CN115073869A - Preparation method of acrylic solid pigment and acrylic solid pigment - Google Patents
Preparation method of acrylic solid pigment and acrylic solid pigment Download PDFInfo
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- CN115073869A CN115073869A CN202110923053.0A CN202110923053A CN115073869A CN 115073869 A CN115073869 A CN 115073869A CN 202110923053 A CN202110923053 A CN 202110923053A CN 115073869 A CN115073869 A CN 115073869A
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- 239000000049 pigment Substances 0.000 title claims abstract description 64
- 239000007787 solid Substances 0.000 title claims abstract description 58
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
- 239000004094 surface-active agent Substances 0.000 claims abstract description 32
- 229920002678 cellulose Polymers 0.000 claims abstract description 25
- 239000001913 cellulose Substances 0.000 claims abstract description 25
- 239000004925 Acrylic resin Substances 0.000 claims abstract description 23
- 229920000178 Acrylic resin Polymers 0.000 claims abstract description 23
- 239000004014 plasticizer Substances 0.000 claims abstract description 21
- 239000006184 cosolvent Substances 0.000 claims abstract description 19
- 239000002270 dispersing agent Substances 0.000 claims abstract description 17
- 238000000034 method Methods 0.000 claims abstract description 17
- 229920003229 poly(methyl methacrylate) Polymers 0.000 claims abstract description 17
- 239000004926 polymethyl methacrylate Substances 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims abstract description 13
- 238000004898 kneading Methods 0.000 claims abstract description 13
- 238000003801 milling Methods 0.000 claims abstract description 9
- 239000012748 slip agent Substances 0.000 claims abstract description 5
- 239000000463 material Substances 0.000 claims description 54
- 238000001816 cooling Methods 0.000 claims description 27
- XFRVVPUIAFSTFO-UHFFFAOYSA-N 1-Tridecanol Chemical compound CCCCCCCCCCCCCO XFRVVPUIAFSTFO-UHFFFAOYSA-N 0.000 claims description 20
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 20
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 20
- 239000002245 particle Substances 0.000 claims description 15
- 239000003945 anionic surfactant Substances 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 12
- HQKMJHAJHXVSDF-UHFFFAOYSA-L magnesium stearate Chemical compound [Mg+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O HQKMJHAJHXVSDF-UHFFFAOYSA-L 0.000 claims description 12
- 229920005552 sodium lignosulfonate Polymers 0.000 claims description 12
- 229920002301 cellulose acetate Polymers 0.000 claims description 10
- 239000003795 chemical substances by application Substances 0.000 claims description 10
- 239000006185 dispersion Substances 0.000 claims description 9
- 238000007599 discharging Methods 0.000 claims description 6
- 235000019359 magnesium stearate Nutrition 0.000 claims description 6
- 238000007873 sieving Methods 0.000 claims description 6
- CEGOLXSVJUTHNZ-UHFFFAOYSA-K aluminium tristearate Chemical compound [Al+3].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CEGOLXSVJUTHNZ-UHFFFAOYSA-K 0.000 claims description 3
- 229940063655 aluminum stearate Drugs 0.000 claims description 3
- AGXUVMPSUKZYDT-UHFFFAOYSA-L barium(2+);octadecanoate Chemical compound [Ba+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O AGXUVMPSUKZYDT-UHFFFAOYSA-L 0.000 claims description 3
- CJZGTCYPCWQAJB-UHFFFAOYSA-L calcium stearate Chemical compound [Ca+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O CJZGTCYPCWQAJB-UHFFFAOYSA-L 0.000 claims description 3
- 235000013539 calcium stearate Nutrition 0.000 claims description 3
- 239000008116 calcium stearate Substances 0.000 claims description 3
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 claims description 3
- 238000004040 coloring Methods 0.000 abstract description 9
- 238000004043 dyeing Methods 0.000 abstract description 8
- 239000002202 Polyethylene glycol Substances 0.000 description 20
- 229920001223 polyethylene glycol Polymers 0.000 description 20
- GVGUFUZHNYFZLC-UHFFFAOYSA-N dodecyl benzenesulfonate;sodium Chemical compound [Na].CCCCCCCCCCCCOS(=O)(=O)C1=CC=CC=C1 GVGUFUZHNYFZLC-UHFFFAOYSA-N 0.000 description 18
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 10
- 229920003023 plastic Polymers 0.000 description 7
- 239000004033 plastic Substances 0.000 description 7
- 239000000126 substance Substances 0.000 description 7
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical group [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 6
- 229920002565 Polyethylene Glycol 400 Polymers 0.000 description 4
- 239000000428 dust Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- -1 acryl Chemical group 0.000 description 3
- 239000011521 glass Substances 0.000 description 3
- 229910052500 inorganic mineral Inorganic materials 0.000 description 3
- 239000011707 mineral Substances 0.000 description 3
- 238000011160 research Methods 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000000843 powder Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- BIHQJMSIEXRWPS-UHFFFAOYSA-N 2-[bis(2-hydroxyethyl)amino]ethanol;dodecyl dihydrogen phosphate Chemical compound OCCN(CCO)CCO.CCCCCCCCCCCCOP(O)(O)=O BIHQJMSIEXRWPS-UHFFFAOYSA-N 0.000 description 1
- LIFHMKCDDVTICL-UHFFFAOYSA-N 6-(chloromethyl)phenanthridine Chemical compound C1=CC=C2C(CCl)=NC3=CC=CC=C3C2=C1 LIFHMKCDDVTICL-UHFFFAOYSA-N 0.000 description 1
- 230000002378 acidificating effect Effects 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- BTBJBAZGXNKLQC-UHFFFAOYSA-N ammonium lauryl sulfate Chemical compound [NH4+].CCCCCCCCCCCCOS([O-])(=O)=O BTBJBAZGXNKLQC-UHFFFAOYSA-N 0.000 description 1
- 229940063953 ammonium lauryl sulfate Drugs 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- TVACALAUIQMRDF-UHFFFAOYSA-N dodecyl dihydrogen phosphate Chemical compound CCCCCCCCCCCCOP(O)(O)=O TVACALAUIQMRDF-UHFFFAOYSA-N 0.000 description 1
- JTNSGMCDSLXGTF-UHFFFAOYSA-N dodecyl methyl hydrogen phosphate Chemical compound CCCCCCCCCCCCOP(O)(=O)OC JTNSGMCDSLXGTF-UHFFFAOYSA-N 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000006081 fluorescent whitening agent Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 239000001023 inorganic pigment Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000012860 organic pigment Substances 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 230000006641 stabilisation Effects 0.000 description 1
- 238000011105 stabilization Methods 0.000 description 1
- 239000007858 starting material Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L33/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
- C08L33/04—Homopolymers or copolymers of esters
- C08L33/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, which oxygen atoms are present only as part of the carboxyl radical
- C08L33/10—Homopolymers or copolymers of methacrylic acid esters
- C08L33/12—Homopolymers or copolymers of methyl methacrylate
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2265—Oxides; Hydroxides of metals of iron
- C08K2003/2272—Ferric oxide (Fe2O3)
Landscapes
- Chemical & Material Sciences (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Developing Agents For Electrophotography (AREA)
Abstract
The invention relates to the technical field of dyeing pigments, in particular to a preparation method of an acrylic solid pigment and the acrylic solid pigment. The solid acrylic pigment is prepared by kneading a toner, cellulose, a dispersing agent, water, a cosolvent, a plasticizer, a surfactant and acrylic resin, then milling, and finally granulating with polymethyl methacrylate, methyl methacrylate and a slip agent. The acrylic solid pigment prepared by the method can disperse high coloring strength in a short time.
Description
Technical Field
The invention relates to the technical field of dyeing pigments, in particular to a preparation method of an acrylic solid pigment and the acrylic solid pigment.
Background
The current acrylic dyeing material on the market mainly comprises powdered dyeing powder and paste-like color paste, but the powdered dyeing powder has the problem of dust flying in the dyeing process, while the paste-like color paste has the problem of waste pollution in the using process, in order to respond to the requirement of the real country for environmental protection and the current situation of the current acrylic material, the applicant previously developed a solid pigment particle and applied for a related patent (the patent number is CN111454530A), and the solid pigment particle avoids the material waste caused by dust flying, and can also avoid the generation of dangerous waste to the greatest extent.
However, in the using process, the dyeing time of the solid pigment particles is relatively long, and long time is needed to achieve good dyeing capability, and on the basis of previous researches, the applicant has carried out the preparation of the acrylic solid pigment in the invention.
Disclosure of Invention
In order to solve the above technical problems, a first aspect of the present invention provides a method for preparing an acryl solid pigment, comprising the steps of:
(1) kneading: heating the kneader to 100-130 ℃, sequentially adding the toner, the cellulose, the dispersant, the water, the cosolvent, the plasticizer, the surfactant and the acrylic resin, kneading for 60-80min, cooling to 40-50 ℃, and discharging to obtain a material a;
(2) cooling the material a to room temperature to obtain a material b;
(3) adding the material b into a two-roller open mill with the roller temperature of 140 ℃ and the temperature of 150 ℃, wherein the roller rotating speed is 30-40r/min, and the open milling time is 60-80 min; cooling the roller to 50-60 ℃, controlling the rotating speed of the roller to 12-18r/min, open-milling until the particle size of the pre-dispersion is less than 200nm, stopping the mill and cooling to room temperature to obtain a material c;
(4) adding the material c, the polymethyl methacrylate, the methyl methacrylate and the slipping agent into a double-screw granulator, heating to 190-;
(5) and (4) sieving the material d by a sieve of 10-500 meshes to obtain the acrylic solid pigment.
As a preferred technical solution of the present invention, the cellulose is cellulose acetate; the dispersant is sodium lignosulfonate.
In a preferred embodiment of the present invention, the surfactant comprises an anionic surfactant.
In a preferred embodiment of the present invention, the anionic surfactant has a structure of C10-C15.
As a preferable technical scheme of the invention, the surfactant also comprises isomeric tridecanol polyoxyethylene ether.
As a preferable technical scheme of the invention, the weight ratio of the acrylic resin to the toner is (1-1.5): (9-11); the weight ratio of the plasticizer to the acrylic resin is (0.5-0.56): (1-1.5); the weight ratio of the water to the cellulose is (5-5.6): (15-17).
As a preferable technical scheme of the invention, the cosolvent is C1-C6 alcohol.
In a preferred embodiment of the present invention, the slip agent is at least one selected from zinc stearate, calcium stearate, magnesium stearate, aluminum stearate, and barium stearate.
As a preferable technical scheme of the invention, the weight ratio of the material c, the polymethyl methacrylate, the methyl methacrylate and the slipping agent is (45-55): (70-75): (9-11): (1.8-2.3); preferably, the ratio of 51: 72: 10: 2.
the second aspect of the invention provides an acrylic solid pigment prepared according to the preparation method of the acrylic solid pigment.
Advantageous effects
1. The prepared acrylic solid pigment does not generate dust in the using process, so that the production operation can be accurately carried out, and meanwhile, the harm of the dust to operators can be avoided;
2. the acrylic solid pigment prepared by the method has good coloring capacity and dispersion effect, has better fluidity compared with the conventional acrylic solid pigment, is easy to package and transport, and reduces the packaging and transportation cost;
3. the use of the specific surfactant in the invention can shorten the coloring time compared with the prior acrylic solid pigment, reduce the using amount of the pigment, shorten the dispersion time and reduce the raw material cost and the time cost.
4. Compared with the prior preparation process of the acrylic solid pigment, the preparation process of the acrylic solid pigment using the C1-C6 alcohol as the cosolvent is more green and environment-friendly.
Detailed Description
In order to solve the above technical problems, a first aspect of the present invention provides a method for preparing an acryl solid pigment, comprising the steps of:
(1) kneading: heating the kneader to 100-130 ℃, sequentially adding the toner, the cellulose, the dispersant, the water, the cosolvent, the plasticizer, the surfactant and the acrylic resin, kneading for 60-80min, cooling to 40-50 ℃, and discharging to obtain a material a;
(2) cooling the material a to room temperature to obtain a material b;
(3) adding the material b into a two-roller open mill with the roller temperature of 140 ℃ and the temperature of 150 ℃, wherein the roller rotating speed is 30-40r/min, and the open milling time is 60-80 min; cooling the roller to 50-60 ℃, controlling the rotating speed of the roller to 12-18r/min, open-milling until the particle size of the pre-dispersion is less than 200nm, stopping the mill and cooling to room temperature to obtain a material c;
(4) adding the material c, the polymethyl methacrylate, the methyl methacrylate and the slipping agent into a double-screw granulator, heating to 190-;
(5) and (4) sieving the material d by a sieve of 10-500 meshes to obtain the acrylic solid pigment.
The toner may be selected according to the color required by the acrylic solid pigment, and is not particularly limited, and may be an organic pigment, an inorganic pigment, a fluorescent pigment, a pearlescent pigment, a fluorescent whitening agent, and the like.
In one embodiment, the toner has an average particle size of 300-500 mesh; preferably 400 mesh.
In the course of experiments, the applicant found that the coloring power of an acryl solid pigment increases as the average particle diameter of the toner decreases within a certain range, but when the average particle diameter of the toner is too low, the coloring power is rather poor. It is possible that within a certain range, the smaller the average particle diameter of the toner is, the more the number of particles of the same weight of toner in the system is, but when the particle diameter is too small, the dispersion property of the system is not good.
In one embodiment, the cellulose is cellulose acetate.
In one embodiment, the cellulose acetate is available from Bofeng chemical Co., Ltd, Dongguan.
In one embodiment, the dispersant is sodium lignosulfonate.
In one embodiment, the sodium lignosulfonate is purchased from longquan chemical company, inc.
In one embodiment, the surfactant comprises an anionic surfactant.
In one embodiment, the anionic surfactant has a structure comprising C10-C15. For example, ammonium lauryl sulfate, sodium dodecylbenzenesulfonate, triethanolamine lauryl sulfate, lauryl phosphate, methyl lauryl phosphate, and triethanolamine lauryl phosphate.
In a preferred embodiment, the surfactant further comprises the isomeric tridecanol polyoxyethylene ether.
In a preferred embodiment, the isomeric tridecanol polyoxyethylene ether has an HLB value of 13, specifically, the isomeric tridecanol polyoxyethylene ether is TO-9.
In a preferred embodiment, the anionic surfactant is sodium dodecylbenzenesulfonate.
In one embodiment, the weight ratio of isomeric tridecanol polyoxyethylene ether to sodium dodecylbenzene sulfonate is 1: (2-3); preferably 1: 2.5.
in a preferred embodiment, the surfactant further comprises 10-20% by mass of polyethylene glycol.
In a more preferred embodiment, the surfactant further comprises 15% by weight of polyethylene glycol.
In a preferred embodiment, the polyethylene glycol has an average molecular weight of 200-; preferably 400; specifically, the polyethylene glycol is PEG-400.
In one embodiment, the weight ratio of the toner, the cellulose, the dispersant and the surfactant is (9-11): (15-17): (0.5-0.55): (0.5-0.55); preferably 10.6: 16: 0.53: 0.53.
the applicant previously prepared an acrylic solid pigment, but during use, it was found that the pigment coloring effect was general, mainly in that a longer time was required to achieve better tinting strength. On the basis of the research, the applicant prepares the acrylic solid pigment, and the acrylic solid pigment can disperse higher coloring strength in a shorter time. The reason is probably that the sodium dodecylbenzene sulfonate belongs to an anionic surfactant, has electronegative groups and can be adsorbed on the toner to a certain extent, but the toner can be positively charged under an acidic condition, and the dispersing performance of a system is influenced because the sodium dodecylbenzene sulfonate is easy to generate bubbles in the system during use, so when the sodium dodecylbenzene sulfonate is used alone as the surfactant, the coloring performance of the acrylic solid pigment is general.
Through a large amount of research and development experiments of an applicant, the TO-9, the polyethylene glycol and the sodium dodecyl benzene sulfonate are used, so that the defect that bubbles appear in a system due TO the sodium dodecyl benzene sulfonate can be overcome, the acrylic solid pigment has excellent coloring capacity, on one hand, the TO-9 and the polyethylene glycol can have an adsorption effect with fibers under the action of a hydrogen bond, then the cellulose can fix toner, on the other hand, the TO-9 and the polyethylene glycol can be inserted into the molecules of the sodium dodecyl benzene sulfonate TO form a compound with high strength, and the system is more stable.
However, in the research, it is found that the addition amounts of the TO-9 and the polyethylene glycol need TO be strictly controlled, probably because the TO-9, the polyethylene glycol and the sodium lignosulfonate have a certain adsorption competition relationship, and the adsorption and the stabilization between the TO-9 and the polyethylene glycol, the sodium lignosulfonate and the sodium dodecylbenzenesulfonate and the cellulose and the toner can reach an optimal balance point only by controlling the TO-9 and the polyethylene glycol.
The acrylic resin in the present invention is not limited in its source, and in one embodiment, is available from Hessie chemical Limited, North lake.
In one embodiment, the weight ratio of the acrylic resin to the toner is (1-1.5): (9-11); preferably 1.3: 10.
in order to increase the mechanical properties of the acrylic solid pigment and the plasticity of the product, in one embodiment, the plasticizer is GX-68 environment-friendly plasticizer which is available from Toho plastic additive Co.
In one embodiment, the weight ratio of the plasticizer to the acrylic resin is (0.5-0.56): (1-1.5); preferably 0.53: 1.3.
in one embodiment, the weight ratio of water to cellulose is (5-5.6): (15-17); preferably, the ratio of 5.3: 16.
in one embodiment, the co-solvent is a C1-C6 alcohol (e.g., methanol, ethanol, propanol, butanol, etc.).
In a preferred embodiment, the co-solvent is ethanol.
In one embodiment, the weight ratio of co-solvent to water is 1: 1.
in one embodiment, the polymethylmethacrylate is available from Shangguan's winning source plastics, Inc.
In one embodiment, the glidant is selected from at least one of zinc stearate, calcium stearate, magnesium stearate, aluminum stearate, barium stearate.
In one embodiment, the weight ratio of the material c, the polymethyl methacrylate, the methyl methacrylate and the slip agent is (45-55): (70-75): (9-11): (1.8-2.3); preferably, the ratio of 51: 72: 10: 2.
the present invention will be specifically described below by way of examples. It should be noted that the following examples are only for illustrating the present invention and should not be construed as limiting the scope of the present invention, and that the insubstantial modifications and adaptations of the present invention by those skilled in the art based on the above disclosure are still within the scope of the present invention.
In addition, the starting materials used are all commercially available, unless otherwise specified.
Examples
Example 1
A preparation method of an acrylic solid pigment comprises the following steps: (1) kneading: heating a kneader to 100 ℃, sequentially adding toner, cellulose, a dispersing agent, water, a cosolvent, a plasticizer, a surfactant and acrylic resin, kneading for 60min, cooling to 40 ℃, and discharging to obtain a material a; (2) cooling the material a to room temperature to obtain a material b; (3) adding the material b into a two-roll open mill with the roll temperature of 140 ℃, wherein the roller rotating speed is 30r/min, and the open milling time is 60 min; cooling the roller to 50 ℃, controlling the rotating speed of the roller to be 12r/min, opening until the particle size of the pre-dispersion is less than 200nm, stopping the machine, and cooling to room temperature to obtain a material c; (4) adding the material c, the polymethyl methacrylate, the methyl methacrylate and the slipping agent into a double-screw granulator, heating to 190 ℃, stirring for 60min at the rotating speed of 270r/min, and cooling and granulating to obtain a material d; (5) sieving the material d by a sieve with 10 meshes to obtain an acrylic solid pigment;
the toner is iron oxide red with the fineness of 400 meshes and is purchased from Hengtai mineral products, Inc., Lingshu county;
the cellulose is cellulose acetate; the cellulose acetate is purchased from Bofeng chemical Co., Ltd, Dongguan city;
the dispersant is sodium lignosulfonate; the sodium lignosulfonate was purchased from Longquan chemical Co., Ltd.
The surfactant comprises an anionic surfactant; the anionic surfactant is sodium dodecyl benzene sulfonate; the surfactant also comprises isomeric tridecanol polyoxyethylene ether. The HLB value of the isomeric tridecanol polyoxyethylene ether is 13, and the isomeric tridecanol polyoxyethylene ether is TO-9; the weight ratio of the isomeric tridecanol polyoxyethylene ether to the sodium dodecyl benzene sulfonate is 1: 2; the surfactant also comprises 10% of polyethylene glycol by mass; the polyethylene glycol is PEG-400; the weight ratio of the toner, the cellulose, the dispersing agent and the surfactant is 9: 15: 0.5: 0.5;
the acrylic resin is purchased from chemical Limited of Hengjing lake; the weight ratio of the acrylic resin to the toner is 1: 9;
the plasticizer is GX-68 environment-friendly plasticizer which is purchased from Toxico Ribo Plastic auxiliaries Co., Ltd; the weight ratio of the plasticizer to the acrylic resin is 0.5: 1;
the weight ratio of the water to the cellulose is 5: 15;
the cosolvent is ethanol; the weight ratio of the cosolvent to the water is 1: 1;
the polymethyl methacrylate was obtained from Sheng Yuan plastics, Inc. of Dongguan;
the glidant is magnesium stearate;
the weight ratio of the material c to the polymethyl methacrylate to the methyl methacrylate to the slipping agent is 45: 70: 9: 1.8.
example 2
A preparation method of an acrylic solid pigment comprises the following steps: (1) kneading: heating a kneader to 130 ℃, sequentially adding toner, cellulose, a dispersing agent, water, a cosolvent, a plasticizer, a surfactant and acrylic resin, kneading for 80min, cooling to 50 ℃, and discharging to obtain a material a; (2) cooling the material a to room temperature to obtain a material b; (3) adding the material b into a two-roll open mill with the roll temperature of 150 ℃, wherein the roller rotating speed is 40r/min, and the open mill lasts 80 min; cooling the roller to 60 ℃, controlling the rotating speed of the roller to be 18r/min, opening until the particle size of the pre-dispersion is less than 200nm, stopping the machine, and cooling to room temperature to obtain a material c; (4) adding the material c, the polymethyl methacrylate, the methyl methacrylate and the slipping agent into a double-screw granulator, heating to 200 ℃, stirring for 80min at the rotating speed of 290r/min, and cooling and granulating to obtain a material d; (5) and (4) sieving the material d with a 500-mesh sieve to obtain the acrylic solid pigment.
The toner is iron oxide red with the fineness of 400 meshes and is purchased from Hengtai mineral products, Inc., Lingshu county;
the cellulose is cellulose acetate; the cellulose acetate is purchased from Bofeng chemical Co., Ltd, Dongguan city;
the dispersant is sodium lignosulfonate; the sodium lignosulfonate is purchased from Longquan chemical company, Anyang;
the surfactant comprises an anionic surfactant; the anionic surfactant is sodium dodecyl benzene sulfonate; the surfactant also comprises isomeric tridecanol polyoxyethylene ether; the HLB value of the isomeric tridecanol polyoxyethylene ether is 13, and the isomeric tridecanol polyoxyethylene ether is TO-9; the weight ratio of the isomeric tridecanol polyoxyethylene ether to the sodium dodecyl benzene sulfonate is 1: 3; the surfactant also comprises 20% of polyethylene glycol by mass; the polyethylene glycol is PEG-400; the weight ratio of the toner, the cellulose, the dispersing agent and the surfactant is 11: 17: 0.55: 0.55;
the acrylic resin is purchased from chemical Limited of Hengjing lake; the weight ratio of the acrylic resin to the toner is 1.5: 11;
the plasticizer is GX-68 environment-friendly plasticizer which is purchased from Toxico Ribo Plastic auxiliaries Co., Ltd; the weight ratio of the plasticizer to the acrylic resin is 0.56: 1.5;
the weight ratio of the water to the cellulose is 5.6: 17;
the cosolvent is ethanol; the weight ratio of the cosolvent to the water is 1: 1;
the polymethyl methacrylate was obtained from Sheng Yuan plastics, Inc. of Dongguan;
the glidant is magnesium stearate; the weight ratio of the material c to the polymethyl methacrylate to the methyl methacrylate to the slipping agent is 55: 75: 11: 2.3.
example 3
A preparation method of an acrylic solid pigment comprises the following steps: (1) kneading: heating a kneader to 110 ℃, sequentially adding toner, cellulose, a dispersing agent, water, a cosolvent, a plasticizer, a surfactant and acrylic resin, kneading for 70min, cooling to 45 ℃, and discharging to obtain a material a; (2) cooling the material a to room temperature to obtain a material b; (3) adding the material b into a two-roll open mill with the roll temperature of 145 ℃, wherein the roller rotating speed is 35r/min, and the open mill lasts for 70 min; cooling the roller to 55 ℃, controlling the rotating speed of the roller to be 15r/min, open-milling until the particle size of the pre-dispersion is less than 200nm, stopping the mill and cooling to room temperature to obtain a material c; (4) adding the material c, the polymethyl methacrylate, the methyl methacrylate and the slipping agent into a double-screw granulator, heating to 195 ℃, stirring for 70min at the rotating speed of 280r/min, and cooling and granulating to obtain a material d; (5) and (4) sieving the material d with a 200-mesh sieve to obtain the acrylic solid pigment.
The toner is iron oxide red with the fineness of 400 meshes and is purchased from Hengtai mineral products, Inc., Lingshu county;
the cellulose is cellulose acetate; the cellulose acetate is purchased from Bofeng chemical Co., Ltd, Dongguan city;
the dispersant is sodium lignosulfonate; the sodium lignosulfonate is purchased from Longquan chemical company, Anyang;
the surfactant comprises an anionic surfactant; the anionic surfactant is sodium dodecyl benzene sulfonate; the surfactant also comprises isomeric tridecanol polyoxyethylene ether; the HLB value of the isomeric tridecanol polyoxyethylene ether is 13, and the isomeric tridecanol polyoxyethylene ether is TO-9; the weight ratio of the isomeric tridecanol polyoxyethylene ether to the sodium dodecyl benzene sulfonate is 1: 2.5; the surfactant also comprises 15% of polyethylene glycol by mass; the polyethylene glycol is PEG-400; the weight ratio of the toner, the cellulose, the dispersing agent and the surfactant is 10.6: 16: 0.53: 0.53;
the acrylic resin is purchased from chemical Limited of Hengjing lake; the weight ratio of the acrylic resin to the toner is 1.3: 10;
the plasticizer is GX-68 environment-friendly plasticizer which is purchased from Toxico Ribo Plastic auxiliaries Co., Ltd; the weight ratio of the plasticizer to the acrylic resin is 0.53: 1.3;
the weight ratio of the water to the cellulose is 5.3: 16;
the cosolvent is ethanol; the weight ratio of the cosolvent to the water is 1: 1;
the polymethyl methacrylate was obtained from Sheng Yuan plastics, Inc. of Dongguan;
the glidant is magnesium stearate;
the weight ratio of the material c to the polymethyl methacrylate to the methyl methacrylate to the slipping agent is 51: 72: 10: 2.
example 4
The specific implementation mode of the preparation method of the acrylic solid pigment is the same as that in example 3, except that polyethylene glycol is not used.
Example 5
The preparation method of the acrylic solid pigment is the same as that of example 3, except that TO-9 is not included.
Example 6
The specific implementation mode of the preparation method of the acrylic solid pigment is the same as that in example 3, but the difference is that the surfactant further comprises 40 mass percent of polyethylene glycol.
Example 7
The specific implementation mode of the preparation method of the acrylic solid pigment is the same as that in example 3, except that the surfactant further comprises 5 mass percent of polyethylene glycol.
Example 8
The specific implementation mode of the preparation method of the acrylic solid pigment is the same as that in example 3, but the difference is that the weight ratio of isomeric tridecanol polyoxyethylene ether to sodium dodecyl benzene sulfonate is 1: 1.
example 9
The specific implementation mode of the preparation method of the acrylic solid pigment is the same as that in example 3, but the difference is that the weight ratio of isomeric tridecanol polyoxyethylene ether to sodium dodecyl benzene sulfonate is 1: 4.
performance testing
5g of standard white paint and 0.1g of the acrylic solid pigment prepared in examples 1 to 9 were weighed out and placed in a glass bottle, and then the glass bottle was put therein, and the glass bottle was shaken in a shaker for a set time of 30 seconds to prepare color cards, and the color difference values and the tinting strength values thereof were read in a Datacoor colorimeter.
The test results are shown in Table 1
TABLE 1
The foregoing examples are merely illustrative and serve to explain some of the features of the method of the present invention. The appended claims are intended to claim as broad a scope as is contemplated, and the examples presented herein are merely illustrative of selected implementations in accordance with all possible combinations of examples. Accordingly, it is applicants' intention that the appended claims are not to be limited by the choice of examples illustrating features of the invention. Also, where numerical ranges are used in the claims, subranges therein are included, and variations in these ranges are also to be construed as possible being covered by the appended claims.
Claims (10)
1. The preparation method of the acrylic solid pigment is characterized by comprising the following steps:
(1) kneading: heating the kneader to 100-130 ℃, sequentially adding the toner, the cellulose, the dispersant, the water, the cosolvent, the plasticizer, the surfactant and the acrylic resin, kneading for 60-80min, cooling to 40-50 ℃, and discharging to obtain a material a;
(2) cooling the material a to room temperature to obtain a material b;
(3) adding the material b into a two-roller open mill with the roller temperature of 140 ℃ and the temperature of 150 ℃, wherein the roller rotating speed is 30-40r/min, and the open milling time is 60-80 min; cooling the roller to 50-60 ℃, controlling the rotating speed of the roller to 12-18r/min, open-milling until the particle size of the pre-dispersion is less than 200nm, stopping the mill and cooling to room temperature to obtain a material c;
(4) adding the material c, the polymethyl methacrylate, the methyl methacrylate and the slipping agent into a double-screw granulator, heating to 190-;
(5) and (4) sieving the material d by a sieve of 10-500 meshes to obtain the acrylic solid pigment.
2. The method for preparing an acrylic solid pigment according to claim 1, wherein the cellulose is cellulose acetate; the dispersant is sodium lignosulfonate.
3. The method for preparing an acrylic solid pigment according to claim 1, wherein the surfactant comprises an anionic surfactant.
4. The method for preparing an acrylic solid pigment according to claim 3, wherein the structure of the anionic surfactant comprises C10-C15 structure. .
5. The method for preparing an acrylic solid pigment according to claim 1 or 3, wherein the surfactant further comprises isomeric tridecanol polyoxyethylene ether.
6. The method for preparing acrylic solid pigment according to claim 1, wherein the weight ratio of the acrylic resin to the toner is (1-1.5): (9-11); the weight ratio of the plasticizer to the acrylic resin is (0.5-0.56): (1-1.5); the weight ratio of the water to the cellulose is (5-5.6): (15-17).
7. The method for preparing acrylic solid pigment according to claim 5, wherein the cosolvent is C1-C6 alcohol.
8. The method for preparing acrylic solid pigment according to claim 1, wherein the slip agent is at least one selected from zinc stearate, calcium stearate, magnesium stearate, aluminum stearate and barium stearate.
9. The method for preparing acrylic solid pigment according to claim 1, wherein the weight ratio of the material c, the polymethyl methacrylate, the methyl methacrylate and the slip agent is (45-55): (70-75): (9-11): (1.8-2.3); preferably, the ratio of 51: 72: 10: 2.
10. an acrylic solid pigment prepared according to the preparation method of any one of claims 1 to 9.
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