CN108084802B - Ethanol-resistant aqueous glaze nano-grade color concentrate - Google Patents
Ethanol-resistant aqueous glaze nano-grade color concentrate Download PDFInfo
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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
- C09D17/00—Pigment pastes, e.g. for mixing in paints
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F293/00—Macromolecular compounds obtained by polymerisation on to a macromolecule having groups capable of inducing the formation of new polymer chains bound exclusively at one or both ends of the starting macromolecule
- C08F293/005—Macromolecular compounds obtained by polymerisation on to a macromolecule having groups capable of inducing the formation of new polymer chains bound exclusively at one or both ends of the starting macromolecule using free radical "living" or "controlled" polymerisation, e.g. using a complexing agent
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- 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
- C09D11/03—Printing inks characterised by features other than the chemical nature of the binder
- C09D11/037—Printing inks characterised by features other than the chemical nature of the binder characterised by the pigment
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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
- C09D17/00—Pigment pastes, e.g. for mixing in paints
- C09D17/003—Pigment pastes, e.g. for mixing in paints containing an organic pigment
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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
- C09D17/00—Pigment pastes, e.g. for mixing in paints
- C09D17/004—Pigment pastes, e.g. for mixing in paints containing an inorganic pigment
- C09D17/007—Metal oxide
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
- C08F2438/00—Living radical polymerisation
- C08F2438/03—Use of a di- or tri-thiocarbonylthio compound, e.g. di- or tri-thioester, di- or tri-thiocarbamate, or a xanthate as chain transfer agent, e.g . Reversible Addition Fragmentation chain Transfer [RAFT] or Macromolecular Design via Interchange of Xanthates [MADIX]
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Abstract
The invention relates to an ethanol-resistant water-based Grice nano-chromogen, which consists of 3-methoxy methyl propionate, ethanol, a surface treating agent, toner, a sulfonic acid type block copolymer dispersant, other auxiliary agents and water; the sulfonic acid type block copolymer dispersant is synthesized by maleic anhydride, vinyl monomer containing sodium sulfonate, RAFT reagent and azo initiator through RAFT technology; the Mn is 3000-10000, and PDI is less than 1.3; the ethanol-resistant water-based Grice nano-grade dye prepared by the invention has excellent tinting strength, transparency, compatibility, alcohol resistance, storage stability, alkali resistance, acid resistance, high temperature resistance of 300 ℃, sun resistance, stain resistance, migration resistance and ultraviolet resistance. The water-based UV paint is widely applied to the fields of woodware color wiping, water-based woodware paint, water-based automobile paint, water-based plastic paint, water-based industrial paint, water-based glass baking paint, water-based metal baking paint, water-based UV paint, water-based surface printing ink and the like.
Description
Technical Field
The invention relates to an aqueous glaze color concentrate, in particular to an ethanol-resistant aqueous glaze nano color concentrate, and belongs to the technical field of aqueous color pastes.
Background
Along with the improvement of the living standard of people's material culture, the requirement of consumers on the coating effect of furniture is higher and higher, thereby driving the rapid growth of the domestic woodware coating. The waterborne glaze of the wood lacquer is inevitable, the waterborne glaze comes along with the movement, most of the waterborne glaze used in the domestic furniture industry at present is waterborne or alcohol-soluble dye essence for wood grain color wiping and finish coloring, but the dye essence has the defects of serious standard exceeding of heavy metals, containing pathogenic substances, poor temperature resistance, sun resistance, stain resistance and migration resistance.
The metal oxide such as anba powder and transparent iron oxide has excellent weather resistance, light resistance, ultraviolet absorptivity, transparency, elegant color, no toxicity, excellent chemical stability, excellent alkali resistance, acid resistance, high temperature resistance of 300 ℃, no bleeding, migration resistance, and better color saturation and color intensity.
The ultraviolet ray is used for destroying the soul of the wood, and the Anba powder and the transparent iron oxide pigment can strongly absorb the ultraviolet radiation, so that the wood is protected, the wood can have a coloring effect, the wood can keep natural textures, and the color is soft; when the pigment is mixed with organic transparent pigment for use, the color of the pigment can be enriched, the chroma is improved, the defects of poor weather resistance and poor temperature resistance of the organic transparent pigment when the pigment is used alone can be obviously overcome, and the wood grain is clear and thorough when the pigment is used for coloring wooden furniture, so that the furniture is elegant, noble, simple and natural.
The wood color-wiping water-based color paste has less resin, keeps proper drying speed, has limitation on water, is unfavorable for wood due to too much water, and is generally added with ethanol to improve the volatilization speed, so the wood color paste has good alcohol resistance on water-based color essence.
The water-based anba powder or iron-permeable color paste is resin-free color paste, also called water-based glaze nano color concentrate, and can show the unique performance only by dispersing to the nano particle size. At present, pigment affinity group block copolymer dispersants such as EFKA-4560, EFKA-4540, BYK-180, BYK-183, BYK-185, Tego752W, HSM-3091 and the like are mostly adopted for dispersing, but the particle size is larger than 1 mu m, and the transparency is poor; easy precipitation and poor stability; poor compatibility and uneven coloring; the color concentrate prepared by the dispersant is diluted by 10 times by 95 percent ethanol and then is layered and precipitated, and the alcohol resistance is poor.
Disclosure of Invention
The invention aims to provide an ethanol-resistant aqueous glaze nano-grade color concentrate.
The invention adopts sulfonic acid anion synthesized by RAFT controlled technologyThe sub-block copolymer is used as a dispersant, the dispersant has an A-B block structure, carboxylate ions and sulfonate ions of an anchoring group of the dispersant are adsorbed on the surface of particles to form a double electric layer to generate electrostatic repulsion, polyacrylate chains do not mutually twine due to steric hindrance and stretch in an aqueous dispersion system, and due to the double effects of the electrostatic repulsion and the steric hindrance, the dispersant not only has high dispersion efficiency, good compatibility and high alcohol resistance, but also forms a stable suspension system; the dispersant contains a plurality of anchor groups completely connected with H on the surface of the particle+Ion combination, large adsorption capacity and good coating effect, and effectively prevents water molecules or ethanol-OH from permeating into the surface of the particles and H+Hydrogen bonds are formed, so that the water resistance and the alcohol resistance are improved, and the pigment is suitable for dispersing high-specific-surface-area pigments such as ambar powder and transparent iron oxide.
In order to improve the alcohol resistance and compatibility of the water-based glaze, the invention selects 3-Methoxy Methyl Propionate (MMP) as a cosolvent, and ether ester group, linear structure and propionyl group in the molecular center in the MMP enable the material to have some properties which are not possessed by other solvents: the dissolving power is strong, and difficult substances such as toner, color paste and the like can be well dispersed; low surface tension, high resistivity, and special function of preventing color paste from thickening and changing hue; the problems of sagging and hidden bubbles of the woodware coating in the high-gloss colored paint can be solved; the paint has light smell, is completely volatilized, has no residual smell on the surface of a paint film, and can improve the leveling property, the luster and the transparency of the paint film; but also has the effect of preventing sedimentation.
In order to solve the technical problems, the invention adopts the following technical scheme: the invention relates to an ethanol-resistant water-based glaze nano-grade color concentrate, which comprises the following components in percentage by weight: 5.0-10.0 percent of 3-methoxy methyl propionate, 20.0-50.0 percent of ethanol, 1.0-3.0 percent of surface treating agent, 20.0-30.0 percent of toner, 10.0-25.0 percent of sulfonic acid type anionic block copolymer dispersant, 0.1-0.5 percent of pH regulator, 0.1-0.5 percent of defoaming agent, 0.2-1.0 percent of anti-settling agent and the balance of deionized water.
Wherein the toner is one of transparent ferric oxide, translucent calcined umber powder and translucent raw umber powder.
The surface treating agent is one of silane coupling agent, zirconate coupling agent and titanate coupling agent.
The sulfonic acid type anionic block copolymer dispersant is synthesized by adopting RAFT technology, and the molecular structural formula is as follows:
m in the molecular formula is 5-20, n is 4-10; the sulfonic acid type block copolymer dispersant is an A-B block structure, the number average molecular weight of the sulfonic acid type block copolymer dispersant is 3000-10000, and the polydispersity number PDI is less than 1.3.
The sulfonic acid type anionic block copolymer dispersant is prepared by the following steps:
a) sequentially adding an organic solvent, a hydroxyl-containing acrylic monomer and cyclic alkyl sultone into a reaction kettle according to the weight ratio of the formula, starting stirring and dissolving uniformly, heating to 60-90 ℃ for reacting for 4-8 h, cooling to 40 ℃, adding methanol for dissolving, then adding acetone for precipitating, performing suction filtration on the precipitate, dissolving with methanol, precipitating with acetone, performing suction filtration, and repeating for 2-3 times to obtain a vinyl monomer I containing a sodium sulfonate group; wherein the molar ratio of the hydroxyl-containing acrylic monomer to the cyclic alkyl sultone is 1.3: 1-1: 1;
b) in N2Sequentially adding 10.0-20.0 parts by weight of maleic anhydride, 0.5-2.0 parts by weight of RAFT reagent and 40.0-60.0 parts by weight of alcohol solvent into a protected reaction kettle, stirring and dissolving, heating to 60-100 ℃, uniformly dropwise adding 8.0-15.0 parts by weight of alcohol solution containing 10% of initiator, keeping at 60-100 ℃ for continuous reaction for 2-3 hours after dropwise adding is finished within 0.5 hour; and then adding 5.0-20.0 parts of a vinyl monomer I containing a sodium sulfonate group, controlling the temperature at 60-100 ℃, continuing to react for 4-8 hours, cooling to 50 ℃, adding a neutralizing agent, stirring for 0.5 hour, and controlling the pH to be 7-9 to obtain the sulfonic acid type anionic block copolymer dispersing agent.
Wherein the acrylic monomer containing hydroxyl is at least one of hydroxyethyl methacrylate, hydroxyethyl acrylate, hydroxypropyl methacrylate, hydroxypropyl acrylate, hydroxybutyl methacrylate, hydroxybutyl acrylate, hydroxypentyl methacrylate, hydroxypentyl acrylate, hydroxyhexyl methacrylate and hydroxyhexyl acrylate.
The cyclic alkyl sultone is at least one of 1, 3-propane sultone, 1-methyl-1, 3-propane sultone, 2-methyl-1, 3-propane sultone, 3-methyl-1, 3-propane sultone, 1, 4-butane sultone, 1-methyl-1, 4-butane sultone, 2-methyl-1, 4-butane sultone, 3-methyl-1, 4-butane sultone and 4-methyl-1, 4-butane sultone.
The organic solvent is at least one of dimethyl sulfoxide, dimethylformamide, dimethylacetamide, acetone and butanone.
The RAFT reagent is anionic or cationic modified water-soluble dithioester or water-soluble trithioester; further, it is preferable that the quaternary ammonium salt is at least one of dithiophenylacetic acid, α -dithiophenylmethyl-p-tolylene pyridinium chloride, S '-bis (α, α' -dimethyl- α ″ -acetic acid) trithiocarbonate, and diethyldithiocarbamate.
The initiator is at least one of azodiisobutyronitrile, azodiisoheptonitrile, azodiisobutyronitrile dimethyl ester and azodiisobutyl amidine hydrochloride.
The alcohol solvent is at least one of methanol, ethanol, n-propanol and isopropanol.
The neutralizing agent is at least one of sodium hydroxide, potassium hydroxide and ammonia water.
The invention provides a preparation method of ethanol-resistant water-based Grice nano color concentrate, which comprises the following steps: according to the weight ratio of the formula, deionized water, ethanol, methyl 3-methoxypropionate and a surface treating agent are added into a dispersing barrel, toner is added after the mixture is uniformly stirred, the mixture is dispersed for 15 to 30min at a high speed of 1000 to 1200r/min, a sulfonic acid type block copolymer dispersing agent is added, the mixture is dispersed for 30 to 45min at a high speed, and the mixture is moved to a nano sand mill for circular grinding for 6 to 12h until the particle size D is reached50Less than 200nm, transferring the mixture into a mixing cylinder, adding a pH regulator, a defoaming agent and an anti-settling agent at the rotating speed of 300-500 r/min, and stirringStirring for 20-30 min, filtering and packaging to obtain the ethanol-resistant aqueous Grice nanometer color concentrate.
The ethanol-resistant aqueous Grice nano-grade dye prepared by the invention has excellent tinting strength, transparency, compatibility, alcohol resistance, storage stability, alkali resistance, acid resistance, high temperature resistance of 300 ℃, sun resistance, stain resistance, migration resistance and ultraviolet resistance. The water-based UV paint is widely applied to the fields of woodware color wiping, water-based woodware paint, water-based automobile paint, water-based plastic paint, water-based industrial paint, water-based glass baking paint, water-based metal baking paint, water-based UV paint, water-based surface printing ink and the like.
Detailed Description
An ethanol-resistant aqueous glaze nanocolone of the present invention is further described below with reference to the examples. It is to be understood that the specific embodiments described herein are merely illustrative of the relevant invention and not restrictive of the invention.
Example 1
A sulfonic acid type anionic block copolymer dispersant A comprises the following steps:
a) sequentially adding dimethyl sulfoxide, hydroxybutyl acrylate and 1, 3-propane sultone into a reaction kettle according to the weight ratio of the formula, starting to stir and dissolve uniformly, heating to 65 ℃ for reaction for 7 hours, cooling to 40 ℃, adding methanol for dissolution, then adding acetone for precipitation, performing suction filtration on the precipitate, dissolving with methanol, precipitating with acetone, performing suction filtration, and repeating for 2-3 times to obtain a vinyl monomer I containing a sodium sulfonate group; wherein the molar ratio of the hydroxybutyl acrylate to the 1, 3-propane sultone is 1.3: 1;
b) in N2Adding 15.0 parts of maleic anhydride, 0.8 part of diethyl dithiocarbamate type quaternary ammonium salt and 32.0 parts of ethanol into a protected reaction kettle in sequence, stirring and dissolving, heating to 80 ℃, uniformly dropwise adding 10.0 parts of ethanol solution containing 10% of azodicyano valeric acid, keeping the temperature at 80 ℃ for continuous reaction for 2.5 hours after dropwise adding is finished within 0.5 hour; adding 10.0 parts of the vinyl monomer I containing the sodium sulfonate group, controlling the temperature at 70 ℃ to continue reacting for 6 hours, cooling to 50 ℃, adding 1.0 part of sodium hydroxide and 6.0 parts of deionized water, stirring for 0.5 hour, and adjusting the pH to 8-8And 5, obtaining the sulfonic acid type anionic block copolymer dispersant A.
Example 2
A sulfonic acid type anionic block copolymer dispersant B comprises the following steps:
a) sequentially adding butanone, hydroxyethyl methacrylate and 1, 4-butanesultone into a reaction kettle according to the weight ratio of the formula, starting stirring and dissolving uniformly, heating to 90 ℃ for reaction for 6 hours, cooling to 40 ℃, adding methanol for dissolution, then adding acetone for precipitation, performing suction filtration on the precipitate, dissolving with methanol, precipitating with acetone, performing suction filtration, and repeating for 2-3 times to obtain a vinyl monomer I containing a sodium sulfonate group; wherein the molar ratio of the hydroxyethyl methacrylate to the 1, 4-butanesultone is 1: 1;
b) in N2Sequentially adding 20.0 parts of maleic anhydride, 0.5 part of alpha-dithiobenzyl p-phenylmethylene pyridinium chloride and 30.0 parts of ethanol into a protected reaction kettle, stirring and dissolving, heating to 90 ℃, uniformly dropwise adding 12.0 parts of ethanol solution containing 10% of azodiisobutyronitrile, keeping the temperature at 90 ℃ for continuous reaction for 3 hours after the dropwise adding is finished within 0.5 hour; and adding 10.0 parts of the vinyl monomer I containing the sodium sulfonate group, controlling the temperature to be 90 ℃, continuously reacting for 6 hours, cooling to 50 ℃, adding 1.5 parts of ammonia water and 14.5 parts of deionized water, stirring for 0.5 hour, and adjusting the pH value to be 8-8.5 to obtain the sulfonic acid type anionic block copolymer dispersant B.
Example 3
A sulfonic acid type anionic block copolymer dispersant C, which comprises the following steps:
a) sequentially adding dimethylformamide, hydroxypropyl methacrylate and 3-methyl-1, 3-propane sultone into a reaction kettle according to the weight ratio of the formula, starting stirring and dissolving uniformly, heating to 70 ℃ for reacting for 6 hours, cooling to 40 ℃, adding methanol for dissolving, then adding acetone for precipitating, carrying out suction filtration on the precipitate, dissolving with methanol, precipitating with acetone, carrying out suction filtration, and repeating for 2-3 times to obtain a vinyl monomer I containing a sodium sulfonate group; wherein the molar ratio of the hydroxypropyl methacrylate to the 3-methyl-1, 3-propane sultone is 1.2: 1;
b) in N2Reaction of protectionSequentially adding 20.0 parts of maleic anhydride, 2.0 parts of dithiophenylacetic acid and 40.0 parts of ethanol into a kettle, stirring and dissolving, heating to 100 ℃, uniformly dropwise adding 15.0 parts of ethanol solution containing 10% of azobisisobutyronitrile, keeping the temperature at 100 ℃ for continuous reaction for 2 hours after dropwise adding is finished within 0.5 hour; adding 12.0 parts of the vinyl monomer I containing the sodium sulfonate group, controlling the temperature at 100 ℃ to continue reacting for 4 hours, cooling to 50 ℃, adding 1.2 parts of sodium hydroxide and 12.0 parts of deionized water, stirring for 0.5 hour, and adjusting the pH to 8.5-9 to obtain the sulfonic acid type anionic block copolymer dispersant C.
Technical indexes of the sulfonic acid type anionic block copolymer dispersant prepared in the embodiment of the invention are shown in table 1:
TABLE 1 technical indices of sulfonic acid type anionic block copolymer dispersants
| Name (R) | Dispersant A | Dispersant B | Dispersant C |
| Solid content% | 40.2 | 41.2 | 40.6 |
| Number average molecular weight Mn | 7254 | 5161 | 4936 |
| Polydisperse coefficient PDI | 1.25 | 1.23 | 1.21 |
Example 4
An ethanol-resistant aqueous glaze nano-grade color concentrate comprises the following components in percentage by weight: 12.6 parts of deionized water, 8.0 parts of methyl 3-methoxypropionate, 30.0 parts of ethanol, 1.5 parts of silane coupling agent, 25.0 parts of transparent iron oxide red or yellow powder, 20.0 parts of sulfonic acid type anionic block copolymer dispersant A, 0.2 part of pH regulator, 0.2 part of defoaming agent and 0.5 part of anti-settling agent.
Example 5
An ethanol-resistant aqueous glaze nano-grade color concentrate comprises the following components in percentage by weight: 14.2 parts of deionized water, 6.0 parts of methyl 3-methoxypropionate, 40.0 parts of ethanol, 1.0 part of titanate coupling agent, 20.0 parts of coffee calcined umber powder, 18.0 parts of sulfonic acid type anionic block copolymer dispersant B, 0.2 part of pH regulator, 0.2 part of defoaming agent and 0.4 part of anti-settling agent.
Example 6
An ethanol-resistant aqueous glaze nano-grade color concentrate comprises the following components in percentage by weight: 14.7 parts of deionized water, 5.0 parts of methyl 3-methoxypropionate, 40.0 parts of ethanol, 1.0 part of titanate coupling agent, 20.0 parts of tamarind seed chromogen debar powder, 18.5 parts of sulfonic acid type anionic block copolymer dispersant, 0.2 part of pH regulator, 0.2 part of defoaming agent and 0.4 part of anti-settling agent.
The examples 4, 5 and 6 were compared with commercially available aqueous transparent iron oxide pastes and aqueous anba pink tints, and the test data are shown in table 2:
TABLE 2 Water-based glaze nanometer color concentrate Performance technical index
While the invention has been described in detail and with reference to specific embodiments thereof, it will be apparent to one skilled in the art that various changes, modifications and variations can be made therein without departing from the spirit and scope of the invention as defined in the following claims.
Claims (3)
1. An ethanol-resistant aqueous glaze nano-grade color concentrate is characterized in that: the composition comprises the following components in percentage by weight: 5.0-10.0 percent of 3-methoxy methyl propionate, 20.0-50.0 percent of ethanol, 1.0-3.0 percent of surface treating agent, 20.0-30.0 percent of toner, 10.0-25.0 percent of sulfonic acid type anionic block copolymer dispersant, 0.1-0.5 percent of pH regulator, 0.1-0.5 percent of defoaming agent, 0.2-1.0 percent of anti-settling agent and the balance of deionized water;
the sulfonic acid type anionic block copolymer dispersant is synthesized by adopting RAFT technology, and the preparation steps are as follows:
a) sequentially adding dimethylformamide, hydroxybutyl acrylate and 1, 3-propane sultone into a reaction kettle according to the weight ratio of the formula, starting stirring and dissolving uniformly, heating to 65 ℃ for reaction for 7 hours, cooling to 40 ℃, adding methanol for dissolving, then adding acetone for precipitation, performing suction filtration on the precipitate, dissolving with methanol, precipitating with acetone, performing suction filtration, and repeating for 2-3 times to obtain a vinyl monomer I containing a sodium sulfonate group; wherein the molar ratio of the hydroxybutyl acrylate to the 1, 3-propane sultone is 1.3: 1;
b) in N2Adding 15.0 parts of maleic anhydride, 0.8 part of diethyl dithiocarbamate type quaternary ammonium salt and 32.0 parts of ethanol solvent into a protected reaction kettle in sequence, stirring and dissolving, heating to 80 ℃, uniformly dropwise adding 10.0 parts of ethanol solution containing 10% of azodicyano valeric acid, keeping the temperature at 80 ℃ for continuous reaction for 2.5 hours after dropwise adding is finished within 0.5 hour; then adding 10.0 parts of vinyl monomer I containing sodium sulfonate groups, controlling the temperature at 70 ℃ to continue reacting for 6 hours, cooling to 50 ℃, adding 1.0 part of sodium hydroxide and 6.0 parts of deionized water, stirring for 0.5 hour, and controlling the pH to be 8-8.5 to prepare the sulfonic acid type anionic block copolymer dispersant;
the sulfonic acid type block copolymer aqueous dispersant is an A-B block structure, the number average molecular weight of the sulfonic acid type block copolymer aqueous dispersant is 7254, and the polydispersity number PDI = 1.25;
the surface treating agent is one of silane coupling agent, zirconate coupling agent and titanate coupling agent.
2. The ethanol-resistant aqueous gelisin nano-concentrate of claim 1, characterized in that: the toner is one of transparent iron oxide, translucent calcined umber powder and translucent raw umber powder.
3. A method of preparing the ethanol-resistant aqueous gelisin nano-concentrate of claim 1, characterized in that: the preparation method comprises the following steps:
according to the weight ratio of the formula, deionized water, ethanol, methyl 3-methoxypropionate and a surface treating agent are added into a dispersing barrel, toner is added after the mixture is uniformly stirred, the mixture is dispersed for 15 to 30min at a high speed of 1000 to 1200r/min, a sulfonic acid type anionic block copolymer dispersing agent is added, the mixture is dispersed for 30 to 45min at a high speed, and the mixture is moved to a nano sand mill for circular grinding for 6 to 12h until the particle size D is reached50And (3) transferring the mixture to a mixing cylinder at the rotating speed of 300-500 r/min, adding a pH regulator, a defoaming agent and an anti-settling agent, stirring for 20-30 min, filtering and packaging to obtain the ethanol-resistant aqueous Grice nano-grade chromogen.
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| JPS59227940A (en) * | 1983-06-09 | 1984-12-21 | Kansai Paint Co Ltd | Aqueous pigment dispersion |
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| WO2005021630A1 (en) * | 2003-08-27 | 2005-03-10 | Ciba Specialty Chemicals Holding Inc. | Composition and process for the controlled synthesis of block copolymers |
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| FR2935000B1 (en) * | 2008-08-12 | 2011-07-01 | Arkema France | PROCESS FOR THE SYNTHESIS OF AMPHIPHILIC COPOLYMERS WITH A GRADIENT OF COMPOSITON AND SOLUBLES IN ALKALI |
| CN101983976A (en) * | 2010-12-10 | 2011-03-09 | 华东理工大学 | Preparation method of fluorine-silicon segmented copolymer |
| JP5223980B2 (en) * | 2011-04-21 | 2013-06-26 | 大日本印刷株式会社 | Color material dispersion, colored resin composition for color filter, color filter, liquid crystal display device and organic light emitting display device |
| CN102363679A (en) * | 2011-06-30 | 2012-02-29 | 成都倍大涂料有限公司 | Water-soluble glaze and preparation method thereof |
| CN103788775B (en) * | 2014-02-17 | 2016-04-13 | 苏州雄鹰纳米科技有限公司 | A kind of water-based paint type nano color paste and preparation method thereof |
| CN103881039B (en) * | 2014-03-03 | 2017-04-26 | 王志军 | Functional segmented copolymer based on living polymerization as well as preparation method and application of copolymer |
| CN107207739B (en) * | 2015-01-05 | 2020-09-01 | 罗地亚经营管理公司 | Amine-imino diol neutralizing agents for low volatile compound waterborne organic coating compositions and methods of use thereof |
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