CN117186437A - Wax emulsion and method for preparing micro-powder wax - Google Patents
Wax emulsion and method for preparing micro-powder wax Download PDFInfo
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- 239000000839 emulsion Substances 0.000 title claims abstract description 81
- 238000000034 method Methods 0.000 title claims abstract description 18
- 239000000843 powder Substances 0.000 title abstract description 34
- 239000002245 particle Substances 0.000 claims abstract description 41
- 239000004698 Polyethylene Substances 0.000 claims abstract description 33
- -1 polyethylene Polymers 0.000 claims abstract description 31
- 229920000573 polyethylene Polymers 0.000 claims abstract description 27
- 239000004094 surface-active agent Substances 0.000 claims abstract description 24
- 239000002736 nonionic surfactant Substances 0.000 claims abstract description 17
- 238000009826 distribution Methods 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 9
- 150000002191 fatty alcohols Chemical class 0.000 claims description 26
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 20
- 229920005682 EO-PO block copolymer Polymers 0.000 claims description 13
- 235000013873 oxidized polyethylene wax Nutrition 0.000 claims description 11
- 239000007787 solid Substances 0.000 claims description 11
- 238000001694 spray drying Methods 0.000 claims description 11
- 239000004209 oxidized polyethylene wax Substances 0.000 claims description 10
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 8
- 238000002844 melting Methods 0.000 claims description 7
- 230000008018 melting Effects 0.000 claims description 7
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 6
- 239000007921 spray Substances 0.000 claims description 6
- 239000012530 fluid Substances 0.000 claims description 5
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 4
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 4
- 229920000570 polyether Polymers 0.000 claims description 4
- 229920001451 polypropylene glycol Polymers 0.000 claims description 4
- 229920006395 saturated elastomer Polymers 0.000 claims description 4
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 3
- 125000000217 alkyl group Chemical group 0.000 claims description 3
- 125000006353 oxyethylene group Chemical group 0.000 claims description 3
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 3
- 235000019422 polyvinyl alcohol Nutrition 0.000 claims description 3
- 150000003573 thiols Chemical class 0.000 claims description 3
- 229920001400 block copolymer Polymers 0.000 claims description 2
- 229920002678 cellulose Polymers 0.000 claims description 2
- 150000002170 ethers Chemical class 0.000 claims description 2
- 239000001913 cellulose Substances 0.000 claims 1
- 239000001993 wax Substances 0.000 abstract description 159
- 239000003973 paint Substances 0.000 abstract description 14
- 239000000654 additive Substances 0.000 abstract description 3
- 230000000996 additive effect Effects 0.000 abstract description 3
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 description 9
- 239000000047 product Substances 0.000 description 9
- 238000012360 testing method Methods 0.000 description 6
- 238000002360 preparation method Methods 0.000 description 5
- 239000002994 raw material Substances 0.000 description 5
- RNMDNPCBIKJCQP-UHFFFAOYSA-N 5-nonyl-7-oxabicyclo[4.1.0]hepta-1,3,5-trien-2-ol Chemical compound C(CCCCCCCC)C1=C2C(=C(C=C1)O)O2 RNMDNPCBIKJCQP-UHFFFAOYSA-N 0.000 description 4
- 230000000844 anti-bacterial effect Effects 0.000 description 4
- 239000003899 bactericide agent Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 239000006185 dispersion Substances 0.000 description 4
- 238000010902 jet-milling Methods 0.000 description 4
- 239000007788 liquid Substances 0.000 description 4
- 239000004810 polytetrafluoroethylene Substances 0.000 description 4
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 241000209504 Poaceae Species 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- CBTVGIZVANVGBH-UHFFFAOYSA-N aminomethyl propanol Chemical compound CC(C)(N)CO CBTVGIZVANVGBH-UHFFFAOYSA-N 0.000 description 3
- 238000011156 evaluation Methods 0.000 description 3
- 150000007529 inorganic bases Chemical class 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000004005 microsphere Substances 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 150000007530 organic bases Chemical class 0.000 description 3
- 238000005507 spraying Methods 0.000 description 3
- 229940058020 2-amino-2-methyl-1-propanol Drugs 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 238000005299 abrasion Methods 0.000 description 2
- 238000007796 conventional method Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- MGIYRDNGCNKGJU-UHFFFAOYSA-N isothiazolinone Chemical compound O=C1C=CSN1 MGIYRDNGCNKGJU-UHFFFAOYSA-N 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000004200 microcrystalline wax Substances 0.000 description 2
- 238000001000 micrograph Methods 0.000 description 2
- 229920001983 poloxamer Polymers 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- XFRVVPUIAFSTFO-UHFFFAOYSA-N 1-Tridecanol Chemical compound CCCCCCCCCCCCCO XFRVVPUIAFSTFO-UHFFFAOYSA-N 0.000 description 1
- MPNXSZJPSVBLHP-UHFFFAOYSA-N 2-chloro-n-phenylpyridine-3-carboxamide Chemical compound ClC1=NC=CC=C1C(=O)NC1=CC=CC=C1 MPNXSZJPSVBLHP-UHFFFAOYSA-N 0.000 description 1
- BFSVOASYOCHEOV-UHFFFAOYSA-N 2-diethylaminoethanol Chemical compound CCN(CC)CCO BFSVOASYOCHEOV-UHFFFAOYSA-N 0.000 description 1
- DKPFZGUDAPQIHT-UHFFFAOYSA-N Butyl acetate Natural products CCCCOC(C)=O DKPFZGUDAPQIHT-UHFFFAOYSA-N 0.000 description 1
- RUPBZQFQVRMKDG-UHFFFAOYSA-M Didecyldimethylammonium chloride Chemical compound [Cl-].CCCCCCCCCC[N+](C)(C)CCCCCCCCCC RUPBZQFQVRMKDG-UHFFFAOYSA-M 0.000 description 1
- IAYPIBMASNFSPL-UHFFFAOYSA-N Ethylene oxide Chemical group C1CO1 IAYPIBMASNFSPL-UHFFFAOYSA-N 0.000 description 1
- UEEJHVSXFDXPFK-UHFFFAOYSA-N N-dimethylaminoethanol Chemical compound CN(C)CCO UEEJHVSXFDXPFK-UHFFFAOYSA-N 0.000 description 1
- 239000004721 Polyphenylene oxide Substances 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 125000000129 anionic group Chemical group 0.000 description 1
- 239000003945 anionic surfactant Substances 0.000 description 1
- 239000012752 auxiliary agent Substances 0.000 description 1
- 230000003115 biocidal effect Effects 0.000 description 1
- 239000003139 biocide Substances 0.000 description 1
- 125000002091 cationic group Chemical group 0.000 description 1
- 239000003093 cationic surfactant Substances 0.000 description 1
- 235000010980 cellulose Nutrition 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
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- 239000013065 commercial product Substances 0.000 description 1
- 229960002887 deanol Drugs 0.000 description 1
- 239000012972 dimethylethanolamine Substances 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- LRMHFDNWKCSEQU-UHFFFAOYSA-N ethoxyethane;phenol Chemical compound CCOCC.OC1=CC=CC=C1 LRMHFDNWKCSEQU-UHFFFAOYSA-N 0.000 description 1
- 239000000499 gel Substances 0.000 description 1
- 150000002327 glycerophospholipids Chemical class 0.000 description 1
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 description 1
- 239000004615 ingredient Substances 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- JPMIIZHYYWMHDT-UHFFFAOYSA-N octhilinone Chemical compound CCCCCCCCN1SC=CC1=O JPMIIZHYYWMHDT-UHFFFAOYSA-N 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000000016 photochemical curing Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000002285 radioactive effect Effects 0.000 description 1
- 150000003384 small molecules Chemical class 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
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- Paints Or Removers (AREA)
Abstract
The present application relates to wax emulsions and methods for preparing micronized waxes. The wax emulsion comprises polyethylene wax or Fischer-Tropsch wax, a high molecular weight nonionic surfactant, a low molecular weight surfactant, and water. The micro powder wax prepared by the wax emulsion and the method has a spherical shape and the particle size can be controlled within 20 microns so as to meet the requirements of different application fields on different particle sizes. Meanwhile, the obtained micro powder wax has narrow particle size distribution and good dispersibility. The film formed by the ink or the paint containing the micro powder wax as the additive has the characteristics of high transparency and gloss, good hand feeling, good wear resistance, good scratch resistance and the like.
Description
Technical Field
The application relates to the field of preparation of micro powder wax. In particular, the present application relates to wax emulsions and methods for preparing micronized waxes.
Background
At present, there are two main modes for producing micro-powder wax, one of which is a jet milling mode. For example, CN102806132a discloses a preparation method of a PE/PTFE mixed micro powder wax for UV photo-curing ink, which is characterized in that the preparation method comprises the following steps of: a) Radiating PE and PTFE resin in a radiation environment by using radioactive rays; b) The PE, PTFE resin and auxiliary agent after radiation are put into a millstone crusher for coarse crushing; c) Carrying out jet milling on the coarsely milled material at normal temperature by using a jet mill; d) And adjusting a particle size grading device of the jet mill to prepare the PE/PTFE mixed micro powder wax.
The micro powder wax produced by the jet milling method has the following characteristics: one is non-spherical, i.e. random; secondly, the particle size distribution is relatively wide. Because of technical limitations, jet milling does not produce a micronized wax product having a relatively small or softer particle size. At the same time, the characteristics of the product limit the application of the product in some fields. For example, in ink applications, irregular micro-powder waxes result in poorer gloss and transparency of the ink.
Another way is known as melt spraying. For example, US5185108 discloses a method of producing wax microspheres from molten wax comprising (a) flowing a molten wax-immiscible thermodynamic liquid through a molten wax-forming orifice of the molten wax to form a dispersion of molten wax; (b) Supplying the molten wax to the pore region of the orifice such that the wax is a dispersed phase and the thermodynamic liquid is a continuous phase in the formed dispersion; (c) Discharging the dispersion into a solidifying liquid immiscible therein, the solidifying liquid being maintained at a controlled temperature below the initial melting point of the wax; (d) Recovering substantially spherical wax microspheres having a bilayer weight distribution, and (e) drying to recover free flowing individual wax microspheres.
The micro powder wax produced by the melt spraying method has the following characteristics: firstly, the product is spherical; secondly, the particle size distribution is relatively wide. In addition, melt spraying methods also fail to produce a micronized wax product having a relatively small particle size.
Thus, there is a need for a process that can be used to prepare spherical and particle size adjustable micro powder waxes.
Disclosure of Invention
It is an object of the present application to provide a process for preparing a micronized wax that can produce a micronized wax that is spherical and has an adjustable particle size.
It is another object of the present application to provide a wax emulsion for preparing a micro powder wax which can be used to prepare a micro powder wax having a spherical shape and an adjustable particle size.
The aim of the application can be achieved by the following technical scheme.
According to a first aspect of the present application there is provided a wax emulsion for use in the preparation of a micronized wax, characterised in that it comprises, based on the total weight of the wax emulsion:
15 to 45 wt% of a polyethylene wax or a fischer-tropsch wax;
0.1 to 10 wt% of a high molecular weight nonionic surfactant;
1 to 10 wt% of a low molecular weight surfactant; and
30-80% by weight of water.
According to a second aspect of the present application, there is provided a process for preparing a micronized wax, comprising:
providing a wax emulsion according to the first aspect of the application and optionally adjusting its solids content; and
the wax emulsion is spray dried to obtain a micronized wax.
According to a third aspect of the present application, there is provided a micro powder wax characterized in that it is obtained using the wax emulsion described above.
The micro powder wax prepared by the wax emulsion and the method has a spherical shape and the particle size can be controlled within 20 microns so as to meet the requirements of different application fields on different particle sizes. Meanwhile, the obtained micro powder wax has narrow particle size distribution and good dispersibility. The film formed by the ink or the paint containing the micro powder wax as the additive has the characteristics of high transparency and gloss, good hand feeling, good wear resistance, good scratch resistance and the like.
Drawings
The application is described and explained in more detail below with reference to the attached drawing figures, wherein:
FIG. 1 is a micrograph of the micro wax P-2 prepared in example 8.
FIG. 2 is a particle size distribution of the fine powder wax P-2 prepared in example 8.
Detailed Description
Various aspects, as well as further objects, features, and advantages of the present application will be more fully apparent hereinafter.
According to a first aspect of the present application there is provided a wax emulsion for use in the preparation of a micronized wax, characterised in that it comprises, based on the total weight of the wax emulsion:
15 to 45 wt% of a polyethylene wax or a fischer-tropsch wax;
0.1 to 10 wt% of a high molecular weight nonionic surfactant;
1 to 10 wt% of a low molecular weight surfactant; and
30-80% by weight of water.
The term "wax" as used herein is generally defined as an organic small molecule substance that is solid at room temperature but has a relatively low viscosity after melting above its melting point, is insoluble in water and any organic solvents, but can be uniformly dispersed as a dispersed phase in the above-mentioned medium.
Advantageously, the wax in the wax emulsion has a molecular weight in the range 800 to 20,000 g/mol, preferably in the range 1000-6000 g/mol.
Advantageously, the wax in the wax emulsion has a melting point in the range of 50 to 170 ℃, preferably 100 to 140 ℃.
Advantageously, the wax in the wax emulsion has a density of from 0.90 to 1.00g/cm 3 Preferably in the range of 0.95-1.00g/cm 3 Range.
Advantageously, the acid number of the wax in the wax emulsion is in the range of 0-100mg KOH/g, preferably in the range of 0-40mg KOH/g.
The polyethylene wax is not particularly limited, and may be polyethylene wax commonly used in the art.
For example, the polyethylene wax may be a polyethylene wax selected from the group consisting of homo-polyethylene wax, oxidized polyethylene wax, co-polyethylene wax, graft modified polyethylene wax, and combinations thereof, preferably selected from the group consisting of homo-polyethylene wax, oxidized polyethylene wax, and combinations thereof.
Preferably, the oxidized polyethylene wax has a density of 0.95 to 1.00g/cm 3 Is a high density oxidized polyethylene wax.
In some embodiments, the wax emulsion comprises a polyethylene wax selected from the group consisting of a homo-polyethylene wax, an oxidized polyethylene wax, a co-polyethylene wax, a graft modified polyethylene wax, and combinations thereof, preferably the wax emulsion comprises a polyethylene wax selected from the group consisting of a homo-polyethylene wax, an oxidized polyethylene wax, and combinations thereof, more preferably the wax emulsion comprises a density of 0.95-1.00g/cm 3 Is a high density oxidized polyethylene wax.
As examples of suitable high density oxidized polyethylene waxes, mention may be made of the series products from the company Honival, such as the AC307 and AC316 products, having a density of 0.98g/cm 3 The method comprises the steps of carrying out a first treatment on the surface of the AC325, AC330 and AC392, with a density of 0.99g/cm 3 The method comprises the steps of carrying out a first treatment on the surface of the AC395 product having a density of 1.00g/cm 3 。
In some embodiments, the wax emulsion comprises 15-45 wt% polyethylene wax, relative to the total weight of the wax emulsion.
The Fischer-Tropsch wax is not particularly limited, and may be one commonly used in the art.
The Fischer-Tropsch wax may be either a non-oxidized Fischer-Tropsch wax or an oxidized Fischer-Tropsch wax, preferably a non-oxidized Fischer-Tropsch wax.
In some embodiments, the wax emulsion comprises 15 to 45 wt% fischer-tropsch wax, relative to the total weight of the wax emulsion.
Preferably, the total amount of Fischer-Tropsch wax and polyethylene wax in the wax emulsion is from 20 to 35 wt% relative to the total weight of the wax emulsion.
The wax particles in the wax emulsion have a maximum particle size D99.90 of not more than 15 μm, as tested according to ISO 13320-2020.
In some embodiments, the wax particles in the wax emulsion have a center particle size in the range of 0.5 to 7 microns as tested in accordance with ISO 13320-2020. For example, in some embodiments, the wax particles in the wax emulsion have a center particle size in the range of 0.5 to 2.5 microns as tested according to ISO 13320-2020.
Advantageously, the weight average molecular weight of the high molecular weight nonionic surfactant is in the range 1100-8000 g/mol.
As examples of the high molecular weight nonionic surfactant that can be used, polyvinyl alcohols, ethylene oxide-propylene oxide block copolymers, polyethers, celluloses or sugar-based surfactants can be mentioned.
In some embodiments, the high molecular weight nonionic surfactant is selected from the group consisting of polyvinyl alcohols, ethylene oxide-propylene oxide block copolymers, polyethers, cellulosics, sugar-based surfactants, and combinations thereof.
Preferably, the wax emulsion comprises a high molecular weight nonionic surfactant selected from the group consisting of ethylene oxide-propylene oxide block copolymers, polyether surfactants, and combinations thereof.
More preferably, the wax emulsion comprises a high molecular weight nonionic surfactant selected from the group consisting of ethylene oxide-propylene oxide block copolymers, phenol polyoxyethylene ethers, fatty alcohol polyoxypropylene ethers, fatty alcohol polyoxyethylene ether and fatty alcohol polyoxypropylene ether block copolymers, and combinations thereof.
Preferably, the wax emulsion comprises a high molecular weight nonionic surfactant selected from the group consisting of ethylene oxide-propylene oxide block copolymers, phenol polyoxyethylene ethers and fatty alcohol polyoxyethylene ethers comprising 2 to 80 ethylene oxide units, wherein the fatty alcohol is a linear or isomeric saturated fatty alcohol having a carbon chain length of 10 to 60, and combinations thereof.
As a commercial example of the high molecular weight ethylene oxide-propylene oxide block copolymer, synperonic PE/F108 from HeDacron chemical Co.
Examples of the polyoxyethylene phenol ether include polyoxyethylene nonylphenol ether and polyoxyethylene octylphenol ether.
As a commercial example of the polyoxyethylene nonylphenol ether, NPE-50 from Saxole corporation may be mentioned.
As commercial examples of the high molecular weight fatty alcohol polyoxyethylene ether, there may be mentioned Slovassol2430 and AEO 80-68S from sasol, brij20 and Brij25 from Croda, inc.
Preferably, the wax emulsion comprises 3-8 wt% of a high molecular weight nonionic surfactant, relative to the total weight of the wax emulsion.
Advantageously, the low molecular weight surfactant has a weight average molecular weight in the range 200-1000 g/mol.
The low molecular weight surfactant may be an anionic, cationic or nonionic low molecular weight surfactant, or may be a combination of an anionic surfactant and a nonionic surfactant or a combination of a cationic surfactant and a nonionic surfactant.
Preferably, the low molecular weight surfactant is a low molecular weight nonionic surfactant.
As examples of the low molecular weight nonionic surfactant that can be used, fatty alcohol polyoxyethylene ethers, polyoxyethylene alkylphenols, ethylene oxide-propylene oxide block copolymers, thiol ethoxylates, alkyl polyglycosides, and the like can be mentioned.
In some embodiments, the low molecular weight surfactant is selected from the group consisting of fatty alcohol polyoxyethylene ethers, polyoxyethylene alkylphenols, ethylene oxide-propylene oxide block copolymers, thiol ethoxylates, alkyl polyglycosides, and combinations thereof.
Preferably, the wax emulsion comprises a low molecular weight surfactant selected from the group consisting of fatty alcohol polyoxyethylene ether surfactants.
Preferably, the wax emulsion comprises a low molecular weight surfactant selected from the group consisting of fatty alcohol polyoxyethylene ethers comprising 2 to 25 oxyethylene units, wherein the fatty alcohol is a linear or isomeric saturated fatty alcohol having a carbon chain length of 10 to 20.
Examples of low molecular weight fatty alcohol-polyoxyethylene ether include Slovasol 6810 and Multiso 13/130 from sasol corporation, foryl2410 from Kekai corporation, and the like.
Preferably, the wax emulsion comprises from 1 to 10 wt% of a low molecular weight surfactant, relative to the total weight of the wax emulsion.
The wax emulsion may also contain an organic or inorganic base to adjust the pH.
Advantageously, the wax emulsion has a pH in the range of 6-9 to facilitate application in ink and coating systems.
As examples of the organic base, 2-amino-2-methyl-1-propanol, dimethylethanolamine, diethylethanolamine, and the like can be mentioned.
As examples of the inorganic base, potassium hydroxide, sodium hydroxide, and the like can be mentioned.
The amount of the organic or inorganic base may be 0.01 to 1 wt% relative to the total weight of the wax emulsion.
The wax emulsion may also contain a biocide.
The bactericide is not particularly limited, and for example, isothiazolinone, kathon and other bactericides can be used.
The amount of bactericide can be determined by the person skilled in the art according to the actual requirements.
Preferably, the wax emulsion is a wax dispersion.
The wax emulsion may be prepared using conventional methods well known to those skilled in the art.
Generally, all raw materials are added into a reaction kettle in proportion, then heated to 10-15 ℃ above the melting point of wax, kept for a period of time, and then rapidly cooled to room temperature to obtain wax emulsion.
According to a second aspect of the present application, there is provided a process for preparing a micronized wax, comprising:
providing a wax emulsion according to the first aspect of the application and optionally adjusting its solids content; and
the wax emulsion is spray dried to obtain a micronized wax.
As described above, the wax emulsion may be prepared using conventional methods well known to those skilled in the art.
The particle size of the final micronized wax is controlled by adjusting the solids content of the wax emulsion, spray drying equipment parameters (such as fluid inlet temperature, outlet temperature), spray drying air flow rate, spray pressure, and nozzle size.
In the present application, the solid content means the content of a nonvolatile component.
Preferably, the wax emulsion used for spray drying has a solids content in the range of 1-40 wt.%, relative to the total weight of the wax emulsion.
The solids content may be adjusted by, for example, adding a combination of one or more of water, ethanol, butyl acetate, and the like.
Preferably, the fluid inlet temperature of the spray drying apparatus is in the range 80-150 ℃.
Preferably, the fluid outlet temperature of the spray drying apparatus is in the range 40-70 ℃.
Preferably, the spray drying air flow rate is in the range of 0.05 to 0.7. 0.7 m 3 In the range of/min.
Preferably, the spray pressure is in the range of 0.05-0.6 MPa.
Preferably, the size of the nozzle is in the range of 200-1800 μm.
According to a third aspect of the present application, there is provided a micro powder wax characterized in that it is obtained using the wax emulsion described above.
The micro powder wax of the present application has a spherical shape or a spheroid shape, preferably a spherical shape.
The micronized waxes according to the application have a maximum particle size (D99.99) of less than 20 microns, a central particle size (D50) in the range 1-7 microns and a particle size distribution in the range 2.5-5, tested according to ISO 13320-2020.
The micro powder wax has narrow particle size distribution and good dispersibility. The film formed by the ink or the paint containing the micro powder wax as the additive has the characteristics of high transparency and gloss, good hand feeling, good wear resistance, good scratch resistance and the like.
In the present application, the descriptions of the features may be combined with each other unless the combination clearly deviates from the spirit and object of the present application.
"preferably" or "preferred" as used in the present application means that the selection is better for the purposes of the present application.
The terms "comprising" and "including" as used in the present application encompass the situation in which other elements not explicitly mentioned are also included or included as well as the situation in which they consist of the elements mentioned.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this application belongs. To the extent that the definitions of terms in this specification are inconsistent with the ordinary understanding of those skilled in the art to which this application pertains, the definitions described herein control.
Unless otherwise indicated, all numbers expressing quantities of ingredients, temperatures, particle sizes, and so forth used in the specification and claims are to be understood as being modified in the term "about". Accordingly, unless indicated to the contrary, the numerical parameters set forth herein are approximations that may vary depending upon the desired properties to be obtained.
Examples
The conception and the technical effects produced by the present application will be further described with reference to examples so that those skilled in the art can fully understand the objects, features, and effects of the present application. It should be understood that the examples are illustrative only and are not intended to limit the scope of the application.
Raw materials used
The main raw materials and sources used in the examples are summarized in table 1 below.
TABLE 1
| Component (A) | Number plate | Suppliers (suppliers) |
| Polyethylene wax | AC316 | Honiswell |
| Fatty alcohol polyoxyethylene ether (55 EO) | AEO 80-68S | Sha Suo |
| Ethylene oxide-propylene oxide block copolymers | Synperonic PE/F108 | Gramineae chemical |
| Polyoxyethylene nonylphenol ether (50 EO) | NPE-50 | Sha Suo |
| Phosphoglycerides | CrodafosTM CS2A | Gramineae chemical |
| Mountain-grass trimethyl ammonium chloride | Incroquat Beheny TMC-25 | Gramineae chemical |
| Fatty alcohol polyoxyethylene ether (10 EO) | SLOVASOL 6810 | Sha Suo |
| Isomeric tridecanol polyoxyethylene ether (13 EO) | MULTISO 13/130 | Sha Suo |
| 2-amino-2-methyl-1-propanol | AMP95 | Angas |
| Isothiazolinone bactericides | Acticide MV | TollChemical chemistry |
Testing and evaluation
The following tests and evaluations were performed in the examples.
Particle size and particle size distribution: the tests were carried out according to ISO 13320-2020 using a Microtrac S3500 type test apparatus.
Gloss: tested according to ASTM D523-2014.
Haze: according to GB/T2410-2008 test.
Hand feeling: after the paint film was prepared, the hand of the paint film was touched by hand, giving a rating.
Abrasion resistance: according to ASTM D5264.
Scratch resistance: tested according to ISO 1518-2011.
Dispersibility: the difficulty of dispersing the micro powder wax in the water-based ink system is examined.
Inventive examples 1-6 (IE 1-IE 6) and comparative examples 1-4 (CE 1-CE 4)
The respective raw materials were mixed in parts by weight shown in tables 2 and 3 to obtain wax-containing compositions. Specifically, the raw materials are mixed according to the parts by weight shown in tables 2 and 3 and are filled into a reaction kettle, the reaction kettle is sealed and heated to 10-15 ℃ above the melting point of wax, the temperature is kept for 1-2 hours, then the temperature is quickly reduced to room temperature, and the materials are filtered and filled.
The wax-containing compositions obtained in inventive examples 1-6 and comparative examples 1 and 3 were emulsions, and the wax-containing compositions obtained in comparative examples 2 and 4 were gels.
The particle diameters of wax particles in the emulsions obtained in inventive examples 1 to 6 and comparative examples 1 and 3 were characterized, and the results are shown in tables 2 and 3.
TABLE 2
TABLE 3 Table 3
As can be seen from tables 2 and 3, the wax particles in the wax emulsions obtained in application examples 1 to 6 were small in particle size.
Inventive examples 7-9 (IE 7-IE 9)
The solids content of the wax emulsions obtained in inventive examples 1 and 2 was adjusted to 5% by weight by adding water. The solids content of the wax emulsion obtained in inventive example 3 was adjusted to 40% by weight by adding water. Micro powder waxes were prepared according to the spray drying conditions listed in Table 3 to obtain micro powder waxes P-1, P-2 and P-3, respectively.
FIG. 1 is a micrograph of the fine powder wax P-2 produced in inventive example 8.
The particle size and distribution of the obtained micro wax were characterized, and the results are summarized in table 4. FIG. 2 is a particle size distribution of the fine wax powder P-2 prepared in inventive example 8.
TABLE 4 Table 4
As can be seen from Table 4, the micro powder wax prepared using the wax emulsion of the present application has a small particle size and a narrow distribution.
The resulting micro powder waxes P-1 and P-2 were added to the aqueous ink and the micro powder wax application performance was evaluated according to the evaluation criteria used in the industry, while comparing with the commercial product aculist C3 from the company holmivir, and the results are summarized in table 5.
TABLE 5
| Product(s) | Haze (%) | Gloss (60 degree) | Hand feel | Scratch resistance | Wear resistance | Dispersibility of |
| P-1 | 16 | 62 | +++ | ++ | ++ | ++ |
| P-2 | 8 | 73 | +++ | ++ | ++ | ++ |
| ACumist C3 | 27 | 52 | + | ++ | +++ | + |
In terms of hand, + stands for: the smoothness of a paint film is common by touching the paint film by hands; ++ stands for: the smoothness of the paint film is good when the paint film is touched by hands; ++ + representing: the smoothness of the paint film is better when the paint film is touched by hands.
In terms of scratch resistance, according to the ISO1518-2011 standard test, + stands for: scratch resistance results <1100g; ++ stands for: the scratch resistance result is 1100-1300 g; ++ + representing: scratch resistance result >1300g.
Regarding abrasion resistance, + stands for: the damage on the surface of the paint film is slightly more; ++ stands for: surface damage of a paint film is moderate; ++ + representing: the damage to the paint film surface is slight.
In terms of dispersibility, + represents: the micro powder wax is dispersed in the system by a high-speed dispersing machine; ++ stands for: the micro powder wax can be dispersed in the system by using a common stirring paddle.
While certain aspects of the present application have been shown and discussed, it will be appreciated by those skilled in the art that changes may be made in these aspects without departing from the principles and spirit of the application, the scope of which is defined in the claims and their equivalents.
Claims (16)
1. A wax emulsion for use in preparing a micronized wax, comprising, based on the total weight of the wax emulsion:
15 to 45 wt% of a polyethylene wax or a fischer-tropsch wax;
0.1 to 10 wt% of a high molecular weight nonionic surfactant;
1 to 10 wt% of a low molecular weight surfactant; and
30-80% by weight of water.
2. Wax emulsion according to claim 1, characterized in that the wax in the wax emulsion has a molecular weight in the range of 800 to 20,000 g/mol and a melting point in the range of 50 to 170 ℃, preferably the central particle size of the wax particles in the wax emulsion is in the range of 0.5-7 micrometers.
3. Wax emulsion according to claim 1 or 2, characterized in that the wax emulsion comprises a polyethylene wax, preferably a homo-polyethylene wax, an oxidized polyethylene wax, a co-polyethylene wax, a graft modified polyethylene wax and combinations thereofThe wax emulsion comprises a polyethylene wax selected from the group consisting of a homo-polyethylene wax, an oxidized polyethylene wax, and combinations thereof, more preferably the wax emulsion comprises a density of 0.95 to 1.00g/cm 3 Is a high density oxidized polyethylene wax.
4. A wax emulsion according to any of claims 1-3, characterized in that the high molecular weight surfactant has a weight average molecular weight in the range 1100-8000 g/mol.
5. The wax emulsion of any of claims 1-4, wherein the high molecular weight surfactant is selected from the group consisting of polyvinyl alcohols, ethylene oxide-propylene oxide block copolymers, polyethers, cellulose based sugar based surfactants and combinations thereof, preferably the wax emulsion comprises a high molecular weight nonionic surfactant selected from the group consisting of ethylene oxide-propylene oxide block copolymers, phenol polyoxyethylene ethers, fatty alcohol polyoxypropylene ethers, fatty alcohol polyoxyethylene ether and fatty alcohol polyoxypropylene ether block copolymers and combinations thereof, more preferably the wax emulsion comprises a high molecular weight nonionic surfactant selected from the group consisting of ethylene oxide-propylene oxide block copolymers, phenol polyoxyethylene ethers and fatty alcohol polyoxyethylene ethers and combinations thereof, the fatty alcohol polyoxyethylene ethers comprising 2-80 oxyethylene units wherein the fatty alcohol is a linear or isomeric saturated fatty alcohol having a carbon chain length of 10-60.
6. Wax emulsion according to any of claims 1 to 5, characterized in that the low molecular weight surfactant has a weight average molecular weight in the range of 200-1000 g/mol.
7. Wax emulsion according to any of claims 1-6, characterized in that the low molecular weight surfactant is a nonionic low molecular weight surfactant, preferably the low molecular weight surfactant is selected from the group consisting of fatty alcohol polyoxyethylene ethers, polyoxyethylene alkylphenols, ethylene oxide-propylene oxide block copolymers, thiol ethoxylates, alkyl polyglycosides and combinations thereof, more preferably the wax emulsion comprises a low molecular weight surfactant selected from the group consisting of fatty alcohol polyoxyethylene ethers comprising 2-25 oxyethylene units, wherein the fatty alcohol is a linear or isomeric saturated fatty alcohol having a carbon chain length of 10-20.
8. A method for preparing a micronized wax, comprising:
providing the wax emulsion according to any of claims 1 to 7 and optionally adjusting its solids content; and
the wax emulsion is spray dried to obtain a micronized wax.
9. The method according to claim 8, characterized in that the solids content of the wax emulsion for spray drying is in the range of 1-40 wt.%, relative to the total weight of the wax emulsion.
10. A method according to claim 8 or 9, characterized in that the fluid inlet temperature of the spray drying apparatus is in the range of 80-150 ℃.
11. The method according to any one of claims 8-10, characterized in that the fluid outlet temperature of the spray drying apparatus is in the range of 40-70 ℃.
12. The method according to any one of claims 8-11, wherein the spray drying gas flow rate is in the range of 0.05-0.7 m 3 In the range of/min.
13. The method according to any one of claims 8-12, wherein the spray pressure is in the range of 0.05-0.6 MPa.
14. The method according to any one of claims 8-13, wherein the size of the nozzle is in the range of 200-1800 μm.
15. A micronized wax, characterized in that it is obtained with a wax emulsion according to any one of claims 1 to 7.
16. The micronized wax according to claim 15, wherein the micronized wax has a maximum particle size (D99.99) of less than 20 microns, a central particle size (D50) in the range of 1-7 microns and a particle size distribution in the range of 2.5-5, as measured according to ISO 13320-2020.
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| CN202210598312.1A CN117186437A (en) | 2022-05-30 | 2022-05-30 | Wax emulsion and method for preparing micro-powder wax |
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