CN115974090B - Preparation method of silicon dioxide for weak solvent ink-jet printing coating - Google Patents
Preparation method of silicon dioxide for weak solvent ink-jet printing coating Download PDFInfo
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Abstract
The invention belongs to the technical field of paint, and particularly relates to a preparation method of silicon dioxide for a weak solvent ink-jet printing coating, which comprises the following steps: s1, preparing a water glass solution, adding silicon dioxide as seed crystals, and adding sulfuric acid to form silica sol; s2, aging and stirring the silica sol, then boosting and heating the reaction system, regulating the pH value to be alkaline, keeping the pH value and the temperature, simultaneously adding the rest water glass and sulfuric acid, then adding an amino silane coupling agent to carry out surface modification, regulating the pH value to be acidic after aging, and then aging to form silica gel; s3, washing the gel sequentially by pure water, ammonium salt aqueous solution and pure water, and then dispersing and emulsifying; s4, drying the dispersed slurry, and then crushing to obtain the final product. The silica particles for the ink-absorbing printing coating are uniform and fine, have good dispersibility and filterability, and can obviously improve the performances of weather resistance, color vividness and the like of the printing coating.
Description
Technical Field
The invention belongs to the technical field of new material application, and particularly relates to a preparation method of silicon dioxide for a weak solvent ink-jet printing coating.
Background
Along with the improvement of the living standard of people, the color preservation demands of people are continuously improved, and digital cameras and ink-jet printers gradually become common tools for people to preserve colors, and the ink-jet printing paper gradually replaces the common paper and advances into the field of vision of people. The inks can be printed on a wide variety of substrates, with relatively large amounts being used in the field of industrial printing and packaging printing. Ink is one of the more critical factors affecting print quality. The weak solvent ink is a novel ink developed on the basis of the aqueous ink and the solvent ink, combines the dual advantages of the aqueous ink and the solvent ink, has the advantages of high printing precision, bright color, UV resistance, aging resistance and the like, and the solvent mainly contains components such as esters, alcohols and the like, and has the advantages of small smell, high volatilization point and the like.
The weak solvent ink is mainly acrylic emulsion, wherein the emulsion is mainly formed by copolymerizing acrylic ester, methacrylic ester or other vinyl monomers. The polyacrylate emulsion has the characteristics of strong adhesive force, smooth coating film, strong light retention and film forming capability, bright and plump coating film and the like, most of ink for inkjet has lower viscosity and lower surface tension, so that the high-viscosity polyacrylate emulsion has high requirements on the pore volume and the absorption performance of a substrate coating layer, while the silicon dioxide has the characteristics of large specific surface area, large pore volume and pore diameter, stable thermodynamics and the like.
Chinese patent CN109403138A discloses a method for producing a highly dispersed silica ink-absorbing agent for color spray paper, which comprises adding a certain amount of surfactant at a certain concentration, keeping at a certain temperature, adding a certain amount of inorganic acid, heating to 40-70 ℃, and adjusting a certain pH; heating to 85-95 ℃, reacting for a certain time, adding inorganic acid, regulating the pH value of the slurry to 3.0-4.0, aging for 30-60 min, adding organic acid to regulate the pH value to 2.0-4.0, and jet milling to obtain the silica with the particle size of 7.0 mu m, the whiteness of 98 ppm, the Fe content of 35ppm, the mass percent of 99.4% and the specific surface area of 350m 2 And/g, the pore volume is 1.98mL/g, and the pore size is 21.9 nm. The silica synthesized by the method has overlarge pore volume, can cause certain ink permeation when being applied in a weak solvent system, and whether the product of the scheme can be applied to color jet printing paper is not described in detail.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a preparation method of silicon dioxide for a weak solvent ink-jet printing coating, and the prepared silicon dioxide ink-absorbing particles are uniform and easy to disperse, have good filterability and dispersibility in a weak solvent system, and have bright color of drawing paper printed by ink-jet printing, so that the silicon dioxide ink-jet printing coating has been successfully applied to the field of ink-jet printing.
The invention aims at providing a preparation method of silica for a weak solvent ink-jet printing coating.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
a preparation method of silica for weak solvent ink-jet printing coating comprises the following steps:
s1, preparing a water glass solution, adding silicon dioxide as seed crystals, and adding sulfuric acid to form silica sol;
s2, aging and stirring the silica sol obtained in the step S1, boosting and heating a reaction system, adjusting the pH value to be alkaline, keeping the pH value and the temperature, simultaneously adding the rest water glass and sulfuric acid, then adding an amino silane coupling agent for surface modification, adjusting the pH value to be acidic after the aging is completed, and aging to form silica gel;
s3, washing the silica gel obtained in the step S2 by pure water, an ammonium salt aqueous solution and pure water in sequence, and then dispersing and emulsifying;
s4, drying the slurry after the dispersion in the step S3, and then crushing to obtain the modified starch.
Preferably, the water glass solution in the step S1 has a water glass modulus of 3.00-3.50, a silicon dioxide concentration of 20wt% to 30wt%, a sodium oxide concentration of 0.15-0.19mol/L and a sulfuric acid concentration of 10wt% to 30wt%.
Preferably, the silica seed crystal in the step S1 has a particle diameter of 6.0 μm to 8.0 μm and a porosity of 1.50cm 3 /g~1.65cm 3 Per gram, bulk density of 0.20g/cm 3 ~0.26g/cm 3 The conductivity is 50 us/cm-100 us/cm, and the silicon dioxide for ink-absorbing printing can be selected from the commercially available silicon dioxide, and the addition amount is total silicon dioxide (the sum of the silicon dioxide amount and the seed crystal silicon dioxide amount in the water glass solution)The content is 0.10-0.50 wt%.
Preferably, the pressure after the step S2 is increased is kept at 1-2 mpa, and the heating temperature is kept at 120-150 ℃.
Preferably, the amino silane coupling agent in the step S2 is one of KH520 (γ -aminopropyl methyldiethoxysilane), KH530 (γ -aminopropyl methyldimethoxysilane), KH540 (γ -aminopropyl trimethoxysilane), KH550 (γ -aminopropyl triethoxysilane), KH792 (N- (β -aminoethyl) - γ -aminopropyl trimethylethoxysilane), KH602 (N- β - (aminoethyl) - γ -aminopropyl methyldimethoxysilane).
Preferably, the addition amount of the silane coupling agent in the step S2 is 0.10-0.50 wt% of the total silicon dioxide content.
Preferably, in step S2, the pH is adjusted to be alkaline to a value of 10.0-11.0, and the pH is adjusted to be acidic to a value of 3.0-5.0.
Preferably, the washing in step S3 means that pure water, an ammonium salt aqueous solution and pure water are respectively used, and the time intervals of the washing sequence are respectively 1:2:3 washing until the conductivity of the silica gel is below 100us/cm; wherein the conductivity of the pure water is lower than 5us/cm, the temperature is 40-70 ℃, the ammonium salt is one of ammonium sulfate, ammonium bisulfate, ammonium carbonate and ammonium bicarbonate, and the concentration of the ammonium salt aqueous solution is 0.10-0.50wt%.
Preferably, in the step S3, the dispersion rotation degree is 1500-2500 rpm, the emulsification rotation degree is 2000-3000 rpm, and the combined action time is 30-60 minutes.
The second object of the present invention is to provide a silica for a weak solvent inkjet printing coating prepared by the above method.
Preferably, the particle size of the synthesized silicon dioxide is 6.0-8.0 mu m, the oil absorption value is 2.40-2.60 g/g, and the porosity is 1.70-1.85 cm 3 Per gram, bulk density of 0.25 to 0.27g/cm 3 The conductivity is less than 100us/cm.
The invention also provides application of the silicon dioxide in preparing a weak solvent ink-jet printing coating.
The silica particles synthesized by the method are uniform and fine, so that the silica for the ink-jet printing coating has good dispersibility and filterability, and the performances of weather resistance of the printing coating, color enrichment of ink-absorbing printing paper and the like are improved.
Compared with the prior art, the invention has the beneficial effects that:
(1) The silicon dioxide for ink-absorbing printing is used as seed crystal, the grain diameter is 6.0 mu m-8.0 mu m, and the porosity is 1.60cm 3 /g~1.65cm 3 Per gram, bulk density of 0.20g/cm 3 ~0.26g/cm 3 The conductivity is 50 us/cm-100 us/cm, the particle size, the porosity, the bulk density and the conductivity of the seed crystal are strictly required, and the stable growth of the seed crystal can be ensured, so that the growth stability of the silicon dioxide particles is ensured.
(2) The preparation method is carried out under the conditions of the pressure of 1 mpa-2 mpa, the temperature of 120 ℃ to 150 ℃ and the pH of 10.0 to 11.0, the reaction of the amino silane coupling agent and the silicon dioxide can be ensured to be complete by the high temperature, the high pressure and the high pH, the stability of the generated silicon dioxide product is high, and the silicon dioxide product is easier to disperse in the silicon dioxide ink-absorbing printing coating.
(3) The silica sol containing silica particles is treated by the amino silane coupling agent, wherein the silane coupling agent can improve the affinity degree of the silica particles and the organic polymer, improve the stability and the dispersibility of the silica in the ink-absorbing printing coating, improve the weather resistance of the printing coating, enrich the color and other performances of the ink-absorbing printing paper.
(4) The pure water washing can reduce the sulfate ion concentration of the synthetic silicon dioxide, and the ammonium salt aqueous solution is used for washing to promote the exchange of ammonium ions and sodium ions, so that the washing efficiency is improved, the washing dosage is saved, and the silicon dioxide particles can be reamed to a certain extent. The combination of the two can accelerate the uniform growth of the silicon dioxide particles to a certain extent.
Detailed Description
The technical solutions of the present invention will be clearly and completely described below in conjunction with examples of the present invention and comparative examples, and it is apparent that the described examples are only some of the examples of the present invention, but not all of the examples. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The test methods used in the following examples are conventional methods unless otherwise specified; the materials, reagents and the like used, unless otherwise specified, are those commercially available.
Example 1
At a temperature of 60 ℃, 5m of the pressure is added 3 2000L of pure water and water glass with the silica concentration of 30wt% are added into a stirring reaction kettle to prepare a silica solution with the sodium oxide concentration of 0.15mol/L, the commercial ink-absorbing printing silica with the silica content of 0.50wt% is added, stirring is carried out at full speed for 10 minutes, then a sulfuric acid solution with the concentration of 10wt% is added into the reaction kettle until the pH value is 9.0, the adding time is 20 minutes, stirring is stopped after the pH value is reached, silica sol is formed after 10 minutes, aging is carried out at the temperature of 60 ℃ for 10 minutes, the silica sol is dispersed for 30 minutes by full speed stirring, a small amount of water glass is added into the reaction kettle to adjust the pH value to 10.0 after full speed dispersion is completed, the water glass with the flow rate of 800L/h is added for 60 minutes, the sulfuric acid solution with the concentration of 10wt% is added into the reaction kettle, and the pH value of the reaction kettle is kept to be 10.0. After the water glass is added, adding a silane coupling agent KH520 (gamma-aminopropyl methyl diethoxy silane) with the silicon dioxide content of 0.50wt%, raising the pressure of a reaction kettle to 2Mpa, raising the temperature to 120 ℃, reacting and aging for 90 minutes under the condition of the pH value, reducing the pressure of the reaction kettle to normal pressure after the aging is finished, adding pure water to reduce the temperature to 90 ℃, adding sulfuric acid to adjust the pH value to 3.0 under the condition of the temperature for aging for 60 minutes, pumping into a filter press plate frame for water washing after the aging is finished, and adding pure water at 50 ℃): ammonium salt solution with concentration of 0.10 wt%: the pure water washing sequence time intervals at 50℃were 1:2:3 washing the filter cake for 5 hours, washing until the conductivity is below 100us/cm, dispersing the emulsified feed liquid for 60 minutes by using a dispersing machine and an emulsifying machine after washing, wherein the rotating speed of the dispersing machine is 2500 rpm, the rotating speed of the emulsifying agent is 2000 rpm, and spray drying the slurry obtained after dispersingAnd (3) carrying out jet milling to obtain the silicon dioxide product for ink-absorbing printing.
The physical and chemical property test method and standard of the product are as follows:
(1) Porosity test: full-automatic specific surface area and porosity analyzer microphone: triStar II 3020;
(2) Average particle diameter: laser particle size analyzer: markov 3000;
(3) Oil absorption value: manual picking method: 1g of silica absorbs dibutyl phthalate; reference is made to the row label HG/T3072-2019;
(4) Conductivity test: lei Ci DDS-11A;
(5) Bulk density testing: bulk density refers to the density obtained by dividing the mass of powder by the volume V of the container in which the powder is present, also known as bulk density.
The physicochemical properties of the seven parallel products are shown in Table 1.
Example 2
At a temperature of 40 ℃, 5m of the pressure is applied 3 Adding 1000L of pure water and water glass with the silica concentration of 30wt% into a stirring reaction kettle to prepare a silica solution with the sodium oxide concentration of 0.18mol/L, adding the commercial ink-absorbing printing silica with the silica content of 0.10wt%, stirring at full speed for 10 minutes, adding a sulfuric acid solution with the concentration of 30wt% into the reaction kettle until the pH value is 8.0, adding for 10 minutes, stopping stirring after the pH value is reached, forming silica sol after 20 minutes, aging for 30 minutes at the temperature of 40 ℃ after the formation of the silica sol, stirring at full speed for dispersing the silica sol for 10 minutes, adding a small amount of water glass to adjust the pH value to 11.0 after full speed dispersion is completed, adding water glass with the flow rate of 600L/h into the reaction kettle for 60 minutes, adding the sulfuric acid solution with the concentration of 30wt% into the reaction kettle while adding the water glass, and keeping the pH value of the reaction kettle to be 11.0. After the water glass is added, adding a silane coupling agent KH530 (gamma-aminopropyl methyl dimethoxy silane) with the silicon dioxide content of 0.10 weight percent, and raising the pressure of the reaction kettle to 1Mpa,Heating to 150 ℃, reacting and aging for 120 minutes under the pH condition, reducing the pressure of a reaction kettle to normal pressure after aging, adding pure water to reduce the temperature to 70 ℃, adding sulfuric acid to adjust the pH to 5.0 under the temperature condition, aging for 30 minutes, pumping into a filter press plate frame for water washing after aging, and adding pure water at 70 ℃): ammonium salt solution with concentration of 0.5 wt%: washing filter cakes by pure water at the temperature of 70 ℃ at the time interval of 1:2:3 respectively, and washing by water for 4 hours until the conductivity is below 100us/cm; after the washing is finished, dispersing the emulsified feed liquid for 30 minutes by using a dispersing machine and an emulsifying machine, wherein the rotating speed of the dispersing machine is 2500 rpm, the rotating speed of the emulsifying agent is 3000 rpm, and the obtained slurry after the dispersing is subjected to spray drying and jet milling to obtain the silicon dioxide product for ink-absorbing printing.
The physical and chemical properties of the product are shown in Table 2, and the physical and chemical properties of seven parallel products are the same as those of example 1.
Example 3
At a temperature of 50 ℃, 5m of the pressure is applied 3 Adding 1500L of pure water and water glass with the silica concentration of 25wt% into a stirring reaction kettle to prepare a silica solution with the sodium oxide concentration of 0.16mol/L, adding the commercial ink-absorbing printing silica with the silica content of 0.20wt%, stirring at full speed for 15 minutes, adding a sulfuric acid solution with the concentration of 25wt% into the reaction kettle until the pH value is 8.5, adding for 15 minutes, stopping stirring after the pH value is reached, forming silica sol after 15 minutes, aging at 50 ℃ for 25 minutes, stirring at full speed for dispersing the silica sol for 20 minutes, adding a small amount of water glass to adjust the pH value to 10.0 after full speed dispersion is completed, adding water glass with the flow rate of 700L/h into the reaction kettle for 60 minutes, adding the sulfuric acid solution with the concentration of 25wt% into the reaction kettle while adding the water glass, and keeping the pH value of the reaction kettle to be 10.0. After the water glass is added, adding a silane coupling agent KH540 (gamma-aminopropyl trimethoxysilane) with the silicon dioxide content of 0.20wt%, and raising the pressure of the reaction kettle to 1.5Mpa and the temperature to 130 ℃, whereinAnd (3) reacting and aging for 100 minutes under the condition of pH, after the aging is finished, reducing the pressure of the reaction kettle to normal pressure, adding pure water to reduce the temperature to 80 ℃, adding sulfuric acid to adjust the pH to 4.0 under the condition of the temperature, aging for 40 minutes, pumping into a filter press plate frame for washing after the aging is finished, and adding pure water at 40 ℃ into the filter press plate frame: ammonium salt solution with a concentration of 0.2 wt.%: the pure water washing sequence time intervals at 40 ℃ are respectively 1:2:3 washing the filter cake, wherein the washing time is 4.5 hours, and the washing time is up to the conductivity of 100us/cm or less; after washing, dispersing the emulsified feed liquid for 40 minutes by using a dispersing machine and an emulsifying machine, wherein the rotating speed of the dispersing machine is 1500 rpm, the rotating speed of the emulsifying agent is 2000 rpm, and the obtained slurry after dispersing is subjected to spray drying and jet milling to obtain the silicon dioxide product for ink-absorbing printing.
The physical and chemical properties of the product were measured in the same manner as in example 1, and the physical and chemical properties of seven parallel products are shown in Table 3.
Example 4
At a temperature of 50 ℃, 5m of the pressure is applied 3 1800L of pure water and water glass with the silica concentration of 28wt% are added into a stirring reaction kettle to prepare a silica solution with the sodium oxide concentration of 0.17mol/L, the commercial ink-absorbing printing silica with the silica content of 0.30wt% is added, full-speed stirring is carried out for 20 minutes, the sulfuric acid solution with the concentration of 28wt% is added into the reaction kettle until the pH value is 8.0, the adding time is 20 minutes, stirring is stopped after the pH value is reached, silica sol is formed after 20 minutes, the silica sol is formed, aging is carried out for 30 minutes at the temperature of 50 ℃, full-speed stirring is carried out for dispersing the silica sol for 30 minutes, a small amount of water glass is added after full-speed dispersion is finished to adjust the pH value to 10.5, the water glass with the flow rate of 750L/h is added into the reaction kettle for 60 minutes, the sulfuric acid solution with the concentration of 28wt% is added into the reaction kettle, and the pH value of the reaction kettle is kept to be 10.5. After the water glass is added, adding a silane coupling agent KH550 (gamma-aminopropyl triethoxysilane) with the silicon dioxide content of 0.30 weight percent, and raising the pressure of the reaction kettle to 2Mpa and the temperature to 140 ℃, and reacting for the long time under the pH conditionAfter the aging is completed, the pressure of the reaction kettle is reduced to normal pressure, pure water is added to reduce the temperature to 75 ℃, sulfuric acid is added to adjust the pH value to 4.5 under the temperature condition for aging for 45 minutes, and after the aging is completed, the reaction kettle is pumped into a filter press plate frame for water washing, and pure water at 60 ℃ is added: ammonium salt solution with a concentration of 0.3 wt.%: washing filter cakes by pure water at 60 ℃ at a sequence time interval of 1:2:3 respectively, and washing for 5 hours until the conductivity is below 100us/cm; after the washing is finished, dispersing the emulsified feed liquid for 60 minutes by using a dispersing machine and an emulsifying machine, wherein the rotating speed of the dispersing machine is 1500 rpm, the rotating speed of the emulsifying agent is 2000 rpm, and the obtained slurry after the dispersing is finished is subjected to spray drying and jet milling to obtain the silicon dioxide product for ink-absorbing printing.
The physical and chemical properties of the product were measured in the same manner as in example 1, and the physical and chemical properties of seven parallel products are shown in Table 4.
Example 5
At 55 deg.C, 5m of the pressure is applied 3 Stirring the reaction kettle, adding 1900L of pure water and water glass with the silica concentration of 30wt% to prepare a silica solution with the sodium oxide concentration of 0.16mol/L, adding the commercially available silica for ink-absorbing printing with the silica content of 0.40wt%, stirring at full speed for 20 minutes, adding a sulfuric acid solution with the concentration of 25wt% to the reaction kettle until the pH value is 8.5, adding for 15 minutes, stopping stirring after the pH value reaches, forming silica sol after 15 minutes, aging for 20 minutes at the temperature of 55 ℃ after forming the silica sol, stirring at full speed for dispersing the silica sol for 20 minutes, adding a small amount of water glass to adjust the pH value to 10.0 after full speed dispersion is completed, adding water glass with the flow rate of 700L/h to the reaction kettle for 60 minutes, adding the sulfuric acid solution with the concentration of 25wt% to the reaction kettle while adding the water glass, and keeping the pH value of the reaction kettle to be 10.0. After the water glass is added, adding a silane coupling agent KH792 (N- (beta-aminoethyl) -gamma-aminopropyl trimethyl (ethoxysilane) with the silicon dioxide content of 0.40wt percent, and raising the pressure of the reaction kettle to 1.8Mpa and the temperature to 150 ℃, and reacting under the pH conditionAging for 120 minutes, after aging, reducing the pressure of the reaction kettle to normal pressure, adding pure water to reduce the temperature to 80 ℃, adding sulfuric acid to adjust the pH value to 5.0 under the temperature condition, aging for 60 minutes, pumping into a filter press plate frame for water washing after aging, and adding pure water at 70 ℃: ammonium salt solution with a concentration of 0.4 wt.%: washing filter cakes by pure water at the temperature of 70 ℃ at the time interval of 1:2:3 respectively, and washing by water for 4.5 hours until the conductivity is below 100us/cm; after the washing is finished, dispersing the emulsified feed liquid for 30 minutes by using a dispersing machine and an emulsifying machine, wherein the rotating speed of the dispersing machine is 2500 rpm, the rotating speed of the emulsifying agent is 3000 rpm, and the obtained slurry after the dispersing is subjected to spray drying and jet milling to obtain the silicon dioxide product for ink-absorbing printing.
The physical and chemical properties of the product were measured in the same manner as in example 1, and the physical and chemical properties of seven parallel products are shown in Table 5.
Example 6
At a temperature of 50 ℃, 5m of the pressure is applied 3 1300L of pure water and water glass with the silica concentration of 25wt% are added into a stirring reaction kettle to prepare a silica solution with the sodium oxide concentration of 0.19mol/L, the commercial ink-absorbing printing silica with the silica content of 0.50wt% is added, stirring is carried out at full speed for 15 minutes, then a sulfuric acid solution with the concentration of 27wt% is added into the reaction kettle until the pH value is 8.8, the adding time is 20 minutes, stirring is stopped after the pH value is reached, a silica sol is formed after 18 minutes, aging is carried out at the temperature of 50 ℃ for 25 minutes, the silica sol is dispersed at full speed for 25 minutes, a small amount of water glass is added to adjust the pH value to 10.8 after full-speed dispersion is completed, water glass with the flow rate of 750L/h is added into the reaction kettle for 60 minutes, the sulfuric acid solution with the concentration of 27wt% is added into the reaction kettle, and the pH value of the reaction kettle is kept to be 10.8. After the water glass is added, adding a silane coupling agent KH602 (N-beta- (aminoethyl) -gamma-aminopropyl methyl dimethoxy silane) with the silicon dioxide content of 0.50 weight percent, and raising the pressure of the reaction kettle to 2.0Mpa and the temperature to 140 ℃, under the pH conditionAging for 110 minutes, after aging, reducing the pressure of the reaction kettle to normal pressure, adding pure water to reduce the temperature to 75 ℃, adding sulfuric acid to adjust the pH value to 4.5 under the temperature condition, aging for 40 minutes, pumping into a filter press plate frame for water washing after aging, and adding pure water at 60 ℃: ammonium salt solution with concentration of 0.5 wt%: washing filter cakes by pure water at 60 ℃ at a sequence time interval of 1:2:3 respectively, and washing by water for 4 hours until the conductivity is below 100us/cm; after washing, dispersing the emulsified feed liquid for 25 minutes by using a dispersing machine and an emulsifying machine, wherein the rotating speed of the dispersing machine is 2000 rpm, the rotating speed of the emulsifying agent is 2500 rpm, and the obtained slurry after dispersing is subjected to spray drying and jet milling to obtain the silicon dioxide product for ink-absorbing printing.
The physical and chemical properties of the product were measured in the same manner as in example 1, and the physical and chemical properties of seven parallel products are shown in Table 6.
Comparative example 1
The difference from example 1 is that the commercial silica for ink-jet printing having a silica content of 0.50wt% was not added as a seed crystal, and the other operations were the same as in example 1.
The physical and chemical properties of the product were measured in the same manner as in example 1, and the physical and chemical properties of seven parallel products are shown in Table 7.
Comparative example 2
The difference from example 1 is that the commercial ink-jet printing silica having a silica content of 0.50wt% is not added as a seed crystal, but a silica having a particle diameter of 6.0 to 8.0 μm and a porosity of 1.70 to 1.85cm is added 3 Per gram, bulk density of 0.15 to 0.19g/cm 3 Silica having a conductivity of 50 to 100us/cm was used in the same manner as in example 1.
The physical and chemical properties of the product were measured in the same manner as in example 1, and the physical and chemical properties of seven parallel products are shown in Table 8.
Comparative example 3
The difference from example 1 was that the reaction vessel was not subjected to the pressure boosting operation, the temperature of the aqueous phase reaction was raised to 100℃at the maximum, and the reaction vessel was kept at this reaction condition and aged for 90 minutes, and the other operations were the same as in example 1.
The physical and chemical properties of the product were measured in the same manner as in example 1, and the physical and chemical properties of seven parallel products are shown in Table 9.
Comparative example 4
The difference compared to example 1 is that pure water at 50℃in example 1 was replaced with pure water at 50): ammonium salt solution with concentration of 0.10 wt%: the filter cake was washed with pure water at 50℃at a sequential time interval of 1:2:3, respectively, with the water washing time unchanged, and the other operations were the same as in example 1.
The physical and chemical properties of the product were measured in the same manner as in example 1, and the physical and chemical properties of seven parallel products are shown in Table 10.
Comparative example 5
The procedure was the same as in example 1 except that the amino silane coupling agent such as silane coupling agent KH520 (gamma-aminopropyl methyldiethoxysilane) having a silica content of 0.50wt% was not added.
The physical and chemical properties of the product were measured in the same manner as in example 1, and the physical and chemical properties of seven parallel products are shown in Table 11.
Comparative example 6
The procedure was the same as in example 1 except that instead of the amino silane coupling agent such as KH520 (γ -aminopropyl trimethoxysilane), a silane coupling agent KH580 (3-mercaptopropyl trimethoxysilane) having a silica content of 0.50wt% was added.
The physical and chemical properties of the product were measured in the same manner as in example 1, and the physical and chemical properties of seven parallel products are shown in Table 12.
Application Performance test
The three silica ink-receptive printing silica example products 1-3, 3-3, 5-3 and comparative examples 1-3, 4-3 prepared by the invention are compared with Grace P508 and domestic space SD640 in weak solvent ink-receptive printing acrylic acid system, pure water is used for: silica for ink-jet printing: PVA (polyvinyl alcohol 2688, petrochemical general works, shandong texas): butyl acrylate emulsion (Tianjin metallocene chemical reagent Co.): according to the following steps: 12:3.2:18.8 application testing was performed as follows:
1. water intake and ink-absorbing printing silica according to 66 parts: preparing a silica suspension according to a proportion of 12 parts;
2. filtering the silicon dioxide suspension liquid through a 2-layer 500-mesh filter screen;
3. adding 3.2 parts of PVA into the filtered filtrate, and stirring for 15 minutes by a dispersing machine of 1000 r/min;
4. after the PVA colloid is added and dispersed, 18.8 parts of butyl acrylate emulsion is added, and the viscosity is tested;
5. after the viscosity is qualified, uniformly rolling the butyl acrylate emulsion on RC coated photographic paper, and drying the RC coated photographic paper at 90 ℃ by using a constant-temperature drying oven;
6. after 10 minutes of drying, printing is performed by using an epson L810 printer, and color differences, physicochemical indexes and application test result data are compared as shown in table 13.
The application test method comprises the following steps:
(1) Rotational viscometer test: a rotational viscometer NDJ-5S;
(2) K value tester: the Kenicamantadine Konica Minolta FD-5 spectrodensitometer has K value and camera index, wherein the K value (K value is quantitatively expressed by Kelvin temperature (K)) is the color temperature, the higher the K value is, the more the developed color tends to be white and blue, the lower the K value is, the more the developed color tends to be yellow and red, the K value is a color judgment standard, the pursuit of the color is carried out by ink-absorption printing, and the pursuit of the K value is higher or close to foreign products in industry;
(3) The weather resistance is irradiated by sunlight and blown by wind, and the condition that the printing paper changes is observed;
(4) Other application testing: observing color and whether ink seeps through eyes;
as can be seen from the materialized detection data of the 6 embodiments, the physical indexes of the products produced according to the technical scheme of the invention are basically close, which indicates that the technical scheme has stable production. And compared with the product in the example 1 and the comparative example 2, the oil absorption value and the porosity of the product are obviously reduced, the bulk density is obviously increased, and the particle size stability of the product is not high without adding seed crystals with the particle size, the porosity, the bulk density and the conductivity meeting the requirements. The specific particle size, the porosity, the bulk density and the conductivity of the crystal seeds (such as the silicon dioxide for the commercial ink-absorbing printing) are used for accelerating the formation of a silicon dioxide structure and the improvement of the porosity, so that the oil absorption value, the porosity and the bulk density of the product are improved and reduced. The application viscosity in weak solvent inkjet printing is low, bleeding appears in the coating, and the K value is low.
Compared with the embodiment 1, the comparative example 3 does not raise the pressure of the reaction kettle to a certain pressure, the temperature of the aqueous phase reaction is raised to the maximum 100 ℃, the oil absorption value and the porosity of the product are obviously reduced, and the bulk density is obviously increased, because the reaction of silica particles and amino silane coupling agents can be promoted under the conditions of a certain pressure and a high temperature, the formation of a silica network structure is accelerated, the porosity and the oil absorption value of the formed silica are higher, the bulk density is lighter, the structure of the silica is more stable, and the application gap in weak solvent ink-jet printing is mainly reflected in the aspects of viscosity, weather resistance, ink permeability and color vividness of printing paper.
The comparative example 4 directly adopts ordinary pure water to replace pure water, ammonium bicarbonate solution and two liquid water washing silica gels, the oil absorption value and the porosity of the product are obviously reduced, the bulk density and the conductivity are obviously increased, and the main reason is that ammonium ions can exchange ions with hydrogen ions, so that the porosity of the silica is richer and larger, the ammonium bicarbonate is reamed, and the exchange of the ammonium ions and the hydrogen ions can improve the water washing efficiency to a certain extent. The application properties are not much inferior to comparative example 3.
The comparative example 5 directly does not add a silane coupling agent for synthesis reaction, the oil absorption value and the porosity of the product are slightly reduced, the bulk density is slightly increased, and the amino silane coupling agent can improve the affinity degree of silica particles and organic polymers and the dispersibility of the silica particles, so that the structure of the silica is more stable, various indexes of the product can be stabilized, and the stability and the dispersibility of the silica in ink-absorbing printing coatings are improved. The application gap in weak solvent ink jet printing is mainly reflected in the aspects of weather resistance, ink permeability and color vividness of printing paper.
In comparative example 6, a silane coupling agent KH580 (3-mercaptopropyl trimethoxy silane) is added to replace an amino silane coupling agent, so that the oil absorption value, the porosity, the bulk density and the particle size fluctuation of a synthetic silicon dioxide product are relatively large, and the product is extremely unstable. Therefore, the technical effect of the invention can be achieved only by the cooperative matching of all the conditions.
From three samples of examples 1-3, 3-3 and 5-3, and four samples of silicon dioxide for ink-absorbing printing of comparative examples 1-3, 3-3, 4-3 and 5-3, compared with Grace P508 and domestic space SD640 silicon dioxide products for ink-absorbing printing, the silicon dioxide for ink-absorbing printing synthesized by the method disclosed by the invention has close physical and chemical indexes and application properties to foreign Grace P508 products, has good dispersibility and filterability, and the printing paper has strong weather resistance, the K value in the color of the drawing paper is close to foreign products, the color vividness is better, and the application properties of the silicon dioxide for ink-absorbing printing synthesized by the examples are obviously better than those of the comparative examples, the commercial silicon dioxide for ink-absorbing printing and the domestic space SD640 products.
It is apparent that the above examples of the present invention are only for clearly illustrating the technical solution of the present invention, and are not limited to the specific embodiments of the present invention. Any modification, equivalent replacement, improvement, etc. that comes within the spirit and principle of the claims of the present invention should be included in the protection scope of the claims of the present invention.
Claims (5)
1. The application of the silicon dioxide in the preparation of the weak solvent ink-jet printing coating for improving the weather resistance and the color degree of the printing coating and reducing the ink permeation performance is characterized in that the silicon dioxide has the particle size of 6.0-8.0 mu m, the oil absorption value of 2.40-2.60 g/g and the porosity of 1.70cm 3 /g~1.85cm 3 Per gram, bulk density of 0.25g/cm 3 ~0.27g/cm 3 Conductivity less than 100us/cm;
the silicon dioxide is prepared by the following steps:
s1, preparing a water glass solution, adding silicon dioxide as seed crystals, and adding sulfuric acid to form silica sol;
s2, aging and stirring the silica sol obtained in the step S1, boosting and heating a reaction system, adjusting the pH value to be alkaline, keeping the pH value and the temperature, simultaneously adding the rest water glass and sulfuric acid, then adding an amino silane coupling agent for surface modification, adjusting the pH value to be acidic after the aging is completed, and aging to form silica gel;
s3, washing the silica gel obtained in the step S2 by pure water, an ammonium salt aqueous solution and pure water in sequence, and then dispersing and emulsifying;
s4, drying the slurry after the dispersion in the step S3, and crushing to obtain the slurry;
the grain diameter of the silicon dioxide for the seed crystal is 6.0-8.0 mu m, and the porosity is 1.50cm 3 /g~1.65cm 3 Per gram, bulk density of 0.20g/cm 3 ~0.26g/cm 3 The conductivity is 50 to 100us/cm, and the addition amount is 0.10 to 0.50 percent of the total content of the silicon dioxide;
s2, the amino silane coupling agent is one of gamma-aminopropyl methyl diethoxy silane, gamma-aminopropyl methyl dimethoxy silane, gamma-aminopropyl trimethoxy silane, N- (beta-aminoethyl) -gamma-aminopropyl trimethyl (ethoxyl) silane and N-beta- (aminoethyl) -gamma-aminopropyl methyl dimethoxy silane; and step S2, the pressure is kept at 1-2 mpa after the pressure is increased, and the heating temperature is kept at 120-150 ℃.
2. The use according to claim 1, wherein the water glass solution in step S1 has a water glass modulus of 3.00-3.50, a silica concentration of 20 wt.% to 30wt%, a sodium oxide concentration of 0.15-0.19mol/L, and a sulfuric acid concentration of 10 wt.% to 30 wt.%.
3. The use according to claim 1, wherein the amino silane coupling agent in step S2 is added in an amount of 0.10wt% to 0.50wt% of the total silica content.
4. The use according to claim 1, wherein in step S2 the pH is adjusted to be alkaline to a value of 10.0 to 11.0 and the pH is adjusted to be acidic to a value of 3.0 to 5.0.
5. The use according to claim 1, wherein the washing in step S3 is performed with pure water, an aqueous ammonium salt solution, and pure water at a time interval of 1 in the washing sequence: 2:3 washing until the conductivity of the silica gel is below 100us/cm; wherein the conductivity of the pure water is lower than 5us/cm, the temperature is 40-70 ℃, the ammonium salt is one of ammonium sulfate, ammonium bisulfate, ammonium carbonate and ammonium bicarbonate, and the concentration of the ammonium salt aqueous solution is 0.10-0.50wt%.
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