CN109777200B - Water-based environment-friendly non-erasable marker ink and preparation method thereof - Google Patents
Water-based environment-friendly non-erasable marker ink and preparation method thereof Download PDFInfo
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- CN109777200B CN109777200B CN201910180767.XA CN201910180767A CN109777200B CN 109777200 B CN109777200 B CN 109777200B CN 201910180767 A CN201910180767 A CN 201910180767A CN 109777200 B CN109777200 B CN 109777200B
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Abstract
The invention belongs to the technical field of chemical industry, and particularly relates to water-based environment-friendly non-erasable marker ink and a preparation method thereof. The technical scheme is as follows: the paint comprises 8-13 parts of pigment, 0.5-1.5 parts of dispersing agent, 0.2-0.4 part of defoaming agent, 0.8-2.0 parts of film-forming assistant, 4-8 parts of humectant, 12-15 parts of water, 10-15 parts of waterborne polyurethane resin, 7-3 parts of anti-settling agent and 57.5-42.1 parts of edible alcohol. The preparation method comprises the steps of firstly adding water and edible alcohol into a pre-dispersion kettle, adding a dispersing agent, a defoaming agent, a film-forming aid, a humectant and an anti-settling agent under low-speed stirring, uniformly mixing, adding a pigment, fully mixing, then transferring into a grinder for fine grinding, stopping grinding when the fineness of the mixture reaches 90nm or less, transferring into a finished product dispersion kettle, adding the waterborne polyurethane resin, uniformly mixing, and then discharging. The marking pen ink prepared by the invention is safe, environment-friendly, healthy and nontoxic, the pigment is not easy to settle, the stability is good, the solvent resistance is excellent, and written marks can be repeatedly wiped by most solvents and do not disappear.
Description
Technical Field
The invention belongs to the technical field of chemical industry, and particularly relates to water-based environment-friendly non-erasable marker ink and a preparation method thereof.
Background
The marking pen is named for its ability to make markings or logos on various writing media such as paper, wood, metal, glass, plastic, ceramic, etc. The marker is classified into an oil-based marker and a water-based marker. The water-based marker can be used for writing on a smooth object surface or a white board and can be wiped off by using a rag. In order to impart durability to a mark, the use of an oil-based marker is frequently seen in daily life.
Most of the conventional oil-based marker inks are organic solvents, and the solvents mainly include esters, ketones, benzene, alcohols and other organic solvents, such as butyl acetate, ethyl acetate, methyl isobutyl ketone, mixed xylene, butanol, isopropanol and the like, and mixtures thereof. They all volatilize into the atmosphere when in use, production and assembly, not only pollute the environment, but also harm human health. Especially, the influence on students and children is larger, and a plurality of uncomfortable symptoms such as headache, cough, allergy and the like can be caused after the volatile organic solvent is inhaled into a human body. As such, organic solvent-based ink markers have been used in developed countries to mark packages for food, pharmaceuticals, and toys. More importantly, under many use scenes, the traditional oily mark still cannot meet the requirement of erasure resistance. Such as: after writing a mark on a container containing an oily substance (alcohol, ink, solvent, etc.), the oily substance inevitably sticks to the outside of the container during use, and the written mark is erased together with a little carelessness when the oily substance is washed, thereby affecting the recognition of the article in the future.
Disclosure of Invention
The invention aims to provide the aqueous environment-friendly non-erasable marker ink and the preparation method thereof by combining the characteristics of high adhesion, high weather resistance, high water resistance, high solvent resistance, environmental protection and no toxicity of the aqueous polyurethane and the environment-friendly natural pigment based on the defects of the prior art.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows: the water-based environment-friendly non-erasable marker ink comprises the following components in parts by mass;
8-13 parts of pigment, 0.5-1.5 parts of dispersing agent, 0.2-0.4 part of defoaming agent, 0.8-2 parts of film-forming assistant, 4-8 parts of humectant, 12-15 parts of water, 10-15 parts of waterborne polyurethane resin, 7-3 parts of anti-settling agent and 57.5-42.1 parts of edible alcohol;
the waterborne polyurethane resin consists of the following raw materials in parts by weight:
17-21 parts of polyoxypropylene glycol with the relative molecular mass of 1000, 58.7-62.9 parts of water, 4-2 parts of dimethylolpropionic acid, 15-11 parts of isophorone diisocyanate, 0.4-0.2 part of 1, 4-butanediol, 3-1.5 parts of triethylamine and 1.9-1.4 parts of ethylenediamine;
the preparation method of the waterborne polyurethane resin comprises the following steps:
weighing 17-21 parts of polyoxypropylene glycol with the relative molecular mass of 1000, placing the polyoxypropylene glycol in a three-neck flask, dehydrating the polyoxypropylene glycol for 120min at the temperature of 120 ℃ and the vacuum degree of-0.09 MPa, cooling the polyoxypropylene glycol to 70-75 ℃, adding 4-2 parts of dimethylolpropionic acid, stirring and mixing the materials, then adding 15-11 parts of isophorone diisocyanate, reacting for 40min at the temperature of 70-75 ℃, heating the reaction temperature to 80-85 ℃, and reacting for 150min to obtain a carboxyl-containing polyurethane prepolymer;
adding 0.4-0.2 part of 1, 4-butanediol into the carboxyl-containing polyurethane prepolymer obtained in the step I, and carrying out chain extension reaction for 60min at the temperature of 80-85 ℃;
thirdly, when the temperature of the reactant subjected to chain extension in the second step is reduced to 55-60 ℃, 3-1.5 parts of triethylamine is added, and neutralization reaction is carried out for 30 min;
adding 1.9-1.4 parts of ethylenediamine, and carrying out end-capping reaction at 50-60 ℃ for 60 min;
finally adding 58.7-62.9 parts of water for emulsification and dispersion to obtain the waterborne polyurethane resin.
The pigment is one of natural red, blue or black plant pigments.
The dispersant is an aqueous dispersant.
The defoaming agent is a water-based defoaming agent.
The film-forming assistant is dipropylene glycol butyl ether or 2,2, 4-trimethyl-1, 3-pentanediol monoester.
The humectant is one of sorbitol, propylene glycol or water-soluble polyethylene glycol with the relative molecular mass of 400.
The anti-settling agent is nano silicon dioxide.
The preparation method of the water-based environment-friendly non-erasable marker ink specifically comprises the following steps:
firstly, adding 12-15 parts of water and 57.5-42.1 parts of edible alcohol into a pre-dispersion kettle, sequentially adding 0.5-1.5 parts of dispersing agent, 0.2-0.4 part of defoaming agent, 0.8-2 parts of film-forming additive, 4-8 parts of humectant and 7-3 parts of anti-settling agent according to the proportion under low-speed stirring, uniformly stirring and mixing, adding 8-13 parts of pigment, fully stirring and mixing, then transferring into a grinder for fine grinding, stopping grinding after the fineness of the mixture reaches the specification of less than or equal to 90nm, then transferring into a finished product dispersion kettle, adding 10-15 parts of waterborne polyurethane resin, continuously fully stirring and uniformly mixing, and then discharging to prepare the waterborne environment-friendly non-erasable marker ink.
The pigment is one of natural red, blue or black plant pigments.
The dispersant is an aqueous dispersant.
The defoaming agent is a water-based defoaming agent.
The film-forming assistant is dipropylene glycol butyl ether or 2,2, 4-trimethyl-1, 3-pentanediol monoester.
The humectant is one of sorbitol, propylene glycol or water-soluble polyethylene glycol with the relative molecular mass of 400.
The anti-settling agent is nano silicon dioxide.
Compared with the prior art, the invention has the following advantages:
1. the natural pigment is fully wrapped by utilizing the high adhesion, high weather resistance, high water resistance and high solvent resistance of the waterborne polyurethane, when the ink is written on a medium, the ink can be quickly dried to form a film, and the written mark also has excellent scratch resistance due to the excellent solvent resistance of the waterborne polyurethane.
2. Compared with the traditional organic solvent type oil type marker ink, the organic solvent type marker ink takes water and edible alcohol as solvents, is environment-friendly and nontoxic, does not cause harm to human bodies, and can reduce the production cost.
3. The water-based polyurethane has the moisturizing wettability, so that the marking pen filled with the ink can still keep moisture for a long time after uncapping under the condition of reducing the using amount of a moisturizing agent in the ink, thereby achieving the purpose of intermittent writing.
4. The addition of the anti-settling agent can prevent the ink from deterioration phenomena such as layering, pigment settling and the like for a long time.
The physicochemical properties of the aqueous environmentally-friendly non-erasable marker ink were tested with reference to relevant standards, and the measured properties are shown in table 1.
TABLE 1 physicochemical Properties of an aqueous environmental non-erasable marker ink
Detailed Description
Example 1:
the water-based environment-friendly non-erasable marker ink disclosed by the embodiment of the invention comprises the following components in parts by mass;
8 parts of natural red plant pigment, 0.5 part of dispersant, 0.2 part of defoamer, 0.8 part of dipropylene glycol butyl ether, 4 parts of sorbitol, 12 parts of water, 10 parts of waterborne polyurethane resin, 7 parts of nano silicon dioxide and 57.5 parts of edible alcohol; the dispersant is Borchi Gen 0451 aqueous dispersant of OMG Borchers company; the defoaming agent is BYK-024 aqueous defoaming agent of Bick company of Germany.
The method for preparing the water-based environment-friendly non-erasable marker ink specifically comprises the following steps:
firstly, adding 12 parts of water and 57.5 parts of edible alcohol into a pre-dispersion kettle, sequentially adding 0.5 part of dispersing agent, 0.2 part of defoaming agent, 0.8 part of dipropylene glycol butyl ether, 4 parts of sorbitol and 7 parts of nano silicon dioxide according to the proportion under low-speed stirring, uniformly stirring and mixing, then adding 8 parts of natural red plant pigment, fully stirring and mixing, then transferring into a grinder for fine grinding, stopping grinding after the fineness of the mixture reaches the specification of less than or equal to 90nm, then transferring into a finished product dispersion kettle, adding 10 parts of waterborne polyurethane resin, continuously fully stirring and uniformly mixing, and then discharging to obtain the waterborne environment-friendly non-erasable marker ink.
The waterborne polyurethane resin described in the embodiment is composed of the following raw materials in parts by mass:
17 parts of polyoxypropylene glycol with the relative molecular mass of 1000, 58.7 parts of water, 4 parts of dimethylolpropionic acid, 15 parts of isophorone diisocyanate, 0.4 part of 1, 4-butanediol, 3 parts of triethylamine and 1.9 parts of ethylenediamine.
The preparation method of the waterborne polyurethane resin described in this embodiment comprises the following steps:
weighing 17 parts of polyoxypropylene glycol with the relative molecular mass of 1000, placing the polyoxypropylene glycol in a three-neck flask, dehydrating the polyoxypropylene glycol for 120min at the temperature of 120 ℃ and the vacuum degree of-0.09 MPa, cooling the polyoxypropylene glycol to 70-75 ℃, adding 4 parts of dimethylolpropionic acid, stirring and mixing the materials, then adding 15 parts of isophorone diisocyanate, reacting for 40min at the temperature of 70-75 ℃, heating the reaction temperature to 80-85 ℃, and reacting for 150min to obtain a carboxyl-containing polyurethane prepolymer;
adding 0.4 part of 1, 4-butanediol into the carboxyl-containing polyurethane prepolymer obtained in the step I, and carrying out chain extension reaction for 60min at the temperature of 80-85 ℃;
thirdly, adding 3 parts of triethylamine when the temperature of the reactant subjected to chain extension in the second step is reduced to 55-60 ℃, and performing neutralization reaction for 30 min;
adding 1.9 parts of ethylenediamine, and carrying out end-capping reaction at 50-60 ℃ for 60 min;
finally adding 58.7 parts of water for emulsification and dispersion to obtain the waterborne polyurethane resin.
Example 2:
the aqueous environment-friendly non-erasable marker ink disclosed by the embodiment of the invention consists of the following components in parts by mass;
13 parts of natural black plant pigment, 1.5 parts of dispersant, 0.4 part of defoamer, 2 parts of 2,2, 4-trimethyl-1, 3-pentanediol monoester, 8 parts of propylene glycol, 15 parts of water, 15 parts of waterborne polyurethane resin, 3 parts of nano silicon dioxide and 42.1 parts of edible alcohol; the dispersant is Borchi Gen 0851 aqueous dispersant of OMG Borchers company; the defoaming agent is BYK-019 water-based defoaming agent of Germany Bike company.
The method for preparing the water-based environment-friendly non-erasable marker ink specifically comprises the following steps:
firstly, adding 15 parts of water and 42.1 parts of edible alcohol into a pre-dispersion kettle, sequentially adding 1.5 parts of dispersing agent, 0.4 part of defoaming agent, 2, 4-trimethyl-1, 3-pentanediol monoester, 2 parts of propylene glycol and 3 parts of nano silicon dioxide according to the proportion under low-speed stirring, uniformly stirring and mixing, then adding 13 parts of natural black plant pigment, fully stirring and mixing, then transferring into a grinder for fine grinding, stopping grinding after the fineness of the mixture reaches the specification of less than or equal to 90nm, then transferring into a finished product dispersion kettle, adding 15 parts of waterborne polyurethane resin, continuously stirring and uniformly mixing, and then discharging to prepare the waterborne environment-friendly non-erasable marker ink.
The waterborne polyurethane resin described in the embodiment is composed of the following raw materials in parts by mass:
21 parts of polyoxypropylene glycol with the relative molecular mass of 1000, 62.9 parts of water, 2 parts of dimethylolpropionic acid, 11 parts of isophorone diisocyanate, 0.2 part of 1, 4-butanediol, 1.5 parts of triethylamine and 1.4 parts of ethylenediamine.
The preparation method of the waterborne polyurethane resin described in this embodiment comprises the following steps:
weighing 21 parts of polyoxypropylene glycol with the relative molecular mass of 1000, placing the polyoxypropylene glycol in a three-neck flask, dehydrating the polyoxypropylene glycol for 120min at the temperature of 120 ℃ and the vacuum degree of-0.09 MPa, cooling the polyoxypropylene glycol to 70-75 ℃, adding 2 parts of dimethylolpropionic acid, stirring and mixing the materials, then adding 11 parts of isophorone diisocyanate, reacting for 40min at the temperature of 70-75 ℃, heating the reaction temperature to 80-85 ℃, and reacting for 150min to obtain a carboxyl-containing polyurethane prepolymer;
adding 0.2 part of 1, 4-butanediol into the carboxyl-containing polyurethane prepolymer obtained in the step I, and carrying out chain extension reaction for 60min at the temperature of 80-85 ℃;
thirdly, adding 1.5 parts of triethylamine when the temperature of the reactant subjected to chain extension in the second step is reduced to 55-60 ℃, and performing neutralization reaction for 30 min;
adding 1.4 parts of ethylenediamine, and carrying out end-capping reaction at 50-60 ℃ for 60 min;
finally adding 62.9 parts of water for emulsification and dispersion to obtain the waterborne polyurethane resin.
Example 3:
the aqueous environment-friendly non-erasable marker ink disclosed by the embodiment of the invention consists of the following components in parts by mass;
11 parts of natural blue plant pigment, 1.2 parts of dispersant, 0.3 part of defoamer, 1.5 parts of dipropylene glycol butyl ether, 6 parts of water-soluble polyethylene glycol with the relative molecular mass of 400, 13 parts of water, 13 parts of waterborne polyurethane resin, 5 parts of nano silicon dioxide and 49 parts of edible alcohol; the dispersant is Borchi Gen 0451 aqueous dispersant of OMG Borchers company; the defoaming agent is BYK-028 aqueous defoaming agent of Germany Bike company.
The method for preparing the water-based environment-friendly non-erasable marker ink specifically comprises the following steps:
firstly, adding 13 parts of water and 49 parts of edible alcohol into a pre-dispersion kettle, sequentially adding 1.2 parts of dispersing agent, 0.3 part of defoaming agent, 1.5 parts of dipropylene glycol butyl ether, 6 parts of water-soluble polyethylene glycol with the relative molecular mass of 400 and 5 parts of nano silicon dioxide according to the proportion under low-speed stirring, uniformly stirring and mixing, then adding 11 parts of natural blue plant pigment, fully stirring and mixing, then transferring into a grinder for fine grinding, stopping grinding after the fineness of the mixture reaches the specification of less than or equal to 90nm, then transferring into a finished product dispersion kettle, adding 13 parts of waterborne polyurethane resin, continuously fully stirring and uniformly mixing, and then discharging to prepare the water-based environment-friendly non-erasable marker ink.
The waterborne polyurethane resin described in the embodiment is composed of the following raw materials in parts by mass:
19 parts of polypropylene oxide glycol with the relative molecular mass of 1000, 60.8 parts of water, 3 parts of dimethylolpropionic acid, 13 parts of isophorone diisocyanate, 0.3 part of 1, 4-butanediol, 2.3 parts of triethylamine and 1.6 parts of ethylenediamine.
The preparation method of the waterborne polyurethane resin described in this embodiment comprises the following steps:
weighing 19 parts of polyoxypropylene glycol with the relative molecular mass of 1000, placing the polyoxypropylene glycol in a three-neck flask, dehydrating the polyoxypropylene glycol for 120min at the temperature of 120 ℃ and the vacuum degree of-0.09 MPa, cooling the polyoxypropylene glycol to 70-75 ℃, adding 3 parts of dimethylolpropionic acid, stirring and mixing the materials, then adding 13 parts of isophorone diisocyanate, reacting for 40min at the temperature of 70-75 ℃, heating the reaction temperature to 80-85 ℃, and reacting for 150min to obtain a carboxyl-containing polyurethane prepolymer;
adding 0.3 part of 1, 4-butanediol into the carboxyl-containing polyurethane prepolymer obtained in the step I, and carrying out chain extension reaction for 60min at the temperature of 80-85 ℃;
thirdly, 2.3 parts of triethylamine is added when the temperature of the reactant subjected to chain extension in the second step is reduced to 55-60 ℃, and neutralization reaction is carried out for 30 min;
adding 1.6 parts of ethylenediamine, and carrying out end-capping reaction at 50-60 ℃ for 60 min;
finally adding 60.8 parts of water for emulsification and dispersion to obtain the waterborne polyurethane resin.
Example 4:
the aqueous environment-friendly non-erasable marker ink disclosed by the embodiment of the invention consists of the following components in parts by mass;
10 parts of natural red plant pigment, 0.8 part of dispersant, 0.2 part of defoamer, 1.2 parts of 2,2, 4-trimethyl-1, 3-pentanediol monoester, 5 parts of sorbitol, 12 parts of water, 12 parts of waterborne polyurethane resin, 6 parts of nano silicon dioxide and 52.8 parts of edible alcohol; the dispersant is Borchi Gen 0851 aqueous dispersant of OMG Borchers company; the defoaming agent is BYK-024 aqueous defoaming agent of Bick company of Germany.
The method for preparing the water-based environment-friendly non-erasable marker ink specifically comprises the following steps:
firstly, adding 12 parts of water and 52.8 parts of edible alcohol into a pre-dispersion kettle, sequentially adding 0.8 part of dispersing agent, 0.2 part of defoaming agent, 1.2 parts of 2,2, 4-trimethyl-1, 3-pentanediol monoester, 5 parts of sorbitol and 6 parts of nano-silica according to the proportion under low-speed stirring, uniformly stirring and mixing, then adding 10 parts of natural red plant pigment, fully stirring and mixing, then transferring into a grinder for fine grinding, stopping grinding after the fineness of the mixture reaches the specification of less than or equal to 90nm, then transferring into a finished product dispersion kettle, adding 12 parts of waterborne polyurethane resin, continuously stirring and uniformly mixing, and then discharging to prepare the waterborne environment-friendly non-erasable marker ink.
The waterborne polyurethane resin described in the embodiment is composed of the following raw materials in parts by mass:
17 parts of polyoxypropylene glycol with the relative molecular mass of 1000, 58.7 parts of water, 4 parts of dimethylolpropionic acid, 15 parts of isophorone diisocyanate, 0.4 part of 1, 4-butanediol, 3 parts of triethylamine and 1.9 parts of ethylenediamine.
The preparation method of the waterborne polyurethane resin described in this embodiment comprises the following steps:
weighing 17 parts of polyoxypropylene glycol with the relative molecular mass of 1000, placing the polyoxypropylene glycol in a three-neck flask, dehydrating the polyoxypropylene glycol for 120min at the temperature of 120 ℃ and the vacuum degree of-0.09 MPa, cooling the polyoxypropylene glycol to 70-75 ℃, adding 4 parts of dimethylolpropionic acid, stirring and mixing the materials, then adding 15 parts of isophorone diisocyanate, reacting for 40min at the temperature of 70-75 ℃, heating the reaction temperature to 80-85 ℃, and reacting for 150min to obtain a carboxyl-containing polyurethane prepolymer;
adding 0.4 part of 1, 4-butanediol into the carboxyl-containing polyurethane prepolymer obtained in the step I, and carrying out chain extension reaction for 60min at the temperature of 80-85 ℃;
thirdly, adding 3 parts of triethylamine when the temperature of the reactant subjected to chain extension in the second step is reduced to 55-60 ℃, and performing neutralization reaction for 30 min;
adding 1.9 parts of ethylenediamine, and carrying out end-capping reaction at 50-60 ℃ for 60 min;
finally adding 58.7 parts of water for emulsification and dispersion to obtain the waterborne polyurethane resin.
Example 5:
the aqueous environment-friendly non-erasable marker ink disclosed by the embodiment of the invention consists of the following components in parts by mass;
12 parts of natural black plant pigment, 1.4 parts of dispersant, 0.4 part of defoamer, 1.8 parts of dipropylene glycol butyl ether, 7 parts of water-soluble polyethylene glycol with the relative molecular mass of 400, 14 parts of water, 14 parts of waterborne polyurethane resin, 4 parts of nano silicon dioxide and 45.4 parts of edible alcohol; the dispersant is Borchi Gen 0851 aqueous dispersant of OMG Borchers company; the defoaming agent is BYK-019 water-based defoaming agent of Germany Bike company.
The method for preparing the water-based environment-friendly non-erasable marker ink specifically comprises the following steps:
firstly, adding 14 parts of water and 45.4 parts of edible alcohol into a pre-dispersion kettle, sequentially adding 1.4 parts of a dispersing agent, 0.4 part of a defoaming agent, 1.8 parts of dipropylene glycol butyl ether, 7 parts of water-soluble polyethylene glycol with the relative molecular mass of 400 and 4 parts of nano silicon dioxide according to the proportion under low-speed stirring, uniformly stirring and mixing, adding 12 parts of natural black plant pigment, fully stirring and mixing, transferring into a grinder for fine grinding, stopping grinding after the fineness of the mixture reaches the specification of less than or equal to 90nm, transferring into a finished product dispersion kettle, adding 14 parts of waterborne polyurethane resin, continuously fully stirring and uniformly mixing, and discharging to prepare the waterborne environment-friendly non-erasable marker ink.
The waterborne polyurethane resin described in the embodiment is composed of the following raw materials in parts by mass:
21 parts of polyoxypropylene glycol with the relative molecular mass of 1000, 62.9 parts of water, 2 parts of dimethylolpropionic acid, 11 parts of isophorone diisocyanate, 0.2 part of 1, 4-butanediol, 1.5 parts of triethylamine and 1.4 parts of ethylenediamine.
The preparation method of the waterborne polyurethane resin described in this embodiment comprises the following steps:
weighing 21 parts of polyoxypropylene glycol with the relative molecular mass of 1000, placing the polyoxypropylene glycol in a three-neck flask, dehydrating the polyoxypropylene glycol for 120min at the temperature of 120 ℃ and the vacuum degree of-0.09 MPa, cooling the polyoxypropylene glycol to 70-75 ℃, adding 2 parts of dimethylolpropionic acid, stirring and mixing the materials, then adding 11 parts of isophorone diisocyanate, reacting for 40min at the temperature of 70-75 ℃, heating the reaction temperature to 80-85 ℃, and reacting for 150min to obtain a carboxyl-containing polyurethane prepolymer;
adding 0.2 part of 1, 4-butanediol into the carboxyl-containing polyurethane prepolymer obtained in the step I, and carrying out chain extension reaction for 60min at the temperature of 80-85 ℃;
thirdly, adding 1.5 parts of triethylamine when the temperature of the reactant subjected to chain extension in the second step is reduced to 55-60 ℃, and performing neutralization reaction for 30 min;
adding 1.4 parts of ethylenediamine, and carrying out end-capping reaction at 50-60 ℃ for 60 min;
finally adding 62.9 parts of water for emulsification and dispersion to obtain the waterborne polyurethane resin.
Claims (4)
1. An aqueous environment-friendly non-erasable marker ink is characterized in that: consists of the following components in portion by mass
8-13 parts of pigment, 0.5-1.5 parts of dispersing agent, 0.2-0.4 part of defoaming agent, 0.8-2.0 parts of film-forming assistant, 4-8 parts of humectant, 12-15 parts of water, 10-15 parts of waterborne polyurethane resin, 3-7 parts of anti-settling agent and 42.1-57.5 parts of edible alcohol;
the waterborne polyurethane resin consists of the following raw materials in parts by weight:
17-21 parts of polyoxypropylene glycol with the relative molecular mass of 1000, 58.7-62.9 parts of water, 2-4 parts of dimethylolpropionic acid, 11-15 parts of isophorone diisocyanate, 0.2-0.4 part of 1, 4-butanediol, 1.5-3 parts of triethylamine and 1.4-1.9 parts of ethylenediamine;
the preparation method of the waterborne polyurethane resin comprises the following steps:
weighing 17-21 parts of polyoxypropylene glycol with the relative molecular mass of 1000, placing the polyoxypropylene glycol in a three-neck flask, dehydrating the polyoxypropylene glycol for 120min at the temperature of 120 ℃ and the vacuum degree of-0.09 MPa, cooling the polyoxypropylene glycol to 70-75 ℃, adding 2-4 parts of dimethylolpropionic acid, stirring and mixing the materials, then adding 11-15 parts of isophorone diisocyanate, reacting for 40min at the temperature of 70-75 ℃, heating the reaction temperature to 80-85 ℃, and reacting for 150min to obtain a carboxyl-containing polyurethane prepolymer;
adding 0.2-0.4 part of 1, 4-butanediol into the carboxyl-containing polyurethane prepolymer obtained in the step I, and carrying out chain extension reaction for 60min at the temperature of 80-85 ℃;
thirdly, cooling the reactant subjected to chain extension in the second step to 55-60 ℃, adding 1.5-3 parts of triethylamine, and performing neutralization reaction for 30 min;
adding 1.4-1.9 parts of ethylenediamine, and carrying out end-capping reaction at 50-60 ℃ for 60 min;
finally adding 58.7-62.9 parts of water for emulsification and dispersion to obtain the waterborne polyurethane resin;
the method for preparing the water-based environment-friendly non-erasable marker ink comprises the following steps:
firstly, adding 12-15 parts of water and 42.1-57.5 parts of edible alcohol into a pre-dispersion kettle, sequentially adding 0.5-1.5 parts of dispersing agent, 0.2-0.4 part of defoaming agent, 0.8-2.0 parts of film-forming additive, 4-8 parts of humectant and 3-7 parts of anti-settling agent according to the proportion under low-speed stirring, stirring uniformly, adding 8-13 parts of pigment, stirring and mixing fully, transferring into a grinder for fine grinding to enable the fineness of the mixture to reach the specification of less than or equal to 90nm, stopping grinding, transferring into a finished product dispersion kettle, adding 10-15 parts of waterborne polyurethane resin, stirring uniformly, and discharging to prepare the waterborne environment-friendly non-erasable marker ink;
the pigment is one of natural red, blue or black plant pigments;
the film-forming assistant is dipropylene glycol butyl ether or 2,2, 4-trimethyl-1, 3-pentanediol monoester;
the humectant is one of sorbitol, propylene glycol or water-soluble polyethylene glycol with the relative molecular mass of 400;
the anti-settling agent is nano silicon dioxide.
2. The aqueous environmentally friendly non-erasable marker ink of claim 1, wherein: the dispersant is an aqueous dispersant.
3. The aqueous environmentally friendly non-erasable marker ink of claim 1, wherein: the defoaming agent is a water-based defoaming agent.
4. A process for preparing the aqueous environmentally friendly non-erasable marker ink of any one of claims 1 to 3, characterized by: the method comprises the following steps:
firstly, adding 12-15 parts of water and 42.1-57.5 parts of edible alcohol into a pre-dispersion kettle, sequentially adding 0.5-1.5 parts of dispersing agent, 0.2-0.4 part of defoaming agent, 0.8-2.0 parts of film-forming additive, 4-8 parts of humectant and 3-7 parts of anti-settling agent according to the proportion under low-speed stirring, stirring uniformly, adding 8-13 parts of pigment, stirring and mixing fully, transferring into a grinder for fine grinding to enable the fineness of the mixture to reach the specification of less than or equal to 90nm, stopping grinding, transferring into a finished product dispersion kettle, adding 10-15 parts of waterborne polyurethane resin, stirring uniformly, and discharging to obtain the waterborne environment-friendly non-erasable marker ink.
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|---|---|---|---|---|
| CN101585904A (en) * | 2008-05-21 | 2009-11-25 | 北京高盟燕山科技有限公司 | Method for preparing binder resin for water-based ink and application thereof |
| CN102532463A (en) * | 2011-12-26 | 2012-07-04 | 四川达威科技股份有限公司 | Aqueous polyurethane and preparation method thereof |
| CN106752367A (en) * | 2016-12-29 | 2017-05-31 | 晋江市美德文具有限公司 | The neutral pen ink and its manufacture method of a kind of high stability |
| CN107083110A (en) * | 2017-06-14 | 2017-08-22 | 中国科学院福建物质结构研究所 | Gel ink pen neutral ink composition and preparation method thereof |
-
2019
- 2019-03-11 CN CN201910180767.XA patent/CN109777200B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101585904A (en) * | 2008-05-21 | 2009-11-25 | 北京高盟燕山科技有限公司 | Method for preparing binder resin for water-based ink and application thereof |
| CN102532463A (en) * | 2011-12-26 | 2012-07-04 | 四川达威科技股份有限公司 | Aqueous polyurethane and preparation method thereof |
| CN106752367A (en) * | 2016-12-29 | 2017-05-31 | 晋江市美德文具有限公司 | The neutral pen ink and its manufacture method of a kind of high stability |
| CN107083110A (en) * | 2017-06-14 | 2017-08-22 | 中国科学院福建物质结构研究所 | Gel ink pen neutral ink composition and preparation method thereof |
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Address after: No. 8, Economic and Technological Development Zone, Guangling County, Datong City, Shanxi Province, 037500 Patentee after: Datong Yingkeao Pen Ink Technology Co., Ltd. Address before: 037501 Zuo Tuan Xiang Ping Cheng Cun, Guangling County, Datong City, Shanxi Province Patentee before: DATONG INKALL CHEMICAL TECHNOLOGY CO.,LTD. |