CN114634734B - Flame-retardant water-based gravure printing ink and preparation method thereof - Google Patents
Flame-retardant water-based gravure printing ink and preparation method thereof Download PDFInfo
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- CN114634734B CN114634734B CN202210279624.6A CN202210279624A CN114634734B CN 114634734 B CN114634734 B CN 114634734B CN 202210279624 A CN202210279624 A CN 202210279624A CN 114634734 B CN114634734 B CN 114634734B
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/14—Printing inks based on carbohydrates
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/10—Printing inks based on artificial resins
- C09D11/106—Printing inks based on artificial resins containing macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
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Abstract
The invention discloses flame-retardant water-based gravure printing ink which is prepared from starch, polyvinyl alcohol, pigment, hexafluoropropylene dimer, nickel sulfate, sodium hypochlorite, a pasting agent and deionized water. The flame-retardant water-based gravure printing ink disclosed by the invention is excellent in comprehensive performance, simple and easy to operate in preparation process, stable in quality of the prepared composite material, safe and environment-friendly in preparation process, and a brand-new preparation technology.
Description
Technical Field
The invention belongs to the technical field of printing, and relates to flame-retardant water-based gravure printing ink and a preparation method thereof.
Background
Most of the resins, pigments, solvents, auxiliaries and the like contained in conventional printing inks have an influence on the environment. As one of the environmental protection inks, the main application fields of the water-based ink are gravure printing and flexographic printing. However, the current gravure ink, flexographic water-based ink and UV-curable ink cannot be completely green, environment-friendly and ecological ink. In order to achieve the environment-friendly ink in the real sense, the emission of volatile organic compounds is reduced from the aspects of raw material selection, product use and final treatment, so that the raw materials for preparing the ink are easier to degrade in the nature under the action of physics, chemistry and biology, or renewable substances are utilized as raw materials and the like. The water-based gravure ink as a green and environment-friendly ink has the greatest characteristics of difficult combustion, good safety, no influence on human health and no pollution to the environment. The danger of inflammable solvents and electrostatic fire is reduced, the toxic residue on the surface of the printed matter is reduced, and the printing equipment is convenient to clean. However, the currently used water-based gravure ink still has the defects of complicated preparation process, high cost, single use, poor water resistance, adhesion, wear resistance, poor drying property and the like. Therefore, the development of multi-purpose, environment-friendly, low-cost and high-quality water-based gravure ink is still an important research direction in the ink field.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a novel water-based gravure ink which is simple in preparation process, low in price, multipurpose, environment-friendly and good in flame retardant property and a preparation method thereof.
In order to realize the purpose of the invention, the invention adopts the following technical scheme:
the flame-retardant water-based gravure printing ink is prepared from the following components in parts by weight:
1 part of starch, namely 1 part of starch,
1 to 10 parts of polyvinyl alcohol,
0.15 to 0.75 portion of hexafluoropropylene dimer,
0.001 to 0.01 portion of nickel sulfate,
0.15 to 0.25 portion of sodium hypochlorite,
0.05 to 0.1 portion of pasting agent,
the pigment is a plurality of pigments,
and a plurality of deionized water.
Further, the starch is firstly prepared into a starch aqueous solution by using deionized water, and the mass ratio of the starch to the deionized water in the starch aqueous solution is 1:10 to 20; firstly, preparing polyvinyl alcohol into a polyvinyl alcohol aqueous solution by using deionized water, wherein the mass ratio of the polyvinyl alcohol to the deionized water in the polyvinyl alcohol aqueous solution is 1:10 to 20; the mass ratio of the starch aqueous solution to the polyvinyl alcohol aqueous solution is 1:1 to 10; the pigment is 5-10% of the weight of the starch water solution and the polyvinyl alcohol water solution.
Further, the polyvinyl alcohol type is one or any two of PVA2099, PVA1799, PVA2088 and PVA 1788.
Further, the starch is one or a mixture of any two or three of wheat starch, corn starch and potato starch; the starch is white powder without peculiar smell, the protein content is less than or equal to 0.5 percent, and the solid content is more than or equal to 96 percent; the ash content is less than or equal to 0.1 percent, and the fineness is 90 to 110 meshes.
Further, the pigment is selected from one of carbon black, titanium dioxide and phthalocyanine blue according to color requirements.
Further, the pasting agent is hydroxide or carbonate of alkali metal and alkaline earth metal.
The invention also aims to provide a preparation method of the flame-retardant water-based gravure printing ink, which adopts the following technical scheme:
a preparation method of flame-retardant water-based gravure printing ink comprises the following steps:
1) Mixing 1 weight part of starch and 10 to 20 weight parts of deionized water, stirring uniformly, slowly heating to 60 ℃, keeping the temperature and stirring, adding 0.15 to 0.25 weight part of hypochlorous acid aqueous solution containing sodium hypochlorite while stirring, keeping the temperature and stirring continuously, adding 0.15 to 0.75 weight part of hexafluoropropylene dimer and 0.001 to 0.01 weight part of nickel sulfate, keeping the temperature and stirring continuously, adding 0.05 to 0.1 weight part of alkali metal and alkaline earth metal hydroxides or carbonate aqueous solution, keeping the temperature and stirring to obtain uniform and transparent light yellow colloid;
2) In addition, slowly mixing 1-10 parts by weight of polyvinyl alcohol and 10-20 parts by weight of deionized water in a container, and stirring at 60 ℃ until the polyvinyl alcohol is completely dispersed and dissolved to prepare a polyvinyl alcohol solution;
3) And (3) mixing the light yellow colloid obtained in the step 1) and the polyvinyl alcohol obtained in the step 2), adding the pigment after uniformly stirring, and uniformly stirring to obtain the flame-retardant water-based gravure ink.
The flame-retardant water-based gravure printing ink is composed of starch, polyvinyl alcohol, pigment, hexafluoropropylene dimer, nickel sulfate, sodium hypochlorite, pasting agent and deionized water, wherein the polyvinyl alcohol is used as water-soluble polymer resin, a molecular chain contains a large amount of hydroxyl groups, the water-soluble polyvinyl alcohol is good in water solubility, and the flame-retardant water-based gravure printing ink is harmless, non-toxic, pollution-free, good in bonding force, toughness, film-forming property and emulsibility and excellent in solvent resistance and oil resistance. The polyvinyl alcohol and the starch molecules contain hydroxyl, so hydrogen bonds can be formed between the polyvinyl alcohol and the starch molecules, the grafting effect between the polyvinyl alcohol and the starch molecules is realized, and the performances of fluidity, caking property, freezing resistance and the like of the connecting material prepared from the mixed emulsion of the polyvinyl alcohol and the starch molecules are optimized. Polyvinyl alcohol can adjust the adhesive property. When the solvent is volatilized during heating, the polyvinyl alcohol molecules can be in close contact with each other, and a film with mechanical properties is formed through intermolecular adsorption. In general, polyvinyl alcohol having a large degree of polymerization has a large adhesive strength.
The starch granule has high permeability, can be dissolved in water, and water molecules can freely enter the interior of the starch granule. The sodium hypochlorite is added in the production to modify the starch, so that water molecules penetrate into the starch granules, and the performance index of the starch is improved. The starch is composed of amylose and amylopectin. The amylose does not contain phosphorus, can be dissolved in hot water, has the polymerization degree of about 70-350, does not generate paste and accounts for about 23 percent of the starch; amylopectin has branches, contains a phosphate ester, is insoluble, can be made into paste, and has an average degree of polymerization of 280-5100, which accounts for about 77% of starch. The modified starch is a good binder because amylopectin can be pasted and amylose can promote gelatinization.
The pigment has strong alkali resistance and can be well dispersed in water.
In the oxidation process of the starch, a proper amount of nickel sulfate is added as a catalyst, so that macromolecular chains of the starch and glycosidic bonds in the macromolecules are broken, hydroxyl groups in a glucose unit of the starch are oxidized into carboxyl and aldehyde groups, the dispersibility, stability, cohesiveness and cold flow property of the starch are improved, the problems of poor water resistance, stability and cohesiveness and the like of the starch are solved, the initial adhesion of the starch is increased, the reaction time of starch gelatinization is shortened, the hydrophilicity of starch molecules is improved, the film forming rate of a cementing surface is increased, and a more uniform adhesive film is formed.
According to the flame-retardant water-based gravure printing ink, sodium hypochlorite is used as an oxidant, after starch is oxidized, a glucoside bond is broken, and hydroxyl is introduced, so that the flame-retardant water-based gravure printing ink has good stability, dispersibility, cold flow property and bonding property; the polyvinyl alcohol is added to increase the toughness of the starch binder and promote film formation; alkali metal and alkaline earth metal hydroxides or carbonates as pasting agents destroy the granular structure of starch and cause the granules to swell, and starch molecules are hydrated and then dissolved in water; the nickel sulfate is used as a catalyst, so that the oxidation process can be accelerated; the hexafluoropropylene dipolymer has specific heat value larger than 1, freezing point of zero, and good flame retardant property, and has the functions of a surfactant and a defoaming agent as well as flame retardant property after being oxidized and hydrolyzed by an oxidant in a reaction system. The starch has the advantages of improving the fluidity, transparency, moisture retention, gloss and color retention, weather resistance, durability, corrosion resistance, quick drying, high hardness and the like of starch in an ink system.
The flame-retardant water-based gravure printing ink disclosed by the invention is excellent in comprehensive performance, simple and easy to operate in preparation process, stable in quality of the prepared composite material, safe and environment-friendly in preparation process, and a brand-new preparation technology.
Detailed Description
The present invention will be described in more detail with reference to the following examples. The practice of the present invention is not limited to the following examples, and any modification or variation of the present invention is within the scope of the present invention.
Example 1
1) 1 kg of corn starch and 10 kg of deionized water are mixed and stirred uniformly, the temperature is slowly raised to 60 ℃, the temperature is kept and the stirring is carried out for 30 minutes, an aqueous solution prepared from 0.15 kg of sodium hypochlorite and 1.5 kg of deionized water is added under the stirring, the temperature is kept and the stirring is carried out for 30 minutes, 0.15 kg of hexafluoropropylene dimer and 1 g of nickel sulfate are added, the temperature is kept and the stirring is carried out for 30 minutes, an aqueous solution prepared from 0.05 kg of sodium hydroxide and 0.5 kg of deionized water is added, and the temperature is kept and the stirring is carried out until the uniform and transparent faint yellow colloid is obtained.
2) 1 kg of polyvinyl alcohol (model PVA 2099) and 10 kg of deionized water are slowly stirred and mixed in another container, and the mixture is stirred at 60 ℃ until the polyvinyl alcohol is completely dispersed and dissolved to prepare the polyvinyl alcohol solution.
3) And mixing the prepared uniform and transparent light yellow colloid with a polyvinyl alcohol solution, uniformly stirring, adding 1.1 kg of pigment carbon black, and uniformly stirring to obtain the flame-retardant water-based gravure ink.
The corn starch in example 1 can be replaced by wheat starch or potato starch, or a mixture of any two of wheat starch, corn starch and potato starch, or a mixture of three of wheat starch, corn starch and potato starch; the sodium hydroxide can be replaced by sodium carbonate, potassium carbonate, calcium carbonate, potassium hydroxide or calcium hydroxide; wherein, preparing sodium hypochlorite aqueous solution, the amount of water can dissolve sodium hypochlorite, preparing sodium hydroxide aqueous solution, and the amount of water can dissolve sodium hydroxide.
Example 2
1) 1 kg of wheat starch and 20 kg of deionized water are mixed and stirred uniformly, the temperature is slowly raised to 60 ℃, the temperature is kept and the stirring is carried out for 30 minutes, 0.25 kg of sodium hypochlorite and 2.5 kg of deionized water are added under the stirring, the temperature is kept and the stirring is carried out for 30 minutes, 0.75 kg of hexafluoropropylene dimer and 10 g of nickel sulfate are added, the temperature is kept and the stirring is carried out for 30 minutes, 0.1 kg of potassium hydroxide and 1 kg of deionized water are added, and the heat is kept and the stirring is carried out until the mixture is uniform and transparent faint yellow colloid.
2) 1 kg of polyvinyl alcohol (model PVA 1799) and 20 kg of deionized water are slowly stirred and mixed in another container, and stirred at 60 ℃ until the polyvinyl alcohol is completely dispersed and dissolved to prepare the polyvinyl alcohol solution.
3) And mixing the prepared uniform and transparent light yellow colloid with a polyvinyl alcohol solution, uniformly stirring, adding 4.2 kg of pigment carbon black, and uniformly stirring to obtain the flame-retardant water-based gravure ink.
The wheat starch in example 2 can be replaced by corn starch or potato starch, or by a mixture of any two of wheat starch, corn starch and potato starch, or by a mixture of three of wheat starch, corn starch and potato starch; the potassium hydroxide can be replaced by sodium carbonate, potassium carbonate, calcium carbonate, sodium hydroxide or calcium hydroxide; wherein, the sodium hypochlorite aqueous solution is prepared, the sodium hypochlorite can be dissolved by the amount of water, and the potassium hydroxide aqueous solution can be prepared, the potassium hydroxide can be dissolved by the amount of water.
Example 3
1) Mixing and stirring 1 kg of potato starch and 15 kg of deionized water uniformly, slowly heating to 60 ℃, keeping the temperature and stirring for 30 minutes, adding an aqueous solution prepared from 0.20 kg of sodium hypochlorite and 2 kg of deionized water while stirring, continuing to keep the temperature and stirring for 30 minutes, adding 0.45 kg of hexafluoropropylene dimer and 5 g of nickel sulfate, continuing to keep the temperature and stirring for 30 minutes, adding an aqueous solution prepared from 0.08 kg of sodium hydroxide and 0.8 kg of deionized water, keeping the temperature and stirring to obtain a uniform and transparent light yellow colloid.
2) 2 kg of polyvinyl alcohol (model PVA 2099) and 30 kg of deionized water are slowly stirred and mixed in another container, and stirred at 60 ℃ until the polyvinyl alcohol is completely dispersed and dissolved to prepare the polyvinyl alcohol solution.
3) And mixing the prepared uniform and transparent light yellow colloid with a polyvinyl alcohol solution, uniformly stirring, adding 4.8 kg of pigment carbon black, and uniformly stirring to obtain the flame-retardant water-based gravure ink.
The potato starch in example 3 can be replaced by corn starch or wheat starch, or by a mixture of any two of wheat starch, corn starch and potato starch, or by a mixture of three of wheat starch, corn starch and potato starch; the potassium hydroxide can be replaced by sodium carbonate, potassium carbonate, calcium carbonate, sodium hydroxide or calcium hydroxide; wherein, sodium hypochlorite aqueous solution is prepared, the amount of water can dissolve sodium hypochlorite, and potassium hydroxide aqueous solution is prepared, and the amount of water can dissolve potassium hydroxide.
Example 4
1) Mixing and stirring 0.5 kg of corn starch, 0.5 kg of wheat starch and 15 kg of deionized water uniformly, slowly heating to 60 ℃, keeping the temperature and stirring for 30 minutes, adding an aqueous solution prepared from 0.15 kg of sodium hypochlorite and 1.5 kg of deionized water while stirring, keeping the temperature and stirring for 30 minutes, adding 0.15 kg of hexafluoropropylene dimer and 1 g of nickel sulfate, keeping the temperature and stirring for 30 minutes, adding an aqueous solution prepared from 0.05 kg of sodium hydroxide and 0.5 kg of deionized water, keeping the temperature and stirring to obtain a uniform and transparent light yellow colloid.
2) Slowly stirring and mixing 5 kg of polyvinyl alcohol (type PVA 2099), 5 kg of polyvinyl alcohol (type PVA 2088) and 200 kg of deionized water in another container, and stirring at 60 ℃ until the polyvinyl alcohol is completely dispersed and dissolved to prepare the polyvinyl alcohol solution.
3) And mixing the prepared uniform and transparent light yellow colloid with a polyvinyl alcohol solution, uniformly stirring, adding 11.25 kg of pigment titanium dioxide, and uniformly stirring to obtain the flame-retardant water-based gravure ink.
Example 5
1) Mixing and stirring 1 kg of potato starch and 20 kg of deionized water uniformly, slowly heating to 60 ℃, keeping the temperature and stirring for 30 minutes, adding an aqueous solution prepared from 0.25 kg of sodium hypochlorite and 2.5 kg of deionized water while stirring, continuing to keep the temperature and stirring for 30 minutes, adding 0.5 kg of hexafluoropropylene dimer and 10 g of nickel sulfate, continuing to keep the temperature and stirring for 30 minutes, adding an aqueous solution prepared from 0.1 kg of sodium carbonate and 1 kg of deionized water, keeping the temperature and stirring to obtain a uniform and transparent light yellow colloid.
2) In another container, 5 kg of polyvinyl alcohol (model PVA 1788) and 100 kg of deionized water are slowly stirred and mixed, and stirred at 60 ℃ until the polyvinyl alcohol is completely dispersed and dissolved to prepare the polyvinyl alcohol solution.
3) And mixing the prepared uniform and transparent light yellow colloid with a polyvinyl alcohol solution, stirring uniformly, adding 12.6 kilograms of pigment phthalocyanine blue, and stirring uniformly to obtain the flame-retardant water-based gravure ink.
Example 6
1) 1 kg of wheat starch and 10 kg of deionized water are mixed and stirred uniformly, the temperature is slowly raised to 60 ℃, the mixture is kept warm and stirred for 30 minutes, aqueous solution prepared from 0.15 kg of sodium hypochlorite and 1.5 kg of deionized water is added under stirring, the mixture is kept warm and stirred for 30 minutes, 0.3 kg of hexafluoropropylene dimer and 5 g of nickel sulfate are added, the mixture is kept warm and stirred for 30 minutes, aqueous solution prepared from 0.1 kg of sodium potassium carbonate and 1 kg of deionized water is added, and the mixture is kept warm and stirred to form uniform and transparent light yellow colloid.
2) 8 kg of polyvinyl alcohol (model PVA 2099) and 160 kg of deionized water are slowly stirred and mixed in another container, and the mixture is stirred at 60 ℃ until the polyvinyl alcohol is completely dispersed and dissolved to prepare the polyvinyl alcohol solution.
3) And mixing the prepared uniform and transparent light yellow colloid with a polyvinyl alcohol solution, uniformly stirring, adding 15.12 kg of pigment carbon black, and uniformly stirring to obtain the flame-retardant water-based gravure ink.
The products obtained in examples 1 to 6 were subjected to the performance tests, the results of which are shown in the following table:
| examples | Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | Example 6 |
| Appearance of the product | Light brightness | Light brightness | Light brightness | Brightness | Light brightness | Light brightness |
| Residual solvent and heavy metal | Is free of | Is free of | Is free of | Is composed of | Is free of | Is free of |
| Viscosity/mpa.s | 128 | 132 | 135 | 141 | 134 | 126 |
| Fineness/um | 4 | 3.8 | 3.9 | 2.8 | 3.2 | 2.9 |
| Solvent resistance/grade | 6 | 6 | 6 | 5 | 6 | 6 |
| Adhesion/grade | 7 | 8 | 6 | 7 | 6 | 7 |
| Water resistance/grade | 5 | 6 | 6 | 5 | 6 | 5 |
| Abrasion resistance/grade | 6 | 6 | 7 | 6 | 5 | 7 |
| Anti-yellowing/grade | 6 | 5 | 7 | 6 | 6 | 5 |
Claims (4)
1. The flame-retardant water-based gravure printing ink is characterized by being prepared from the following components in parts by weight:
1 part of starch, namely 1 part of starch,
1 to 10 parts of polyvinyl alcohol,
0.15 to 0.75 portion of hexafluoropropylene dimer,
0.001 to 0.01 portion of nickel sulfate,
0.15 to 0.25 portion of sodium hypochlorite,
0.05 to 0.1 portion of pasting agent,
the pigment is a plurality of pigments,
a plurality of deionized water;
the starch is firstly prepared into a starch aqueous solution by using deionized water, and the mass ratio of the starch to the deionized water in the starch aqueous solution is 1:10 to 20;
the polyvinyl alcohol is firstly prepared into a polyvinyl alcohol aqueous solution by using deionized water, and the mass ratio of the polyvinyl alcohol to the deionized water in the polyvinyl alcohol aqueous solution is 1:10 to 20; the mass ratio of the starch aqueous solution to the polyvinyl alcohol aqueous solution is 1:1 to 10; the pigment accounts for 5 to 10 percent of the weight of the starch water solution and the polyvinyl alcohol water solution;
the pasting agent is hydroxide or carbonate of alkali metal and alkaline earth metal;
the preparation method of the flame-retardant water-based gravure printing ink comprises the following steps:
1) Mixing 1 weight part of starch and 10 to 20 weight parts of deionized water, stirring uniformly, slowly heating to 60 ℃, keeping the temperature and stirring, adding 0.15 to 0.25 weight part of sodium hypochlorite aqueous solution containing sodium hypochlorite while stirring, continuing to keep the temperature and stirring, adding 0.15 to 0.75 weight part of hexafluoropropylene dimer and 0.001 to 0.01 weight part of nickel sulfate, continuing to keep the temperature and stirring, adding 0.05 to 0.1 weight part of alkali metal and alkaline earth metal hydroxides or carbonates aqueous solution, keeping the temperature and stirring to obtain uniform and transparent light yellow colloid;
2) In addition, slowly mixing 1-10 parts by weight of polyvinyl alcohol and 10-20 parts by weight of deionized water in a container, and stirring at 60 ℃ until the polyvinyl alcohol is completely dispersed and dissolved to prepare a polyvinyl alcohol aqueous solution;
3) And (3) mixing the light yellow colloid obtained in the step 1) and the polyvinyl alcohol obtained in the step 2), adding the pigment after uniformly stirring, and uniformly stirring to obtain the flame-retardant water-based gravure ink.
2. The flame-retardant water-based gravure printing ink as claimed in claim 1, wherein said polyvinyl alcohol type is one or two of PVA2099, PVA1799, PVA2088 and PVA 1788.
3. A fire retardant aqueous gravure printing ink according to claim 1, wherein said starch is one or a mixture of any two or three of wheat starch, corn starch and potato starch; the starch is white powder without peculiar smell, the protein content is less than or equal to 0.5 percent, and the solid content is more than or equal to 96 percent; the ash content is less than or equal to 0.1 percent, and the fineness is 90 to 110 meshes.
4. A fire-retardant aqueous intaglio printing ink according to claim 1 characterized in that said pigment is selected from one of carbon black, titanium dioxide and phthalocyanine blue.
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