CN118027742A - Method for preparing water-based ink by modifying natural rosin - Google Patents
Method for preparing water-based ink by modifying natural rosin Download PDFInfo
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- CN118027742A CN118027742A CN202410121312.1A CN202410121312A CN118027742A CN 118027742 A CN118027742 A CN 118027742A CN 202410121312 A CN202410121312 A CN 202410121312A CN 118027742 A CN118027742 A CN 118027742A
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- rosin
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- polyethylene glycol
- based ink
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- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 title claims abstract description 156
- KHPCPRHQVVSZAH-HUOMCSJISA-N Rosin Natural products O(C/C=C/c1ccccc1)[C@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 KHPCPRHQVVSZAH-HUOMCSJISA-N 0.000 title claims abstract description 156
- KHPCPRHQVVSZAH-UHFFFAOYSA-N trans-cinnamyl beta-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OCC=CC1=CC=CC=C1 KHPCPRHQVVSZAH-UHFFFAOYSA-N 0.000 title claims abstract description 156
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 73
- 238000000034 method Methods 0.000 title claims abstract description 20
- 239000002202 Polyethylene glycol Substances 0.000 claims abstract description 60
- 150000002148 esters Chemical class 0.000 claims abstract description 60
- 229920001223 polyethylene glycol Polymers 0.000 claims abstract description 60
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 49
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims abstract description 37
- 239000011230 binding agent Substances 0.000 claims abstract description 37
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 32
- 238000003756 stirring Methods 0.000 claims abstract description 26
- 238000002360 preparation method Methods 0.000 claims abstract description 25
- 239000000839 emulsion Substances 0.000 claims abstract description 23
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims abstract description 21
- 238000002156 mixing Methods 0.000 claims abstract description 20
- 239000003054 catalyst Substances 0.000 claims abstract description 19
- 239000002270 dispersing agent Substances 0.000 claims abstract description 15
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 14
- 239000008367 deionised water Substances 0.000 claims abstract description 14
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 14
- 239000000049 pigment Substances 0.000 claims abstract description 13
- 239000002518 antifoaming agent Substances 0.000 claims abstract description 12
- 238000009835 boiling Methods 0.000 claims abstract description 10
- 239000003999 initiator Substances 0.000 claims abstract description 9
- 229920002565 Polyethylene Glycol 400 Polymers 0.000 claims description 12
- 238000010438 heat treatment Methods 0.000 claims description 11
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 6
- FDZZZRQASAIRJF-UHFFFAOYSA-M malachite green Chemical group [Cl-].C1=CC(N(C)C)=CC=C1C(C=1C=CC=CC=1)=C1C=CC(=[N+](C)C)C=C1 FDZZZRQASAIRJF-UHFFFAOYSA-M 0.000 claims description 6
- 229940107698 malachite green Drugs 0.000 claims description 6
- USHAGKDGDHPEEY-UHFFFAOYSA-L potassium persulfate Chemical group [K+].[K+].[O-]S(=O)(=O)OOS([O-])(=O)=O USHAGKDGDHPEEY-UHFFFAOYSA-L 0.000 claims description 6
- OQBLGYCUQGDOOR-UHFFFAOYSA-L 1,3,2$l^{2}-dioxastannolane-4,5-dione Chemical compound O=C1O[Sn]OC1=O OQBLGYCUQGDOOR-UHFFFAOYSA-L 0.000 claims description 5
- 238000004321 preservation Methods 0.000 claims description 5
- GCLGEJMYGQKIIW-UHFFFAOYSA-H sodium hexametaphosphate Chemical compound [Na]OP1(=O)OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])OP(=O)(O[Na])O1 GCLGEJMYGQKIIW-UHFFFAOYSA-H 0.000 claims description 5
- 235000019982 sodium hexametaphosphate Nutrition 0.000 claims description 5
- 239000001577 tetrasodium phosphonato phosphate Substances 0.000 claims description 5
- 239000000203 mixture Substances 0.000 claims description 4
- 230000001105 regulatory effect Effects 0.000 claims description 4
- AMTWCFIAVKBGOD-UHFFFAOYSA-N dioxosilane;methoxy-dimethyl-trimethylsilyloxysilane Chemical group O=[Si]=O.CO[Si](C)(C)O[Si](C)(C)C AMTWCFIAVKBGOD-UHFFFAOYSA-N 0.000 claims description 2
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 2
- 229940083037 simethicone Drugs 0.000 claims description 2
- 239000013530 defoamer Substances 0.000 claims 1
- 239000002253 acid Substances 0.000 abstract description 16
- 238000007639 printing Methods 0.000 abstract description 11
- 238000001035 drying Methods 0.000 abstract description 10
- 230000003647 oxidation Effects 0.000 abstract description 5
- 238000007254 oxidation reaction Methods 0.000 abstract description 5
- 239000000976 ink Substances 0.000 description 66
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 18
- 239000000243 solution Substances 0.000 description 10
- 239000012855 volatile organic compound Substances 0.000 description 10
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- 239000011347 resin Substances 0.000 description 7
- 229920005989 resin Polymers 0.000 description 7
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 239000012752 auxiliary agent Substances 0.000 description 4
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 4
- 230000000977 initiatory effect Effects 0.000 description 4
- 238000005259 measurement Methods 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 229920002545 silicone oil Polymers 0.000 description 4
- 238000010521 absorption reaction Methods 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 239000002904 solvent Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 238000009736 wetting Methods 0.000 description 3
- 239000004925 Acrylic resin Substances 0.000 description 2
- 229920000178 Acrylic resin Polymers 0.000 description 2
- 238000003917 TEM image Methods 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 238000013329 compounding Methods 0.000 description 2
- 238000005886 esterification reaction Methods 0.000 description 2
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- 238000004806 packaging method and process Methods 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- 239000012086 standard solution Substances 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- RSWGJHLUYNHPMX-ONCXSQPRSA-N abietic acid Chemical group C([C@@H]12)CC(C(C)C)=CC1=CC[C@@H]1[C@]2(C)CCC[C@@]1(C)C(O)=O RSWGJHLUYNHPMX-ONCXSQPRSA-N 0.000 description 1
- 235000013361 beverage Nutrition 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
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- 239000003153 chemical reaction reagent Substances 0.000 description 1
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- 125000004185 ester group Chemical group 0.000 description 1
- 238000004880 explosion Methods 0.000 description 1
- 238000007647 flexography Methods 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 125000000524 functional group Chemical group 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000001023 inorganic pigment Substances 0.000 description 1
- 239000004816 latex Substances 0.000 description 1
- 229920000126 latex Polymers 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000005543 nano-size silicon particle Substances 0.000 description 1
- 239000012860 organic pigment Substances 0.000 description 1
- 238000005191 phase separation Methods 0.000 description 1
- 229920000058 polyacrylate Polymers 0.000 description 1
- 229940068918 polyethylene glycol 400 Drugs 0.000 description 1
- 229920002635 polyurethane Polymers 0.000 description 1
- 239000004814 polyurethane Substances 0.000 description 1
- 238000003918 potentiometric titration Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- AHBGXTDRMVNFER-UHFFFAOYSA-L strontium dichloride Chemical class [Cl-].[Cl-].[Sr+2] AHBGXTDRMVNFER-UHFFFAOYSA-L 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000004448 titration Methods 0.000 description 1
- 239000002966 varnish Substances 0.000 description 1
Landscapes
- Inks, Pencil-Leads, Or Crayons (AREA)
Abstract
The invention discloses a preparation method for preparing water-based ink by modifying natural rosin, which comprises the following steps: ① The rosin ethylene glycol is prepared by uniformly stirring and mixing natural rosin, an emulsifying agent and a catalyst; ② Preparing a pre-emulsion: the method comprises the steps of carrying out ultrasonic mixing on an emulsifier, an initiator, acrylic acid and deionized water to obtain the product; ③ Preparation of an acrylic modified rosin binder: adding NaHCO 3 solution and boiling water into the prepared rosin polyethylene glycol ester, adding the prepared 1/2 volume of pre-emulsion, stirring and reacting, and adding the rest pre-emulsion to prepare the acrylic acid modified rosin binder; ④ Preparation of aqueous ink: and adding a dispersing agent, a defoaming agent, a pigment agent and deionized water into the prepared acrylic modified rosin binder to obtain the water-based ink. The water-based ink prepared by the invention has the advantages of better low viscosity, low acid value and high fixed content, can remarkably improve the stability, printing adhesiveness and drying speed of the ink, has strong oxidation resistance and can be stored for a long time.
Description
Technical Field
The invention belongs to the technical field of ink production, and particularly relates to a preparation method for preparing water-based ink by modifying natural rosin.
Background
The water-based ink has been widely used in the printing industry, especially in the production of flexible packages and paper, because of its advantages of fast drying speed, strong adhesion and near zero emission. Compared with the traditional ink based on the organic solvent, the water-based ink uses water as the solvent, so that the use of the organic solvent is reduced, the emission of Volatile Organic Compounds (VOC) is reduced, the harmful emission in the printing process is relatively low, the healthier working environment is provided, the water-based ink is generally free of dangerous chemicals, the treatment and storage of the water-based ink are safer, and fire or explosion is unlikely to be caused. The water-based ink has the advantages of low price, good adhesive force after printing, quick drying, strong water resistance and the like, and is widely used for packaging printed matters in industries of foods, medicines, beverages and the like.
In recent years, many people adopt various compounding methods to produce water-based ink, such as compounding substances such as polyacrylate and silicon dioxide to prepare the water-based ink, the preparation method is that acrylic acid and other substances are used, water-based acrylic resin is generated through a better reaction method, the modified nano silicon dioxide is used for modifying the water-based acrylic resin, so that the finally obtained water-based ink has better film forming property after printing, high brightness and good ink adaptability, and can be applied to flexography and gravure to produce high-grade packaging printed matters.
The natural rosin has the characteristics of degradability, heat resistance, hydrophobicity and the like, is compounded with the acrylic acid product, and has the advantages of high gloss, high hardness, solvent resistance, high attaching strength and the like of the acrylic acid product. Therefore, the preparation of the water-based ink by adopting the acrylic acid modified natural rosin resin is an effective means which is economical, environment-friendly and better in use effect at present.
Disclosure of Invention
In order to solve the problems in the background art, the invention aims to provide the preparation method for preparing the water-based ink by modifying the natural rosin, which has the advantages of simple process, low raw material cost, strong adaptability, excellent product performance and long-time storage.
The preparation method of the water-based ink by modifying natural rosin is characterized by comprising the following steps of:
① Preparing rosin ethylene glycol, namely uniformly stirring and mixing natural rosin, an emulsifying agent and a catalyst, wherein the adding amount of the emulsifying agent is 35-45% of the mass of the natural rosin, the adding amount of the catalyst is 25-35% of the mass of the natural rosin, heating to 130-150 ℃, and carrying out heat preservation reaction for 3-4 hours at 130-150 ℃ to obtain rosin polyethylene glycol ester;
② Preparing a pre-emulsion: the rosin polyethylene glycol ester is prepared by ultrasonic mixing of an emulsifier accounting for 35 to 45 percent of the mass of the rosin polyethylene glycol ester, an initiator accounting for 8 to 12 percent of the mass of the rosin polyethylene glycol ester, acrylic acid accounting for 5 to 15 percent of the mass of the rosin polyethylene glycol ester and deionized water accounting for 2 to 3 times of the mass of the rosin polyethylene glycol ester;
③ Preparation of an acrylic modified rosin binder: when the temperature of the rosin polyethylene glycol ester prepared in the step ① is reduced to 50-60 ℃, adding 0.1mol/L NaHCO 3 solution and boiling water into the rosin polyethylene glycol ester, then heating to 80-90 ℃, adding 1/2 volume of the pre-emulsion prepared in the step ②, stirring and reacting for 30-40 min, adding the rest of the pre-emulsion, stirring and reacting for 30-40 min, filtering, and regulating the PH to 8-9.5 to prepare the acrylic acid modified rosin binder;
④ Preparation of aqueous ink: adding 8-12% of dispersing agent, 45-55% of defoaming agent and 1-3% of pigment agent into the acrylic acid modified rosin binder prepared in the step ③, adding 2-3 times of deionized water into the acrylic acid modified rosin binder, stirring, and uniformly mixing by ultrasonic to obtain the water-based ink.
Further, in step ①, the catalyst is one of alumina and stannous oxalate or a mixture of both.
Further, in step ① and step ②, the emulsifier is PEG-400, and PEG-400 is polyethylene glycol 400, and the product is directly purchased when in use.
Further, in step ②, the initiator is potassium persulfate.
Further, in step ③, the addition amount of the NaHCO 3 solution is 4-6% of the rosin polyethylene glycol ester by volume.
Further, in step ③, boiling water is added in an amount of 2 to 3 times the mass of the rosin polyethylene glycol ester.
Further, in step ④, the dispersing agent is OT-75 type or sodium hexametaphosphate, the dispersing agent is OT-75 type wetting dispersing agent, and has the functions of wetting, dispersing and stabilizing, and can be used as wetting and leveling agent in the aspects of coating, printing ink and varnish, and can be directly used for purchasing finished products on trial production
Further, in step ④, the antifoaming agent is simethicone.
Further, in step ④, the pigment is malachite green.
Compared with the traditional mode for preparing the water-based ink, the invention has the advantages that:
According to the invention, natural rosin is adopted as a raw material for preparing the water-based ink, so that the cost is low, the utilization rate of the rosin is improved, the preparation of the water-based ink is effectively reduced, meanwhile, the rosin is mainly used as a vehicle in the ink, the adhesive force of the ink to paper can be enhanced, the printing effect of the ink is improved, if the rosin is not used in the ink, the phenomenon of dull and blurred color tone of the printed ink is generated, and after the rosin is added, the color tone of the printed ink is harmonious, the handwriting is clear, and the use effect is good;
The acrylic acid modified natural rosin resin is adopted, so that the characteristics of degradability, heat resistance, hydrophobicity and the like of rosin are reserved, the advantages of high gloss, high hardness, solvent resistance, high attaching strength and the like of an acrylic acid product are increased, the formed acrylic acid rosin resin with multiple functional groups can be better compatible with organic and inorganic pigments, the universality of the ink is improved, the rosin resin is adopted as a raw material, the water-based ink has better low viscosity, low acid value and high fixed content, the prepared water-based ink has low viscosity of 320-400 mPa.s, low acid value of 10-25 mg/NaOHg and high fixed content of 80-90%, the stability, printing adhesiveness and drying speed of the ink are obviously improved, and the emission of Volatile Organic Compounds (VOC) is reduced;
the raw materials adopted by the invention are easy to obtain, the preparation process is simple and easy to implement, the prepared water-based ink can be used in the fields of flexible packages, paper and the like for application, the application range is wide, the applicability is strong, the water-based ink has excellent compatibility to different auxiliary agents, the bonding effect is good, the oxidation resistance is strong, and the water-based ink can be stored for a long time.
Drawings
FIG. 1 is a Fourier transform Infrared Spectroscopy (FTIR) diagram of the esterification reaction of rosin with an emulsifier in example 1;
FIG. 2 is a TEM image of an acrylic-modified rosin binder obtained from the acrylic-modified rosin resin in example 1;
Detailed Description
The invention is further described below with reference to the examples and the accompanying drawings, which are not in any way limiting, but are any changes or substitutions based on the teachings of the invention, and which fall within the scope of the invention.
The invention provides a preparation method for preparing water-based ink by modifying natural rosin, which comprises the following steps:
① Preparing rosin ethylene glycol, namely uniformly stirring and mixing natural rosin, an emulsifying agent and a catalyst, wherein the emulsifying agent is PEG-400, the catalyst is one or a mixture of aluminum oxide and stannous oxalate, the adding amount of the emulsifying agent is 35-45% of the mass of the natural rosin, the adding amount of the catalyst is 25-35% of the mass of the natural rosin, heating to 130-150 ℃, and carrying out heat preservation reaction for 3-4 h at 130-150 ℃ to obtain rosin polyethylene glycol ester;
② Preparing a pre-emulsion: the emulsion is prepared by ultrasonic mixing of an emulsifier with the mass of 35-45% of rosin polyethylene glycol ester, an initiator with the mass of 8-12% of rosin polyethylene glycol ester, acrylic acid with the mass of 5-15% of rosin polyethylene glycol ester and deionized water with the mass of 2-3 times of that of rosin polyethylene glycol ester, wherein the emulsifier is PEG-400, and the initiator is potassium persulfate;
③ Preparation of an acrylic modified rosin binder: when the temperature of the rosin polyethylene glycol ester prepared in the step ① is reduced to 50-60 ℃, adding 0.1mol/L NaHCO 3 solution and boiling water into the rosin polyethylene glycol ester, wherein the addition amount of the NaHCO 3 solution is 4-6% of the volume of the rosin polyethylene glycol ester, adding 2-3 times of the mass of the rosin polyethylene glycol ester, heating to 80-90 ℃, adding 1/2 volume of the pre-emulsion prepared in the step ②, stirring for reacting for 30-40 min, adding the rest of the pre-emulsion, stirring for reacting for 30-40 min, filtering, and adjusting the PH to 8-9.5 to prepare the acrylic acid modified rosin binder;
④ Preparation of aqueous ink: adding 8-12% of dispersing agent, 45-55% of defoaming agent and 1-3% of pigment agent into the acrylic acid modified rosin binder prepared in the step ③, wherein the pigment agent is malachite green, the dispersing agent is OT-75 or sodium hexametaphosphate, the defoaming agent is dimethyl silicone oil, adding deionized water with 2-3 times of the mass of the acrylic acid modified rosin binder, stirring, and uniformly mixing by ultrasonic to obtain the water-based ink.
The following are exemplary but non-limiting examples of the invention:
Example 1
The preparation method of the water-based ink prepared by modifying the natural rosin in the embodiment 1 comprises the following steps:
① Preparing rosin ethylene glycol, namely uniformly stirring and mixing natural rosin, an emulsifying agent and a catalyst, wherein the emulsifying agent is PEG-400, the catalyst is alumina, the adding amount of the emulsifying agent is 35% of the mass of the natural rosin, the adding amount of the catalyst is 25% of the mass of the natural rosin, the temperature is raised to 130 ℃, the reaction is kept for 3 hours at 130 ℃, the inventor adopts Fourier transform infrared spectroscopy (FTIR) to characterize the rosin polyethylene glycol ester, as shown in figure 1, the result shows that a broadband is provided at 3439 cm -1, which is the stretching vibration characteristic of an-OH group in a rosin carboxylic acid group, a strong absorption peak is provided at 1690 cm -1, which is the characteristic peak of a C=O group in the rosin acid group, an asymmetric deformation vibration absorption peak of C-H is provided at 1460 cm -1, a strong absorption peak appears at 1102 cm -1, which is the characteristic peak of an ester group, and indicates that esterification reaction of rosin and PEG-400 occurs;
② Preparing a pre-emulsion: the rosin polyethylene glycol ester is prepared by ultrasonic mixing of an emulsifying agent accounting for 35% of the mass of rosin polyethylene glycol ester, an initiating agent accounting for 8% of the mass of rosin polyethylene glycol ester, acrylic acid accounting for 5% of the mass of rosin polyethylene glycol ester and deionized water accounting for 2 times of the mass of rosin polyethylene glycol ester, wherein the emulsifying agent is PEG-400, and the initiating agent is potassium persulfate;
③ Preparation of an acrylic modified rosin binder: when the temperature of the rosin polyethylene glycol ester prepared in the step ① is reduced to 50 ℃, adding 0.1mol/L NaHCO 3 solution and boiling water into the rosin polyethylene glycol ester, wherein the addition amount of the NaHCO 3 solution is 4% of the volume of the rosin polyethylene glycol ester, 2 times of the mass of the rosin polyethylene glycol ester, heating to 80 ℃, adding 1/2 volume of the pre-emulsion prepared in the step ②, stirring for reacting for 30min, adding the rest of the pre-emulsion, stirring for reacting for 30min, filtering, and regulating the pH to 8 by using NaOH to prepare the acrylic acid modified rosin binder; the inventor adopts a Transmission Electron Microscope (TEM) to analyze the microstructure of the prepared acrylic acid modified rosin binder, as shown in figure 2, as can be seen from figure 2, the latex particles of the prepared acrylic acid modified rosin binder are uniformly distributed in a spherical shape, and can be observed in TEM images of acrylic acid modified rosin resin, the acrylic acid modified rosin binder with a shell-core structure is successfully prepared, the prepared acrylic acid modified rosin binder has a neat particle structure, and a layer of protection rings is formed around emulsion particles by the emulsifier, so that the acrylic acid rosin resin has good stability;
④ Preparation of aqueous ink: adding 8% of dispersing agent, 45% of defoaming agent and 1% of pigment agent into the acrylic modified rosin binder prepared in the step ③, wherein the pigment agent is malachite green, the dispersing agent is OT-75 type, the defoaming agent is dimethyl silicone oil, deionized water with the mass being 2 times that of the acrylic modified rosin binder is added, stirring and uniformly mixing by ultrasonic to obtain the water-based ink.
The inventors measured the solid content, acid value and viscosity of the aqueous ink prepared in example 1 by taking three samples, and the measurement results are shown in table 1:
TABLE 1
As can be seen from the data in Table 1, the aqueous ink prepared in example 1 has an average solid content of 83.43%, an average acid value of 19.39mg/NaOHg, an average viscosity of 320.76mpa.s, and average fluidity and dryness of 11.03s and 11.5s, respectively, which indicates that the aqueous ink prepared has a good low viscosity, a low acid value and a high fixed content, can remarkably improve the stability of the ink, the printing adhesion and the drying speed, reduces the emission of Volatile Organic Compounds (VOC), has excellent compatibility with different auxiliary agents, has a good bonding effect, and has a strong oxidation resistance and can be stored for a long time.
Example 2
Example 2 the method for preparing water-based ink by modifying natural rosin in example 1 comprises the following steps:
① Preparing rosin ethylene glycol, namely uniformly stirring and mixing natural rosin, an emulsifying agent and a catalyst, wherein the emulsifying agent is PEG-400, the catalyst is stannous oxalate, the adding amount of the emulsifying agent is 40% of the mass of the natural rosin, the adding amount of the catalyst is 30% of the mass of the natural rosin, heating to 140 ℃, and carrying out heat preservation reaction for 3.5 hours at 140 ℃ to obtain rosin polyethylene glycol ester;
② Preparing a pre-emulsion: the rosin polyethylene glycol ester is prepared by ultrasonic mixing of an emulsifying agent accounting for 40% of the mass of rosin polyethylene glycol ester, an initiating agent accounting for 10% of the mass of rosin polyethylene glycol ester, acrylic acid accounting for 10% of the mass of rosin polyethylene glycol ester and deionized water accounting for 2.5 times of the mass of rosin polyethylene glycol ester, wherein the emulsifying agent is PEG-400, and the initiating agent is potassium persulfate;
③ Preparation of an acrylic modified rosin binder: when the temperature of the rosin polyethylene glycol ester prepared in the step ① is reduced to 55 ℃, adding 0.1mol/L NaHCO 3 solution and boiling water into the rosin polyethylene glycol ester, wherein the addition amount of the NaHCO 3 solution is 5% of the volume of the rosin polyethylene glycol ester, the addition amount of the boiling water is 2.5 times of the mass of the rosin polyethylene glycol ester, then heating to 85 ℃, adding 1/2 volume of the pre-emulsion prepared in the step ②, stirring and reacting for 35min, adding the rest of the pre-emulsion, stirring and reacting for 35min, filtering, and adjusting the pH to 8.5 by NaOH to prepare the acrylic acid modified rosin binder;
④ Preparation of aqueous ink: adding 10% of dispersing agent, 50% of defoaming agent and 2% of pigment agent into the acrylic modified rosin binder prepared in the step ③, wherein the pigment agent is malachite green, the dispersing agent is OT-75 type or sodium hexametaphosphate, the defoaming agent is dimethyl silicone oil, adding deionized water with the mass of 2.5 times of the acrylic modified rosin binder, stirring, and uniformly mixing by ultrasonic to obtain the water-based ink.
The inventors measured the solid content, acid value and viscosity of the aqueous ink prepared in example 2 by taking three samples, and the measurement results are shown in table 2:
TABLE 2
As can be seen from the data in Table 2, the aqueous ink prepared in example 2 has an average solid content of 81.2%, an average acid value of 18.24mg/NaOHg, an average viscosity of 355.43mpa.s, and average fluidity and dryness of 11.65s and 37.65s, respectively, which indicates that the aqueous ink prepared has a relatively good low viscosity, a low acid value and a high fixed content, can remarkably improve the stability, printing adhesion and drying speed of the ink, reduces the emission of Volatile Organic Compounds (VOC), has excellent compatibility with different auxiliary agents, and has good bonding effect and strong oxidation resistance, and can be stored for a long time.
Example 3
Example 3 the method for preparing water-based ink by modifying natural rosin in example 1 comprises the following steps:
① Preparing rosin ethylene glycol, namely uniformly stirring and mixing natural rosin, an emulsifying agent and a catalyst, wherein the emulsifying agent is PEG-400, the catalyst is a mixture of alumina and stannous oxalate in an equal ratio, the adding amount of the emulsifying agent is 45% of the mass of the natural rosin, the adding amount of the catalyst is 35% of the mass of the natural rosin, heating to 150 ℃, and carrying out heat preservation reaction for 4 hours at 150 ℃ to obtain rosin polyethylene glycol ester;
② Preparing a pre-emulsion: the rosin polyethylene glycol ester is prepared by ultrasonic mixing of an emulsifier accounting for 45% of the mass of the rosin polyethylene glycol ester, an initiator accounting for 12% of the mass of the rosin polyethylene glycol ester, acrylic acid accounting for 15% of the mass of the rosin polyethylene glycol ester and deionized water which is 3 times of the mass of the rosin polyethylene glycol ester, wherein the emulsifier is PEG-400, and the initiator is potassium persulfate;
③ Preparation of an acrylic modified rosin binder: when the temperature of the rosin polyethylene glycol ester prepared in the step ① is reduced to 60 ℃, adding 0.1mol/L NaHCO 3 solution and boiling water into the rosin polyethylene glycol ester, wherein the addition amount of the NaHCO 3 solution is 6% of the volume of the rosin polyethylene glycol ester, 3 times of the mass of the rosin polyethylene glycol ester, heating to 90 ℃, adding 1/2 volume of the pre-emulsion prepared in the step ②, stirring for reacting for 30-40 min, adding the rest of the pre-emulsion, stirring for reacting for 30-40 min, filtering, and regulating the pH to 9 by NaOH to prepare the acrylic acid modified rosin binder;
④ Preparation of aqueous ink: adding a dispersing agent with the mass of 12% of the acrylic acid modified rosin binder, a defoaming agent with the mass of 55% of the acrylic acid modified rosin binder and a pigment with the mass of 3% into the acrylic acid modified rosin binder prepared in the step ③, wherein the pigment is malachite green, the dispersing agent is OT-75 or sodium hexametaphosphate, the defoaming agent is dimethyl silicone oil, adding deionized water with the mass of 3 times of the acrylic acid modified rosin binder, stirring, and uniformly mixing by ultrasonic to obtain the water-based ink.
The inventors measured the solid content, acid value and viscosity of the aqueous ink prepared in example 3 by taking three samples, and the measurement results are shown in table 3:
TABLE 3 Table 3
As can be seen from the data in Table 3, the aqueous ink prepared in example 3 has an average solid content of 81.6%, an average acid value of 20.85mg/NaOHg, an average viscosity of 361.83mpa.s and average fluidity and dryness of 10.41 and 18.31s, respectively, which indicates that the aqueous ink prepared has a relatively good low viscosity, a low acid value and a high fixed content, can remarkably improve the stability of the ink, the printing adhesion and the drying speed, reduces the emission of Volatile Organic Compounds (VOC), has excellent compatibility to different auxiliary agents, has a good bonding effect and strong oxidation resistance, and can be stored for a long time.
In the present invention, the solid content, acid value, viscosity, fluidity and dryness in the aqueous ink were measured in examples 1 to 3 described above by the following measurement methods:
The solids content in the examples is determined by the method described in the "Effects of the reagent molar ratio on the phase separation and properties of waterborne polyurethane for application in a water-based ink binder" literature.
(1)
Wherein G is the solid content of the aqueous ink binder; m 2: total mass g after drying; m 1: total mass g before drying; m: mass g of the dish.
The acid number in the examples is determined by the method described in the "Effects of calcium, magnesium, and strontium chlorides in determining the total acid number using potentiometric titration" literature.
(2)
Wherein, X: acid value of the aqueous ink binder; v: volume of sodium hydroxide standard solution consumed during titration; m: molar concentration of sodium hydroxide standard solution; w: sample weight g;40:1 mol/L NaOH equivalent.
Measurement of viscosity in examples viscosity of aqueous inks was measured accurately using an NDJ-5S Pro digital viscometer.
The fluidity was measured by the inclined drop method, the clean glass dish was placed horizontally, and the time taken for the ink to run from the edge to the center was recorded with a stopwatch.
Dryness test ink drying times were recorded with a stopwatch at fixed temperature, humidity and pressure.
The data in tables 1,2, and 3, measured using the above measurement methods, are true and valid.
Claims (9)
1. The preparation method for preparing the water-based ink by modifying the natural rosin is characterized by comprising the following steps of:
① Preparing rosin ethylene glycol, namely uniformly stirring and mixing natural rosin, an emulsifying agent and a catalyst, wherein the adding amount of the emulsifying agent is 35-45% of the mass of the natural rosin, the adding amount of the catalyst is 25-35% of the mass of the natural rosin, heating to 130-150 ℃, and carrying out heat preservation reaction for 3-4 hours at 130-150 ℃ to obtain rosin polyethylene glycol ester;
② Preparing a pre-emulsion: the rosin polyethylene glycol ester is prepared by ultrasonic mixing of an emulsifier accounting for 35 to 45 percent of the mass of the rosin polyethylene glycol ester, an initiator accounting for 8 to 12 percent of the mass of the rosin polyethylene glycol ester, acrylic acid accounting for 5 to 15 percent of the mass of the rosin polyethylene glycol ester and deionized water accounting for 2 to 3 times of the mass of the rosin polyethylene glycol ester;
③ Preparation of an acrylic modified rosin binder: when the temperature of the rosin polyethylene glycol ester prepared in the step ① is reduced to 50-60 ℃, adding 0.1mol/L NaHCO 3 solution and boiling water into the rosin polyethylene glycol ester, then heating to 80-90 ℃, adding 1/2 volume of the pre-emulsion prepared in the step ②, stirring and reacting for 30-40 min, adding the rest of the pre-emulsion, stirring and reacting for 30-40 min, filtering, and regulating the PH to 8-9.5 to prepare the acrylic acid modified rosin binder;
④ Preparation of aqueous ink: adding 8-12% of dispersing agent, 45-55% of defoaming agent and 1-3% of pigment agent into the acrylic acid modified rosin binder prepared in the step ③, adding 2-3 times of deionized water into the acrylic acid modified rosin binder, stirring, and uniformly mixing by ultrasonic to obtain the water-based ink.
2. The method for preparing the water-based ink by modifying the natural rosin according to claim 1, which is characterized by comprising the following steps: in step ①, the catalyst is one or a mixture of aluminum oxide and stannous oxalate.
3. The method for preparing the water-based ink by modifying the natural rosin according to claim 1, which is characterized by comprising the following steps: in steps ① and ②, the emulsifier is PEG-400.
4. The method for preparing the water-based ink by modifying the natural rosin according to claim 1, which is characterized by comprising the following steps: in step ②, the initiator is potassium persulfate.
5. The method for preparing the water-based ink by modifying the natural rosin according to claim 1, which is characterized by comprising the following steps: in the step ③, the addition amount of the NaHCO 3 solution is 4-6% of the volume of the rosin polyethylene glycol ester.
6. The method for preparing the water-based ink by modifying the natural rosin according to claim 1, which is characterized by comprising the following steps: in the step ③, the adding amount of boiling water is 2-3 times of the mass of the rosin polyethylene glycol ester.
7. The method for preparing the water-based ink by modifying the natural rosin according to claim 1, which is characterized by comprising the following steps: in step ④, the dispersant is OT-75 type or sodium hexametaphosphate.
8. The method for preparing the water-based ink by modifying the natural rosin according to claim 1, which is characterized by comprising the following steps: in step ④, the defoamer is simethicone.
9. The method for preparing the water-based ink by modifying the natural rosin according to claim 1, which is characterized by comprising the following steps: in step ④, the pigment is malachite green.
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