DEG C through DSC.Emulsion resin melt index 5.1g/10min (125 DEG C,
15kg).Lotion is without n- dodecyl mereaptan characteristic odor.
Embodiment 2：
Configure 5% polyoxyethylene (10) alkyl-carboxylic acid ether aqueous solution of 820.0g mass fractions, and have 916.0g styrene,
248.0g n-butyl acrylates, 36.0g hydroxyethyl methacrylates, 2.0g methacrylic acids and 12.0g n- dodecyl mereaptans it is mixed
Close monomer (common 1214.0g).
In the tetra- mouthfuls of reaction bulbs of 5000ml for being equipped with stirring motor, reflux condensing tube, thermometer and peristaltic pump, add
1500ml deionized waters, 300.0g polyoxyethylene (10) alkyl-carboxylic acid ether aqueous solution (mass fraction 5%), add 120.0g mixing
Monomer, starts stirring, and it is 8.2-8.6 to adjust pH value with ammonium hydroxide, heats the mixture to 82 DEG C, being uniformly added into 40.0g concentration is
3.5% ammonium persulfate aqueous solution, reacts 60min, and seed emulsion is prepared at 85 DEG C in maintenance system.Then it is residue is mixed
Monomer 1094.0g is closed, polyoxyethylene (10) alkyl-carboxylic acid ether aqueous solution (mass fraction 5%) 520.0g, 200.0g concentration is
2.0% ammonium persulfate aqueous solution, while reaction kettle is uniformly added into, maintain 85-86 DEG C and stir, time for adding is respectively
180min, 180min, 200min.After being added dropwise to complete, temperature is increased to 87 DEG C, the reaction was continued 120min.Carry out after reaction
Vacuum distillation, stops after distilling 60min at 20kPa, 87 DEG C.Reactant is cooled down, after filtering, obtained emulsion resin is denoted as
B.This emulsion resin weight average molecular weight is 41200 (being measured with gel permeation chromatography), and the glass transition temperature of polymer passes through
DSC is determined as 56.5 DEG C.Emulsion resin melt index 12.7g/10min (110 DEG C, 10kg).Lotion is without obvious n- dodecyl mereaptan
Characteristic odor.
Embodiment 3：
Configure 5% polyoxyethylene (10) alkyl-carboxylic acid ether aqueous solution of 820.0g mass fractions, and have 720.0g styrene,
140.0g n-butyl acrylates, 300.0g n-BMAs, 40.0g hydroxyethyl methacrylates, 6.0g metering systems
The mix monomer (common 1218.0g) of acid and 12.0g n- dodecyl mereaptans.
In the tetra- mouthfuls of reaction bulbs of 5000ml for being equipped with stirring motor, reflux condensing tube, thermometer and peristaltic pump, add
1500ml deionized waters, 300.0g polyoxyethylene (10) alkyl-carboxylic acid ether aqueous solution (mass fraction 5%), add 120.0g mixing
Monomer, starts stirring, and it is 8.2-8.6 to adjust pH value with ammonium hydroxide, heats the mixture to 82 DEG C, being uniformly added into 40.0g concentration is
3.5% ammonium persulfate aqueous solution, reacts 60min, and seed emulsion is prepared at 85 DEG C in maintenance system.Then it is residue is mixed
Monomer 1098.0g is closed, polyoxyethylene (10) alkyl-carboxylic acid ether aqueous solution (mass fraction 5%) 520.0g, 200.0g concentration is
2.0% ammonium persulfate aqueous solution, while reaction kettle is uniformly added into, maintain 85-86 DEG C and stir, time for adding is respectively
180min, 180min, 200min.After being added dropwise to complete, temperature is increased to 87 DEG C, the reaction was continued 120min.Carry out after reaction
Vacuum distillation, stops after distilling 60min at 20kPa, 87 DEG C.Reactant is cooled down, after filtering, obtained emulsion resin is denoted as
C.This emulsion resin weight average molecular weight is 43100 (being measured with gel permeation chromatography), and the glass transition temperature of polymer passes through
DSC is determined as 46.2 DEG C.Emulsion resin melt index 10.1g/10min (100 DEG C, 10kg).Lotion is without obvious n- dodecyl mereaptan
Characteristic odor.
Embodiment 4：
Configure 5% polyoxyethylene (10) alkyl-carboxylic acid ether aqueous solution of 820.0g mass fractions, and have 990.0g styrene,
180.0g n-butyl acrylates, 30.0g hydroxyethyl methacrylates, 3.0g methacrylic acids and 18.0g n- dodecyl mereaptans it is mixed
Close monomer (common 1221.0g).
In the tetra- mouthfuls of reaction bulbs of 5000ml for being equipped with stirring motor, reflux condensing tube, thermometer and peristaltic pump, add
1500ml deionized waters, 300.0g polyoxyethylene (10) alkyl-carboxylic acid ether aqueous solution (mass fraction 5%), add 120.0g mixing
Monomer, starts stirring, and it is 8.2-8.6 to adjust pH value with ammonium hydroxide, heats the mixture to 82 DEG C, being uniformly added into 40.0g concentration is
3.5% ammonium persulfate aqueous solution, reacts 60min, and seed emulsion is prepared at 85 DEG C in maintenance system.Then it is residue is mixed
Monomer 1101.0g is closed, polyoxyethylene (10) alkyl-carboxylic acid ether aqueous solution (mass fraction 5%) 520.0g, 200.0g concentration is
2.0% ammonium persulfate aqueous solution, while reaction kettle is uniformly added into, maintain 85-86 DEG C and stir, time for adding is respectively
180min, 180min, 200min.After being added dropwise to complete, temperature is increased to 87 DEG C, the reaction was continued 120min.Carry out after reaction
Vacuum distillation, stops after distilling 60min at 20kPa, 87 DEG C.Reactant is cooled down, after filtering, obtained emulsion resin is denoted as
D.This emulsion resin weight average molecular weight is 28700 (being measured with gel permeation chromatography), and the glass transition temperature of polymer passes through
DSC is determined as 62.5 DEG C.Emulsion resin melt index 6.5g/10min (110 DEG C, 10kg).Lotion has slight n- dodecyl mereaptan spy
Levy smell.
Embodiment 5：
Configure 5% polyoxyethylene (10) alkyl-carboxylic acid ether aqueous solution of 820.0g mass fractions, and have 900.0g styrene,
270.0g n-butyl acrylates, 24.0g hydroxyethyl methacrylates, 6.0g methacrylic acids and 24.0g n- dodecyl mereaptans it is mixed
Close monomer (common 1224.0g).
In the tetra- mouthfuls of reaction bulbs of 5000ml for being equipped with stirring motor, reflux condensing tube, thermometer and peristaltic pump, add
1500ml deionized waters, 300.0g polyoxyethylene (10) alkyl-carboxylic acid ether aqueous solution (mass fraction 5%), add 120.0g mixing
Monomer, starts stirring, and it is 8.2-8.6 to adjust pH value with ammonium hydroxide, heats the mixture to 82 DEG C, being uniformly added into 40.0g concentration is
3.5% ammonium persulfate aqueous solution, reacts 60min, and seed emulsion is prepared at 85 DEG C in maintenance system.Then it is residue is mixed
Monomer 1104.0g is closed, polyoxyethylene (10) alkyl-carboxylic acid ether aqueous solution (mass fraction 5%) 520.0g, 200.0g concentration is
2.0% ammonium persulfate aqueous solution, while reaction kettle is uniformly added into, maintain 85-86 DEG C and stir, time for adding is respectively
180min, 180min, 200min.After being added dropwise to complete, temperature is increased to 87 DEG C, the reaction was continued 120min.Carry out after reaction
Vacuum distillation, stops after distilling 60min at 20kPa, 87 DEG C.Reactant is cooled down, after filtering, obtained emulsion resin is denoted as
E.This emulsion resin weight average molecular weight is 22300 (being measured with gel permeation chromatography), emulsion resin melt index 16.1g/
10min (100 DEG C, 10kg).The glass transition temperature of polymer is determined as 52.3 DEG C through DSC.Lotion has obvious positive 12 sulphur
Alcohol characteristic odor.
Embodiment 6：
200.0g emulsion resins A, 1800.0g emulsion resin B is taken, is stirred evenly, by the mixed emulsion resin solid content tune
Save to 33.0% and obtain low-temperature fixing chemistry ink powder resin：First.The low-temperature fixing chemistry ink powder resin first (abbreviation resin first)
T1/2Softening point is 114.7 DEG C through rheometer measurement.
The carbon black moisture that 1200.0g resin first, 100.0g are stablized by anion emulsifier is added in 5000ml reaction kettles
Dispersion liquid (solid content 30%, volume average particle size DV50 be 120nm), the Brazil waxs stablized by anion emulsifier of 80.0g
Lotion (solid content 25%, volume average particle size DV50 be 280nm), the charge control agents stablized by anion emulsifier of 50.0g
(CCA) aqueous dispersions (solid content 30%, volume average particle size DV50 be 300nm) and 2700ml deionized waters, stir evenly,
It is 2.5% sulfuric acid solution that concentration is added under high shear agitation, until pH value is down to 2.0-2.2, makes mixed liquor generation co-agglomeration.
Above-mentioned mixed liquor is warming up to 57 DEG C, when stirring reaction 2 is small.PH value is adjusted to 6.5-7.0 with diluted sodium hydroxide solution, will be reacted
Kettle pressurizes, and mixed liquor is heated to 118 DEG C, when insulation 3 is small.Obtained toner particles are filtered, are fully washed with deionized water, are done
It is dry, flow modifier auxiliary agent is added, such as fumed silica, is made ink powder, toner volume average grain diameter DV50 be 7.5 μm, grain
Footpath breadth coefficient (GSD) is 1.23 (by laser diffraction particle size analysis-e/or determinings).
Embodiment 7：
600.0g emulsion resins A, 1400.0g emulsion resin B is taken, is stirred evenly, by the mixed emulsion resin solid content tune
Save to 33.0% and obtain low-temperature fixing chemistry ink powder resin：Second.The low-temperature fixing chemistry ink powder resin second (abbreviation resin second)
T1/2Softening point is 117.2 DEG C through rheometer measurement.
1200.0g resins second is added in 5000ml reaction kettles, the carbon black moisture that 100.0g is stablized by anion emulsifier
Dispersion liquid (solid content 30%, volume average particle size DV50 be 120nm), the Brazil waxs stablized by anion emulsifier of 80.0g
Lotion (solid content 25%, volume average particle size DV50 be 280nm), the charge control agents stablized by anion emulsifier of 50.0g
(CCA) aqueous dispersions (solid content 30%, volume average particle size DV50 be 300nm) and 2700ml deionized waters, stir evenly,
It is 2.5% sulfuric acid solution that concentration is added under high shear agitation, until pH value is down to 2.0-2.2, makes mixed liquor generation co-agglomeration.
Above-mentioned mixed liquor is warming up to 57 DEG C, when stirring reaction 2 is small.PH value is adjusted to 6.5-7.0 with diluted sodium hydroxide solution, will be reacted
Kettle pressurizes, and mixed liquor is heated to 120 DEG C, when insulation 3 is small.Obtained toner particles are filtered, are fully washed with deionized water, are done
It is dry, flow modifier auxiliary agent is added, such as fumed silica, is made ink powder, toner volume average grain diameter DV50 be 7.3 μm, grain
Footpath breadth coefficient (GSD) is 1.21 (by laser diffraction particle size analysis-e/or determinings).
Embodiment 8：
200.0g emulsion resins A, 1600.0g emulsion resin B, 200.0g emulsion resin C is taken, stirs evenly, this is mixed
Emulsion resin solid content adjusts to 33.0% and obtains low-temperature fixing chemistry ink powder resin：Third.The low-temperature fixing chemistry ink powder resin
The T of third (abbreviation resin the third)1/2Softening point is 114.1 DEG C through rheometer measurement.
1200.0g resins third are added in 5000ml reaction kettles, the carbon black moisture that 100.0g is stablized by anion emulsifier
Dispersion liquid (solid content 30%, volume average particle size DV50 be 120nm), the Brazil waxs stablized by anion emulsifier of 80.0g
Lotion (solid content 25%, volume average particle size DV50 be 280nm), the charge control agents stablized by anion emulsifier of 50.0g
(CCA) aqueous dispersions (solid content 30%, volume average particle size DV50 be 300nm) and 2700ml deionized waters, stir evenly,
It is 2.5% sulfuric acid solution that concentration is added under high shear agitation, until pH value is down to 2.0-2.2, makes mixed liquor generation co-agglomeration.
Above-mentioned mixed liquor is warming up to 57 DEG C, when stirring reaction 2 is small.PH value is adjusted to 6.5-7.0 with diluted sodium hydroxide solution, will be reacted
Kettle pressurizes, and mixed liquor is heated to 118 DEG C, when insulation 3 is small.Obtained toner particles are filtered, are fully washed with deionized water, are done
It is dry, flow modifier auxiliary agent is added, such as fumed silica, is made ink powder, toner volume average grain diameter DV50 be 7.8 μm, grain
Footpath breadth coefficient (GSD) is 1.19 (by laser diffraction particle size analysis-e/or determinings).
Embodiment 9：
200.0g emulsion resins A, 1000.0g emulsion resin B, 800.0g emulsion resin C is taken, stirs evenly, this is mixed
Emulsion resin solid content adjusts to 33.0% and obtains low-temperature fixing chemistry ink powder resin：Fourth.The low-temperature fixing chemistry ink powder resin
The T of fourth (abbreviation resin fourth)1/2Softening point is 108.9 DEG C through rheometer measurement.
1200.0g resins fourth is added in 5000ml reaction kettles, the carbon black moisture that 100.0g is stablized by anion emulsifier
Dispersion liquid (solid content 30%, volume average particle size DV50 be 120nm), the Brazil waxs stablized by anion emulsifier of 80.0g
Lotion (solid content 25%, volume average particle size DV50 be 280nm), the charge control agents stablized by anion emulsifier of 50.0g
(CCA) aqueous dispersions (solid content 30%, volume average particle size DV50 be 300nm) and 2700ml deionized waters, stir evenly,
It is 2.5% sulfuric acid solution that concentration is added under high shear agitation, until pH value is down to 2.0-2.2, makes mixed liquor generation co-agglomeration.
Above-mentioned mixed liquor is warming up to 57 DEG C, when stirring reaction 2 is small.PH value is adjusted to 6.5-7.0 with diluted sodium hydroxide solution, will be reacted
Kettle pressurizes, and mixed liquor is heated to 115 DEG C, when insulation 3 is small.Obtained toner particles are filtered, are fully washed with deionized water, are done
It is dry, flow modifier auxiliary agent is added, such as fumed silica, is made ink powder, toner volume average grain diameter DV50 be 6.9 μm, grain
Footpath breadth coefficient (GSD) is 1.31 (by laser diffraction particle size analysis-e/or determinings).
Embodiment 10：
200.0g emulsion resins A, 1200.0g emulsion resin B, 600.0g emulsion resin C is taken, stirs evenly, this is mixed
Emulsion resin solid content adjusts to 33.0% and obtains low-temperature fixing chemistry ink powder resin：Penta.The low-temperature fixing chemistry ink powder resin
The T of penta (abbreviation resin penta)1/2Softening point is 107.4 DEG C through rheometer measurement.
1200.0g resins penta are added in 5000ml reaction kettles, the carbon black moisture that 100.0g is stablized by anion emulsifier
Dispersion liquid (solid content 30%, volume average particle size DV50 be 120nm), the Brazil waxs stablized by anion emulsifier of 80.0g
Lotion (solid content 25%, volume average particle size DV50 be 280nm), the charge control agents stablized by anion emulsifier of 50.0g
(CCA) aqueous dispersions (solid content 30%, volume average particle size DV50 be 300nm) and 2700ml deionized waters, stir evenly,
It is 2.5% sulfuric acid solution that concentration is added under high shear agitation, until pH value is down to 2.0-2.2, makes mixed liquor generation co-agglomeration.
Above-mentioned mixed liquor is warming up to 57 DEG C, when stirring reaction 2 is small.PH value is adjusted to 6.5-7.0 with diluted sodium hydroxide solution, will be reacted
Kettle pressurizes, and mixed liquor is heated to 115 DEG C, when insulation 3 is small.Obtained toner particles are filtered, are fully washed with deionized water, are done
It is dry, flow modifier auxiliary agent is added, such as fumed silica, is made ink powder, toner volume average grain diameter DV50 be 7.2 μm, grain
Footpath breadth coefficient (GSD) is 1.30 (by laser diffraction particle size analysis-e/or determinings).
Embodiment 11：
200.0g emulsion resins A, 1800.0g emulsion resin D is taken, is stirred evenly, by the mixed emulsion resin solid content tune
Save to 33.0% and obtain low-temperature fixing chemistry ink powder resin：Oneself.The low-temperature fixing chemistry ink powder resin oneself (abbreviation resin oneself)
T1/2Softening point is 118.2 DEG C through rheometer measurement.
The carbon black moisture that addition 1200.0g resins oneself, 100.0g are stablized by anion emulsifier in 5000ml reaction kettles
Dispersion liquid (solid content 30%, volume average particle size DV50 be 120nm), the Brazil waxs stablized by anion emulsifier of 80.0g
Lotion (solid content 25%, volume average particle size DV50 be 280nm), the charge control agents stablized by anion emulsifier of 50.0g
(CCA) aqueous dispersions (solid content 30%, volume average particle size DV50 be 300nm) and 2700ml deionized waters, stir evenly,
It is 2.5% sulfuric acid solution that concentration is added under high shear agitation, until pH value is down to 2.0-2.2, makes mixed liquor generation co-agglomeration.
Above-mentioned mixed liquor is warming up to 63 DEG C, when stirring reaction 2 is small.PH value is adjusted to 6.5-7.0 with diluted sodium hydroxide solution, will be reacted
Kettle pressurizes, and mixed liquor is heated to 125 DEG C, when insulation 3 is small.Obtained toner particles are filtered, are fully washed with deionized water, are done
It is dry, flow modifier auxiliary agent is added, such as fumed silica, is made ink powder, toner volume average grain diameter DV50 be 8.3 μm, grain
Footpath breadth coefficient (GSD) is 1.25 (by laser diffraction particle size analysis-e/or determinings).
Embodiment 12：
500.0g emulsion resins A, 1500.0g emulsion resin D is taken, is stirred evenly, by the mixed emulsion resin solid content tune
Save to 33.0% and obtain low-temperature fixing chemistry ink powder resin：Heptan.Low-temperature fixing chemistry ink powder resin heptan (abbreviation resin heptan)
T1/2Softening point is 122.0 DEG C through rheometer measurement.
1200.0g resins heptan is added in 5000ml reaction kettles, the carbon black moisture that 100.0g is stablized by anion emulsifier
Dispersion liquid (solid content 30%, volume average particle size DV50 be 120nm), the Brazil waxs stablized by anion emulsifier of 80.0g
Lotion (solid content 25%, volume average particle size DV50 be 280nm), the charge control agents stablized by anion emulsifier of 50.0g
(CCA) aqueous dispersions (solid content 30%, volume average particle size DV50 be 300nm) and 2700ml deionized waters, stir evenly,
It is 2.5% sulfuric acid solution that concentration is added under high shear agitation, until pH value is down to 2.0-2.2, makes mixed liquor generation co-agglomeration.
Above-mentioned mixed liquor is warming up to 63 DEG C, when stirring reaction 2 is small.PH value is adjusted to 6.5-7.0 with diluted sodium hydroxide solution, will be reacted
Kettle pressurizes, and mixed liquor is heated to 125 DEG C, when insulation 3 is small.Obtained toner particles are filtered, are fully washed with deionized water, are done
It is dry, flow modifier auxiliary agent is added, such as fumed silica, is made ink powder, toner volume average grain diameter DV50 be 8.5 μm, grain
Footpath breadth coefficient (GSD) is 1.21 (by laser diffraction particle size analysis-e/or determinings).
Embodiment 13：
400.0g emulsion resins A, 1600.0g emulsion resin E is taken, is stirred evenly, by the mixed emulsion resin solid content tune
Save to 33.0% and obtain low-temperature fixing chemistry ink powder resin：It is pungent.The low-temperature fixing chemistry ink powder resin pungent (abbreviation resin is pungent)
T1/2Softening point is 101.3 DEG C through rheometer measurement.
The carbon black moisture that 1200.0g resins are pungent, 100.0g is stablized by anion emulsifier is added in 5000ml reaction kettles
Dispersion liquid (solid content 30%, volume average particle size DV50 be 120nm), the Brazil waxs stablized by anion emulsifier of 80.0g
Lotion (solid content 25%, volume average particle size DV50 be 280nm), the charge control agents stablized by anion emulsifier of 50.0g
(CCA) aqueous dispersions (solid content 30%, volume average particle size DV50 be 300nm) and 2700ml deionized waters, stir evenly,
It is 2.5% sulfuric acid solution that concentration is added under high shear agitation, until pH value is down to 2.0-2.2, makes mixed liquor generation co-agglomeration.
Above-mentioned mixed liquor is warming up to 53 DEG C, when stirring reaction 2 is small.PH value is adjusted to 6.5-7.0 with diluted sodium hydroxide solution, will be reacted
Kettle pressurizes, and mixed liquor is heated to 105 DEG C, when insulation 3 is small.Obtained toner particles are filtered, are fully washed with deionized water, are done
It is dry, flow modifier auxiliary agent is added, such as fumed silica, is made ink powder, toner volume average grain diameter DV50 be 6.5 μm, grain
Footpath breadth coefficient (GSD) is 1.22 (by laser diffraction particle size analysis-e/or determinings).
Experimental method
Chemical ink powder prepared by 6-13 of the embodiment of the present invention is evaluated using following methods：
(1) it is fixed degree：The region of 10*10mm, first uses color at the center of 100% color density test sheets selection one
Densimeter measures its color density value, then sticks normal transparent glue, then slowly tears transparent adhesive tape off, and the color for measuring the region is close
Angle value, it is desirable to which color density value is greater than or equal to 90% with above the ratio between color density value below.
(2) transferring rate：Transferring rate=(always consuming powder+remaining powder)/(always consuming powder+remaining powder+useless powder), it is desirable to which transferring rate is more than or equal to
90%.
(3) resistance to packed and transported and transport storage capability：Tested according to mechanical industry standard JB/T 9444-1999.Survey
Ink powder print performance is normally then determined as qualification after examination, is otherwise determined as unqualified.
(4) anticaking capacity：Tested according to mechanical industry standard JB/T 8262.1-1999, ink powder is without caking after test
Then it is determined as qualification, is otherwise determined as unqualified.
Table 1 (emulsion property)：
| Embodiment | Numbering | Mw | Tg/℃ | Smell |
| 1 | A | 242300 | 49.0 | Nothing |
| 2 | B | 41200 | 56.5 | Nothing |
| 3 | C | 43100 | 46.2 | Nothing |
| 4 | D | 28700 | 62.5 | Slightly |
| 5 | E | 22300 | 52.3 | Substantially |
Table 2 (chemical ink powder performance test)：
Above content, it is intended to illustrate the technological means of the present invention, not limit the technical scope of the present invention.Art technology
Personnel are the present invention conspicuously improved or replace with reference to existing common knowledge, also fall into the protection of the claims in the present invention
Within the scope of.
Claims (9)
1. a kind of preparation method of low-temperature fixing chemistry ink powder resin, it is characterised in that including following preparation process：
1) seed emulsion is prepared, using alkenyl unsaturated monomer, the mixed mixture gross mass of mercaptan type chain transfer agent as 100 parts
Meter, the alkenyl unsaturated monomer include phenylethylene alkenyl unsaturated monomer, esters of acrylic acid alkenyl unsaturated monomer, contain
The unsaturated function monomer of hydroxyl or carboxylic group；Wherein described mercaptan type chain transfer agent accounts for the 0- of the mixture gross mass
1.5%；5-15 parts of mixture is taken, 10-35 parts of mass fractions is added and is the emulsifier aqueous solution of 5-10%, and add 100-150
Part deionized water and appropriate pH buffer, adjust pH value to 7-9, are uniformly mixed, obtain seed emulsion；It is uniformly added into 3-6
The initiator solution that part mass fraction is 3-6%, 20-60min is heated at 85-90 DEG C；
2) low-temperature fixing emulsion resin is prepared, the emulsification for being 5-10% by remaining 85-95 parts of mixture, 15-50 parts of mass fractions
Agent aqueous solution, 10-25 part mass fraction are the initiator solution of 1-3%, are uniformly added into respectively in reaction kettle, react 150-
200min, then reaction temperature is raised 2-5 DEG C and maintains stirring reaction 60-120min；After reaction, subtract at 50-90 DEG C
Pressure distillation, volatile component is evaporated off, that is, low molecule is prepared or high-molecular low-temperature is fixed emulsion resin；
3) low-temperature fixing chemistry ink powder resin is prepared, using low molecule low-temperature fixing emulsion resin mass percent as 60-90%, height
Molecule low-temperature fixing emulsion resin mass percent is 10-40%, is 100% by the sum of both shared mass percents, proportioning
Mixed emulsion resin is obtained, which is adjusted to 33.0% and obtains low-temperature fixing chemistry ink powder resin；
The low molecule low-temperature fixing emulsion resin weight average molecular weight control is between 20000-100000, glass transition temperature Tg controls
System is at 45-65 DEG C；The high-molecular low-temperature is fixed the control of emulsion resin weight average molecular weight between 100000-300000, glass
Change temperature Tg controls at 50-60 DEG C.
2. the preparation method of low-temperature fixing chemistry ink powder resin according to claim 1, it is characterised in that the low temperature
Fixing chemistry ink powder resin is several mixtures in the interpolymer latex of polystyrene and acrylic ester of different molecular weight.
3. the preparation method of low-temperature fixing chemistry ink powder resin according to claim 1 or 2, it is characterised in that：The benzene
Vinyl alkenyl unsaturated monomer for styrene, methyl styrene, vinyltoluene, one or more of groups of divinylbenzene
Close；The esters of acrylic acid alkenyl unsaturated monomer is methyl methacrylate, ethyl methacrylate, methacrylic acid fourth
Ester, isooctyl methacrylate, isobornyl methacrylate, lauryl methacrylate, methyl acrylate, acrylic acid second
One or more combination in ester, n-butyl acrylate, isobutyl acrylate, Isooctyl acrylate monomer, lauryl acrylate；It is described
Function monomer for acrylic acid, methacrylic acid, fumaric acid, itaconic acid, maleic acid, methacrylic acid carboxylic ethyl ester, methylol third
One kind in acrylamide, hydroxyethyl methacrylate, hydroxy-ethyl acrylate, hydroxypropyl acrylate, hydroxy propyl methacrylate or
Several combinations.
4. the preparation method of low-temperature fixing chemistry ink powder resin according to claim 1 or 2, it is characterised in that：Described
Mercaptan type chain transfer agent is tert-butyl mercaptan, n-butyl mercaptan, spicy thioalcohol, decyl mercaptan, n- dodecyl mereaptan, tert-dodecyl mercaptan, positive 14
One or more combination in mercaptan, positive 16 mercaptan, mercaptoethanol, thioacetic acid.
5. the preparation method of low-temperature fixing chemistry ink powder resin according to claim 1 or 2, it is characterised in that：Described
Emulsifying agent is anion emulsifier and/or nonionic emulsifier, and anion emulsifier is dodecyl sodium sulfate, dodecyl sulphur
Sour sodium, neopelex, fatty alcohol polyoxyethylene ether sulfate, alkyl diphenyl ether sulfonate, soap, fatty alcohol
The combination of polyethenoxy ether carboxylate one or more, nonionic emulsifier is octyl phenol polyoxyethylene ether, polyoxyethylene nonyl phenyl second
Alkene ether, polyoxyethylene alkyl-carboxylic acid ether, fatty alcohol polyoxyethylene ether, tween, the one or more combination of sapn.
6. the preparation method of low-temperature fixing chemistry ink powder resin according to claim 1 or 2, it is characterised in that：Described
PH buffer is one in sodium acid carbonate, ammonium hydrogen carbonate, sodium dihydrogen phosphate, ammonium dihydrogen phosphate, ammonium hydroxide, sodium hydroxide, sodium acetate
Kind or two kinds of combinations.
7. the preparation method of low-temperature fixing chemistry ink powder resin according to claim 1 or 2, it is characterised in that described draws
Hair agent is water soluble starter, and initiator is ammonium persulfate, sodium peroxydisulfate, potassium peroxydisulfate, hydrogen peroxide, tert-butyl hydroperoxide
One or two kinds of combinations of hydrogen, isopropyl benzene hydroperoxide, azo diisobutyl miaow hydrochloride.
8. a kind of low-temperature fixing chemistry ink powder resin-made with described in claim 1 is for the method for ink powder, it is characterised in for preparing
Method is：Take 20-50 parts of the low-temperature fixing chemistry ink powder resin, 1-5 parts of colorant, 1-3 parts of charge adjusting agent CCA dispersion liquids,
40-70 parts of 1-3 parts of wax emulsion, water mixing, shear agitation are uniformly added into the dilute sulfuric acid that 5-15 parts of mass fractions are 2-4% at the same time,
Then heat to 50-65 DEG C, when insulation 1-3 is small；The sodium hydroxide solution of 5-10 parts of 2-4% is added, adjusts pH=6-8, heating
To 110-135 DEG C, when insulation 1-5 is small, then cooling discharge；1-4 parts are added by drying after press filtration, then by every 100 parts of ink powders
Auxiliary agent obtains finished product low-temperature fixing chemistry ink powder after mixing.
9. low-temperature fixing chemistry ink powder resin-made according to claim 8 is for the method for ink powder, it is characterised in that the color
Material uses following proportioning：Dispersant 5-15%, pigment 30-50%, water 50-75%, the sum of mass percent is shared by each component
100%；The CCA dispersion liquids use following proportioning：Dispersant 5-15%, CCA15-35%, water 65-75%, shared by each component
The sum of mass percent is 100%；The wax emulsion uses following proportioning：Dispersant 5-15%, wax 15-35%, water 65-
75%, the sum of mass percent shared by each component is 100%.
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| CN113136014B (en) * | 2021-04-06 | 2022-09-09 | 东莞理工学院 | Styrene-acrylic emulsion, preparation method and application thereof |
| CN114989342A (en) * | 2022-05-30 | 2022-09-02 | 张家港威迪森化学有限公司 | Copolymer resin for positive charge ink powder and preparation method thereof |
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