CN104330960A - Anionic nano wax emulsion as well as preparation method and application thereof - Google Patents
Anionic nano wax emulsion as well as preparation method and application thereof Download PDFInfo
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- CN104330960A CN104330960A CN201410558852.2A CN201410558852A CN104330960A CN 104330960 A CN104330960 A CN 104330960A CN 201410558852 A CN201410558852 A CN 201410558852A CN 104330960 A CN104330960 A CN 104330960A
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Abstract
The invention relates to a stable anionic nano wax emulsion as well as a preparation method and application thereof. The preparation process of the nano wax emulsion comprises the following steps: (1) heating wax and a surfactant until the temperature is greater than the melting point of the wax, and then stirring until the wax and the surfactant are uniformly mixed; (2) adding an aqueous solution of the surfactant into a system of the step (1), performing emulsification reaction, and continuously stirring after the reaction is ended until the system is cooled to room temperature so as to obtain the nano wax emulsion. The preparation process is safe, simple and environment-friendly; the prepared anionic nano wax emulsion can be stably stored; when the anionic nano wax emulsion is applied to a gathering and combining method, colored ink powder which is high in yield and can meet the requirement on high-quality laser printing or electrostatic copying (such as brightening and demolding) can be obtained.
Description
Technical field
The invention belongs to wax emulsion and preparation field thereof, be specifically related to a kind of anionic nanometer paraffin wax emulsion and preparation method thereof and application.
Background technology
Toner (also claims ink powder or carbon dust, Toner) be laser printing or xerographi main consumptive material, its fundamental component comprises resin, pigment, lubricant (wax) and charge control agent (CCA) etc., be (generally account for 70 – 90wt.%) based on resin can charged powder body material.
The preparation method of toner comprises Physical and chemical method.Toner particle prepared by chemical method has function admirable (the regular spherical in shape or elliposoidal of powder shape, all even particle size distribution of composition are narrow), be applicable to preparation high-quality toner, and there is production run low power consumption and other advantages, so be subject to the favor in market.And the agglomeration step of gathering-fusion method powder process conventional in chemical method generally completes under adjust ph condition, the uniform composition in each emulsion is assembled, and this just requires that each composition has enough little particle diameter.
Wax emulsion is a kind of dispersed system utilizing emulsifying agent wax and water to be formed through emulsion process.Because wax emulsion is with water to replace organic solvent, environmental pollution can be reduced widely, be conducive to environmental protection, and there is safety, the advantage such as efficient, economic and easy to use, so the development and utilization of wax emulsion has society and economic worth widely.
On the other hand, because wax itself has very strong hydrophobicity, be not easy to be dispersed in aqueous phase.This situation easily produces distinct issues, namely can not stablize within a certain period of time and deposit after the uneven or dispersion of the dispersion of wax, easily form oarse-grained gathering, make toner particle assemble formed time uneven components, the requirement of blast and demoulding can not be met, the quality that impact prints; Produce a large amount of useless powder in addition, affect yield.Therefore, this problems demand of wax emulsion that gathering-fusion method technology is used improves.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of nanometer paraffin wax emulsion.
The preparation method of nanometer paraffin wax emulsion of the present invention comprises the steps:
1) wax and surfactant are heated to more than the fusing point of wax, are then stirred to wax and surfactant mixes; Described surfactant is anionic surfactant or anionic surfactant and neutral surface active agent is the potpourri that (2:1) ~ (8:1) forms according to mass ratio;
2) again to step 1) system in add the aqueous solution of surfactant and carry out emulsion reaction, emulsion reaction terminates rear continuation and stirs until system is cooled to room temperature, obtains described nanometer paraffin wax emulsion.
In above-mentioned preparation method, step 1) in, described wax is selected from following at least one: Tissuemat E, polypropylene wax, natural wax, ester type waxes and palm wax; Described natural wax is specially beeswax; Described ester type waxes is specially Clariant Licowax E; Described palm wax is specially Brazil wax.
The hydrophilic-hydrophobic balance value (HLB) of described surfactant is 10 ~ 30.
Described surfactant is specifically selected from following at least one: AEO (i.e. peregal), neopelex, NaLS, sorbitan mono-oleic acid ester (namely taking charge of class 80) and sodium oleate.
The mass ratio of described wax and surfactant is (3:1) ~ (10:1).
The fusing point of described wax is 50 DEG C ~ 130 DEG C.
Described more than the fusing point of wax that is heated to is for being heated above described wax fusing point 10 DEG C ~ 40 DEG C.
The rotating speed of described stirring is 100rpm ~ 1500rpm, is specially 500rpm ~ 600rpm.
The time of described stirring is 1h ~ 2h.
In above-mentioned preparation method, step 2) in, described surfactant is selected from anionic surfactant and/or neutral surface active agent, is specifically selected from following at least one: neopelex, NaLS, sodium oleate, AEO (i.e. peregal), sorbitan mono-oleic acid ester (namely taking charge of class 80) and potassium oleate.
In the aqueous solution of described surfactant, the massfraction of surfactant is 0.1% ~ 3%.
The aqueous solution quality of described surfactant and step 1) described in the ratio of quality sum of wax and surfactant be (3:1) ~ (10:1).
Described emulsion reaction mulser realizes, and the rotating speed of described mulser is 10000rpm ~ 20000rpm, is specially 10000rpm.
The temperature of described emulsion reaction is 50 DEG C ~ 150 DEG C, is specially 90 DEG C ~ 100 DEG C.
The time of described emulsion reaction is 5min ~ 20min.
The number of times of described emulsion reaction is 2 times ~ 4 times.
The rotating speed of described stirring is 1000rpm ~ 2000rpm.
The time of described stirring is 0.5h ~ 3h, is specially 1h.
Another object of the present invention is to provide a kind of nanometer paraffin wax emulsion prepared by described preparation method.
Described nanometer paraffin wax emulsion is anionic.
In described nanometer paraffin wax emulsion, the particle diameter of nanometer paraffin wax is 50nm ~ 150nm.
Further object of the present invention is to provide a kind of described nanometer paraffin wax emulsion preparing the application in ink powder.
Described ink powder is color toner.
Described being applied as prepares application in color toner at routine gathering-fusion method.
The basic process of described conventional gathering-fusion method is: first utilize emulsion polymerization to prepare the water base serum of resin balls, prepare the pigment of aqueous medium more respectively, wax dispersion (i.e. wax emulsion) and charge adjusting agent, by above-mentioned each feed composition mixing and stirring, by regulation system pH value or ionic strength, induction particle is close to each other, progressively pool cluster, heating makes cluster grow up, add other surfactant when reaching required size again to increase further to limit it, heat on plexiglas temperature Tg, impel loose cluster to bond and form compact texture granule, collect, dry and add other acceptable necessary compositions, obtain ink powder.
Compared with prior art, tool of the present invention has the following advantages, by adopting agent-in-oil method, by wax and high hlb surfactant (being convenient to form stable oil-in-water and O/W structure) Homogeneous phase mixing, wax is dispersed in aqueous phase uniformly and stably, but not in organic phase solvent, avoid environmental pollution, and there is the advantages such as safe, efficient, economic and easy to use; Prepared anionic nanometer paraffin wax emulsion can be stablized and deposits, and it can be made to occur to assemble formation cluster by adjust ph, and then breakdown of emulsion is separated out, be convenient to do in ink powder and wrap up wax, be applied to can obtain high yield in gathering-fusion method and the color toner of high-quality laser printing or xerox requirement (as blast and demoulding) can be met.
Embodiment
Be described method of the present invention below by specific embodiment, but the present invention is not limited thereto, all any amendments done within the spirit and principles in the present invention, equivalent replacement and improvement etc., all should be included within protection scope of the present invention.
Experimental technique described in following embodiment, if no special instructions, is conventional method; Described reagent and material, if no special instructions, all can obtain from commercial channels.
Embodiment one: the preparation of nanometer paraffin wax emulsion
In 500 milliliters of reactors, (model is to add 20 grams of Tissuemat Es
400, fusing point MP81 DEG C), 1 gram of paregal O-20 and 2 grams of neopelexes, being heated to 95 DEG C, stirring (500rpm) 2 little of mixing completely;
Slowly add the deionized water 175 milliliters containing 1 gram of neopelex again, with mulser (10000rpm) process at 100 DEG C, emulsification twice, each 5min, then strong stirring (1000rpm) 1 hour, be quickly cooled to room temperature, prevent wax drop from high temperature assembling, stable nanometer paraffin wax emulsion can be obtained, recording its mean grain size with Malvern laser particle analyzer is 90nm, solid content is 10wt.%, preparation-obtained nanometer paraffin wax emulsion is left standstill placement after 15 days, nanometer paraffin wax emulsion there will not be lamination, energy stable existence, and nanometer paraffin wax emulsion even particle size distribution, domain size distribution is narrower.
Embodiment two: the preparation of nanometer paraffin wax emulsion
In 500 milliliters of reactors, add 40 grams of beeswaxs (fusing point MP63 DEG C), 1.5 grams of paregal Os-20,2 grams of NaLSs and 0.5 gram of class 80 of department, being heated to 90 DEG C, stirring (600rpm) 1 little of mixing completely;
Slowly add the deionized water 155 milliliters containing 1 gram of NaLS again, with mulser (20000rpm) process at 90 DEG C, emulsification twice, each 5min, then strong stirring (2000rpm) 1 hour; Make it rapidly cooling to room temperature, prevent wax drop from high temperature assembling, nanometer paraffin wax emulsion that can be stable, recording mean grain size with Malvern laser particle analyzer is 100nm, and solid content is 20wt.%.Preparation-obtained nanometer paraffin wax emulsion is left standstill placement after 15 days, nanometer paraffin wax emulsion there will not be lamination, and energy stable existence, and nanometer paraffin wax emulsion even particle size distribution, domain size distribution is narrower.
Embodiment three: the preparation of powdered black ink
In the pressure reaction still of 500 milliliters, add the nanometer paraffin wax emulsion (15 grams, 20wt.%) prepared by embodiment two, resin emulsion (150 grams, 20wt.%, commercial commodity), carbon black aqueous-based dispersions (40 grams, 15wt.%, commercial commodity) and charge adjusting agent zinc salicylate aqueous-based dispersions (5 grams, 10wt.%, commercial commodity), then add the deionized water 100 grams containing 1 gram of neopelex, mixing and stirring;
The pH value of regulation system to about 1, and is heated to 60 DEG C, strong stirring (5000rpm) 2 hours, and raised temperature to 95 DEG C stirs 5 hours; Cool, filter, wash, dry, obtain ink powder (powder is subsphaeroidal, and mean grain size is 8 μm), then (as: 20nm improved silica, marque is Degussa to be incorporated as the fluidity enhancers of toner mass 2%
202) external additive such as, obtains being applicable to laser printing or xerographi powdered black ink.
Adopt the preparation method of as above embodiment three, use yellow uitramarine (as: pigment yellow-83), product look pigment (as: paratonere-122) or green pigment (as: phthalocyanine ketone) dispersion liquid to replace black pigment dispersion liquid (as: the carbon black aqueous-based dispersions in embodiment three) respectively, can obtain being applicable to the Huang of color laser printing, product or cyan ink powder.
Claims (10)
1. a preparation method for nanometer paraffin wax emulsion, comprises the steps:
1) wax and surfactant are heated to after more than the fusing point of wax, are then stirred to wax and surfactant mixes; Described surfactant is anionic surfactant or anionic surfactant and neutral surface active agent is the potpourri that (2:1) ~ (8:1) forms according to mass ratio;
2) again to step 1) system in add the aqueous solution of surfactant and carry out emulsion reaction, emulsion reaction terminates rear continuation and stirs until system is cooled to room temperature, obtains described nanometer paraffin wax emulsion.
2. preparation method according to claim 1, is characterized in that: step 1) in, described wax is selected from following at least one: Tissuemat E, polypropylene wax, natural wax, ester type waxes and palm wax;
Described natural wax is beeswax;
Described ester type waxes is Clariant Licowax E wax;
Described palm wax is Brazil wax.
3. preparation method according to claim 1 or 2, is characterized in that: step 1) in, the hydrophilic-hydrophobic balance value of described surfactant is 10 ~ 30;
Described surfactant is selected from following at least one: AEO, neopelex, NaLS, sorbitan mono-oleic acid ester and sodium oleate.
4. preparation method according to any one of claim 1-3, is characterized in that: the mass ratio of described wax and surfactant is (3:1) ~ (10:1);
The fusing point of described wax is 50 DEG C ~ 130 DEG C;
Described more than the fusing point of wax that is heated to is for being heated above described wax fusing point 10 DEG C ~ 40 DEG C;
The rotating speed of described stirring is 100rpm ~ 1500rpm;
The time of described stirring is 1h ~ 2h.
5. preparation method according to any one of claim 1-4, it is characterized in that: step 2) in, described surfactant is selected from anionic surfactant and/or neutral surface active agent, is specifically selected from following at least one: neopelex, NaLS, sodium oleate, AEO, sorbitan mono-oleic acid ester and potassium oleate;
In the aqueous solution of described surfactant, the massfraction of surfactant is 0.1% ~ 3%;
The aqueous solution quality of described surfactant and step 1) described in the ratio of quality sum of wax and surfactant be (3:1) ~ (10:1).
6. preparation method according to any one of claim 1-5, is characterized in that: step 2) in, described emulsion reaction mulser realizes, and the rotating speed of described mulser is 10000rpm ~ 20000rpm;
The temperature of described emulsion reaction is 50 DEG C ~ 150 DEG C;
The time of described emulsion reaction is 5min ~ 20min;
The number of times of described emulsion reaction is 2 times ~ 4 times;
The rotating speed of described stirring is 1000rpm ~ 2000rpm;
The time of described stirring is 0.5h ~ 3h.
7. the nanometer paraffin wax emulsion that preparation method prepares according to any one of claim 1-6.
8. nanometer paraffin wax emulsion according to claim 7, is characterized in that: described nanometer paraffin wax emulsion is anionic;
In described nanometer paraffin wax emulsion, the particle diameter of nanometer paraffin wax is 50nm ~ 150nm.
9. nanometer paraffin wax emulsion described in claim 7 or 8 is preparing the application in ink powder.
10. apply according to claim 9, it is characterized in that: described ink powder is color toner;
Described being applied as prepares application in color toner at routine gathering-fusion method.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106243743A (en) * | 2016-08-15 | 2016-12-21 | 张枫浩 | A kind of self-emulsified microcrystalline wax and preparation method thereof |
| CN107239014A (en) * | 2017-07-24 | 2017-10-10 | 南京理工大学 | The color toner and method prepared using mini-emulsion polymerization and ball-milling |
| CN109207063A (en) * | 2018-08-06 | 2019-01-15 | 湖州赛德新材料科技有限公司 | A kind of solid wood furniture protection wax and preparation method thereof |
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| CN101250436A (en) * | 2008-04-08 | 2008-08-27 | 上海焦耳蜡业有限公司 | Method for preparing nano micro-emulsified wax |
| CN102718911A (en) * | 2012-06-18 | 2012-10-10 | 中国科学院化学研究所 | Wax wrapped type nano resin emulsion and preparation method and application thereof |
| CN102736458A (en) * | 2012-07-03 | 2012-10-17 | 邯郸汉光办公自动化耗材有限公司 | Method for preparing black and colorful powdered ink by gathering-fusing method |
| CN102809905A (en) * | 2012-08-14 | 2012-12-05 | 西北工业大学 | Method for preparing chemical carbon powder by coagulation on basis of modified latex particles and modified pigment emulsion |
| US8691488B2 (en) * | 2012-03-29 | 2014-04-08 | Xerox Corporation | Toner process |
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2014
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Patent Citations (5)
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| CN101250436A (en) * | 2008-04-08 | 2008-08-27 | 上海焦耳蜡业有限公司 | Method for preparing nano micro-emulsified wax |
| US8691488B2 (en) * | 2012-03-29 | 2014-04-08 | Xerox Corporation | Toner process |
| CN102718911A (en) * | 2012-06-18 | 2012-10-10 | 中国科学院化学研究所 | Wax wrapped type nano resin emulsion and preparation method and application thereof |
| CN102736458A (en) * | 2012-07-03 | 2012-10-17 | 邯郸汉光办公自动化耗材有限公司 | Method for preparing black and colorful powdered ink by gathering-fusing method |
| CN102809905A (en) * | 2012-08-14 | 2012-12-05 | 西北工业大学 | Method for preparing chemical carbon powder by coagulation on basis of modified latex particles and modified pigment emulsion |
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| CN106243743A (en) * | 2016-08-15 | 2016-12-21 | 张枫浩 | A kind of self-emulsified microcrystalline wax and preparation method thereof |
| CN107239014A (en) * | 2017-07-24 | 2017-10-10 | 南京理工大学 | The color toner and method prepared using mini-emulsion polymerization and ball-milling |
| CN109207063A (en) * | 2018-08-06 | 2019-01-15 | 湖州赛德新材料科技有限公司 | A kind of solid wood furniture protection wax and preparation method thereof |
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Application publication date: 20150204 |