CN109971237A - A kind of pigment anti-settling agent - Google Patents
A kind of pigment anti-settling agent Download PDFInfo
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- CN109971237A CN109971237A CN201910181288.XA CN201910181288A CN109971237A CN 109971237 A CN109971237 A CN 109971237A CN 201910181288 A CN201910181288 A CN 201910181288A CN 109971237 A CN109971237 A CN 109971237A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
- C08G65/26—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds
- C08G65/2603—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing oxygen
- C08G65/2606—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing oxygen containing hydroxyl groups
- C08G65/2609—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring from cyclic ethers and other compounds the other compounds containing oxygen containing hydroxyl groups containing aliphatic hydroxyl groups
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G65/00—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule
- C08G65/02—Macromolecular compounds obtained by reactions forming an ether link in the main chain of the macromolecule from cyclic ethers by opening of the heterocyclic ring
- C08G65/32—Polymers modified by chemical after-treatment
- C08G65/329—Polymers modified by chemical after-treatment with organic compounds
- C08G65/333—Polymers modified by chemical after-treatment with organic compounds containing nitrogen
- C08G65/33348—Polymers modified by chemical after-treatment with organic compounds containing nitrogen containing isocyanate group
- C08G65/33351—Polymers modified by chemical after-treatment with organic compounds containing nitrogen containing isocyanate group acyclic
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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
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/40—Additives
- C09D7/45—Anti-settling agents
Abstract
The invention discloses a kind of pigment anti-settling agents, belong to coating anti-settling agent field.The present invention prepares anti-settling additive, and the shear stress between fluid layer reduces, and results in viscosity decline, when shearing force disappearance, winds again, makes it have preferable anti-shear ability, and reduces sedimentation possibility；The association additive of preparation forms bridging so that anti-settling agent can form preferable association micella with the oil base in pigment ink when in use, forms network structure with ink base, prevents its sedimentation；Emulsifier is added, form fine and close interfacial film, reduce oil water interfacial tension, so that the system of anti-settling agent keeps stablizing, anti-settling agent can preferably penetrate into the gap between ink particle and particle, the package for carrying out pigment ink particle carries out anti-settling, improves and emulsifies anti-settling efficiency, and makes anti-settling to reach ideal effect.The present invention solves the problems, such as that current anti-settling agent mechanical performance and anti-settling performance are poor.
Description
Technical field
The present invention relates to coating anti-settling agent technical fields, and in particular to a kind of pigment anti-settling agent.
Background technique
Sedimentation phenomenon is the major issue usually encountered in coating material production and use process.In coating material production and use each
A stage, the rheological property of coating are also must be taken into consideration an important factor for.With the research and development of special functional coating,
Requirement to coating property is higher and higher.The addition of metal powder makes the settlement issues of coating become research people in conducting function coating
The main problem of member's concern.Anti-settling agent is added in coating, i.e., introduces loose webs thixotropy structure in coating, face can be made
Filler particles suspend without agglomerating, and prevent pigment sedimentation, improve coating property, keep excellent levelability etc..In coating, ink
Etc. in industries, pigments and fillers it is anti-settling be coating and printing ink storing technology important link.Pigment forms solid-liquid in coating, ink
Easy to form to sink to the bottom phenomenon under state, that is, the pigment to suspend in a solvent can occur flocculation after a certain time and sink to the bottom.Relative to working as
It is preceding just for the building coating (emulsion paint etc.) based on widely applied organic matter, include petrifaction, noninflammability, thoroughly
Gas, sterile and tongue fur Ji breed, painting color never fades, the feature of environmental protection, odorless, are suitble to all mineral construction materials etc. all
More feature performance benefits, so aqueous inorganic paint is increasingly by the favor in market；But aqueous inorganic paint face one it is great
If technical problem, that is, aqueous inorganic paint system adds filler, the anti-settling of filler is difficult to solve, in painting, storage, construction
May it assemble in.Stable homogeneous dispersion in order to obtain, it is often necessary to use anti-settling agent.Anti-settling agent is a kind of painting
The rheology control agent of material, it makes coating have anti-settling property, and viscosity greatly improves, and anti-settling agent plays important work in modern coatings
With being had an important influence on to the production of coating, storage, coating and film performance, so its use is paid more and more attention.Common
Anti-settling agent such as polyamide, bentonite, fumed silica etc. is in the absolutely not anti-settling effect of the system, and the filler of addition is in coating
In precipitate and form scleroma block quickly, good application effect can not be kept in practical applications, castor oil derivative is anti-settling
Castor oil derivative is dissolved in nonpolar solvent by agent using castor oil derivative as major ingredient, by dispersing, activating, is swollen
Long-chain is mutually wound thixotroping structure and plays thickening power, and when by shearing force, winding is opened, and structure is destroyed, viscosity
It can decline, when shearing force disappearance, wind again.Traditional anti-settling agent producing process is very complicated, it be by 1-6 hexamethylene diamine,
Rilanit special reaction is added and generates polyamide slurry, is then cooled into solid polyamide powder, then pass through slice process
After being handled, investment pulverizer carries out solid crushing, and powder particle diameter D50 is about 6-7 μm, is then added in 20% solvent
Room temperature emulsification is carried out, polyamide slurry is made, constant temperature roaster is placed into and carries out activation 3-4 days, or so totally 70 hours, finally make
At finished product.Thus technique as it can be seen that there are more drawback and mechanical performance it is bad, Fast curing is slow, be easy to appear return it is thick bad
Phenomenon is unfavorable for reaching the ideal result of prevention of product, the side that patent CN105368103A uses filler and resin separately to store
Formula solves the problems, such as that the storage of coating is anti-settling, but this mode is also needed in paint spraying by filler and resin dispersion machine point
Dissipate the uniformly coating that just can be carried out, it is more complicated when compared to this patent construction, once and the construction time it is too long, filler
The block that precipitates and have the tendency that harden can be generated therefore to study new anti-settling agent and be of great significance.
Summary of the invention
The technical problems to be solved by the invention: it for the problem of current anti-settling agent mechanical performance and anti-settling performance difference, mentions
For a kind of pigment anti-settling agent.
In order to solve the above technical problems, the present invention is using technical solution as described below:
A kind of pigment anti-settling agent, according to parts by weight, including 3 ~ 7 parts of complex additives, 1 ~ 3 part of emulsifier, 20 ~ 30 parts of water, also
Including 20 ~ 30 parts of anti-settling additives, 5 ~ 10 parts of association additives.
The anti-settling additive the preparation method comprises the following steps:
(1) it takes activity gel raw material 2 ~ 5:5 in mass ratio ~ 10 that chlorination (1- butyl -3- methylimidazole) mixing is added, obtains mixture,
It takes tetramethylammonium hydroxide 1 ~ 3:10 in mass ratio ~ 15 that water is added to be stirred, obtains mixed liquor, take mixed liquor in mass ratio 2 ~ 5:
It is stirred in 30 ~ 50 addition mixtures, obtains stirring mixture；
(2) take stirring mixture 10 ~ 20:1 in mass ratio ~ 3 be added dodecenylsuccinic anhydride, addition be stirred amount of substance 3 ~
5% n,N-diisopropylethylamine, is passed through nitrogen protection, is stirred, and must stir mixture a, takes stirring mixture a by quality
Acetic acid is added than 10 ~ 20:2 ~ 5 to be stirred, filters, filter residue is taken to wash through dehydrated alcohol, it is dry to get anti-settling additive.
Activity gel raw material in the step (1) are as follows: take guar gum 4 ~ 8:2 in mass ratio ~ 5 that carragheen mixing is added, i.e.,
?.
The association additive stirs the preparation method comprises the following steps: taking mechanical strength enhancer 2 ~ 5:3 in mass ratio ~ 9 that solvent is added
Mixing is mixed, the dry toluene that solvent quality 3 ~ 8% is added is stirred, then is cooled to 70 ~ 80 DEG C and is stirred, and must be stirred
Object a, take stirring mixture a 5 ~ 10:2 in mass ratio ~ 5 be added octadecylisocyanate, add stirring mixture a mass 1 ~
3% isooctyl acid bismuth is stirred, vacuum distillation, object a must be evaporated under reduced pressure, take be stirred 1 ~ 4:5 ~ 10 in mass ratio a go from
Sub- water is stirred to get association additive.
The preparation method of the mechanical strength enhancer: taking raw polyol 80 ~ 100:2 in mass ratio ~ 5 that potassium hydroxide is added,
It is kept under 30 ~ 40 DEG C, -0.095MPa state, 10 ~ 15 times of raw polyol quality of ethylene oxide is added, protected in 110 ~ 120 DEG C
Temperature, vacuum distillation, obtains vacuum distillation object, takes vacuum distillation object 100 ~ 150:2 in mass ratio ~ 7 that dimethyl carbonate is added, is passed through nitrogen
Gas shielded, the epoxychloropropane that 20 ~ 30 times of amount of substance of vacuum distillation is added are stirred, and vacuum distillation is to get mechanical strength increasing
Strong agent.
The raw polyol are as follows: take sorbierite 3 ~ 5:1 in mass ratio ~ 4:1 ~ 3 be added mannitol, laruyl alcohol mixing to get.
The solvent are as follows: take dimethylbenzene 7 ~ 9:1 in mass ratio ~ 3 be added isopropanol mixing to get.
The complex additive are as follows: take carbomer 10 ~ 15:2 in mass ratio ~ 5:3 ~ 7 that stearic acid, glucose mixing is added,
To obtain the final product.
The emulsifier are as follows: take dodecyl sodium sulfonate calcium 3 ~ 5:2 in mass ratio ~ 7:5 ~ 10 that 2- acrylamido -2- is added
Methyl propane sulfonic acid, polyisobutene succinimide mixing to get.
The present invention is compared with other methods, and advantageous effects are:
(1) prepare anti-settling additive be to be dissolved using activity gel raw material as raw material through imidazole ion liquid to the present invention, after catalysis and
Dodecenylsuccinic anhydride is reacted, and obtains the anti-settling additive with thickening effect, after pigment ink is added, through imidazoles from
Son dissolved activity gel raw material increases the efficiency of substitution reaction when being reacted, introduce dodecenyl-succinic acid in molecule
Side chain, molecular weight increases, so that the increase of ink apparent viscosity, and the strand of activity gel raw material is random arrangement
, it is wound between long-chain, very big resistance can be generated, play the role of hindering flowing, when being generated flowing by shear stress,
The entanglement of long-chain molecule is destroyed, and the shear stress between fluid layer reduces, and results in viscosity decline, when shearing force disappearance, and again
New winding makes it have preferable anti-shear ability, and reduces sedimentation possibility；
(2) association additive prepared by the present invention is first that reacting ethylene oxide is added and generates low molecule using raw polyol as initiator
The alcohols material of amount, then make with epoxychloropropane formation mechanical strength enhancer with preferable toughness under catalytic action
The anti-settling agent film that ink particle surface must be adsorbed in has excellent shock resistance, makes it when by shear action to ink
It is protected, recycles mechanical strength enhancer hydroxyl to react with octadecylisocyanate, the octadecyl of oleophylic is connected to
On polyethylene glycol end group, it is made of hydrophilic segment and oleophylic segment, and hydrophilic and oleophylic segment is then by hydroxyl and isocyanide
The carbamate groups that acid esters reaction generates are connected, and can preferably disperse in anti-settling agent while it is with preferable oleophylic
End group associative property forms bridge so that anti-settling agent can form preferable association micella with the oil base in pigment ink when in use
Even, network structure is formed with ink base, prevents its sedimentation；
(3) present invention be added in emulsifier be added the derivative surfactant containing fatty acid and alkyl sulfonic acid and amide groups and
The surfactant compound of hydroxyl can make it first soak to ink particle, re-form fine and close interfacial film, reduce oil
Water interfacial tension, so that the system of anti-settling agent keeps stablizing, anti-settling agent can preferably penetrate between ink particle and particle
Gap, the package for carrying out pigment ink particle carries out anti-settling, improves and emulsifies anti-settling efficiency, and makes anti-settling to reach ideal
Effect；
(4) present invention is first increased with anti-settling additive and is wound between long-chain, generates resistance, viscous when by shear stress generation flowing
Degree decline is wound again when shearing force disappears, and makes it have preferable anti-shear ability, and reduces sedimentation possibility, then lead to
The bridging effect between association additive increase ink and anti-settling agent is crossed, resistance to stress surge protection is carried out to ink particle surface,
Mechanical performance is improved, cross-linked structure is formed faster, improves anti-settling efficiency, carries out accelerating anti-settling agent infiltration finally by emulsifier
Effect shortens onset time, reaches ideal result of prevention.
Specific embodiment
Activity gel raw material are as follows: take guar gum 4 ~ 8:2 in mass ratio ~ 5 be added carragheen mixing to get.
Anti-settling additive the preparation method comprises the following steps:
(1) it takes activity gel raw material 2 ~ 5:5 in mass ratio ~ 10 that chlorination (1- butyl -3- methylimidazole) mixing is added, obtains mixture,
It takes tetramethylammonium hydroxide 1 ~ 3:10 in mass ratio ~ 15 that water is added and is stirred 20 ~ 30min, obtain mixed liquor, take mixed liquor by matter
Amount is added in mixture than 2 ~ 5:30 ~ 50, and 20 ~ 40min is stirred in 2 ~ 5 DEG C, obtains stirring mixture；
(2) take stirring mixture 10 ~ 20:1 in mass ratio ~ 3 be added dodecenylsuccinic anhydride, addition be stirred amount of substance 3 ~
5% n,N-diisopropylethylamine, is passed through nitrogen protection, is stirred 1 ~ 3h in 25 ~ 30 DEG C, must stir mixture a, takes stirring
Acetic acid is added in mixture a 10 ~ 20:2 in mass ratio ~ 5, is stirred 20 ~ 30min, filters, filter residue is taken to wash through dehydrated alcohol,
Drying is to get anti-settling additive.
Raw polyol are as follows: take sorbierite 3 ~ 5:1 in mass ratio ~ 4:1 ~ 3 be added mannitol, laruyl alcohol mixing to get.
The preparation method of mechanical strength enhancer:
Take raw polyol 80 ~ 100:2 in mass ratio ~ 5 be added potassium hydroxide, under 30 ~ 40 DEG C, -0.095MPa state keep 20 ~
10 ~ 15 times of raw polyol quality of ethylene oxide is added in 30min, and in 110 ~ 120 DEG C of 1 ~ 3h of heat preservation, vacuum distillation must be evaporated under reduced pressure
Object takes vacuum distillation object 100 ~ 150:2 in mass ratio ~ 7 that dimethyl carbonate is added, is passed through nitrogen protection, and vacuum distillation object is added
The epoxychloropropane that 20 ~ 30 times of quality is stirred 2 ~ 4h in 140 ~ 150 DEG C, is evaporated under reduced pressure to get mechanical strength enhancer.
Solvent are as follows: take dimethylbenzene 7 ~ 9:1 in mass ratio ~ 3 be added isopropanol mixing to get.
Associate additive the preparation method comprises the following steps:
It takes mechanical strength enhancer 2 ~ 5:3 in mass ratio ~ 9 that solvent is added, is stirred 20 ~ 30min, solvent quality 3 ~ 8% is added
Dry toluene, be warming up to 100 ~ 110 DEG C and be stirred 2 ~ 4h, then be cooled to 70 ~ 80 DEG C and be stirred 20 ~ 40min, must stir
Mixture a takes stirring mixture a 5 ~ 10:2 in mass ratio ~ 5 that octadecylisocyanate is added, and adds stirring mixture a matter
The isooctyl acid bismuth of amount 1 ~ 3%, is stirred 3 ~ 5h in 80 ~ 90 DEG C, is evaporated under reduced pressure, must be evaporated under reduced pressure object a, take and be stirred a by matter
Amount compares the deionized water of 1 ~ 4:5 ~ 10, is stirred 20 ~ 40min to get association additive.
Complex additive are as follows: take carbomer 10 ~ 15:2 in mass ratio ~ 5:3 ~ 7 be added stearic acid, glucose mixing to get.
Emulsifier are as follows: take dodecyl sodium sulfonate calcium 3 ~ 5:2 in mass ratio ~ 7:5 ~ 10 that 2- acrylamido -2- methyl is added
Propane sulfonic acid, polyisobutene succinimide mixing to get.
A kind of pigment anti-settling agent, according to the mass fraction, including 20 ~ 30 parts of anti-settling additives, 5 ~ 10 parts of association additives, 3 ~
7 parts of complex additives, 1 ~ 3 part of emulsifier, 20 ~ 30 parts of water.
Activity gel raw material are as follows: take guar gum 4:2 in mass ratio be added carragheen mixing to get.
Anti-settling additive the preparation method comprises the following steps:
(1) it takes activity gel raw material 2:5 in mass ratio that chlorination (1- butyl -3- methylimidazole) mixing is added, obtains mixture, take tetramethyl
Base ammonium hydroxide 1:10 in mass ratio is added water and is stirred 20min, obtains mixed liquor, takes mixed liquor 2:30 to be in mass ratio added mixed
It closes in object, is stirred 20min in 2 DEG C, obtains stirring mixture；
(2) it takes stirring mixture 10:1 in mass ratio that dodecenylsuccinic anhydride is added, the N for being stirred amount of substance 3% is added,
N- diisopropylethylamine, is passed through nitrogen protection, is stirred 1h in 25 DEG C, must stir mixture a, takes stirring mixture a by matter
Acetic acid is added than 10:2 in amount, is stirred 20min, filters, filter residue is taken to wash through dehydrated alcohol, dry to get anti-settling additive.
Raw polyol are as follows: take sorbierite 3:1:1 in mass ratio be added mannitol, laruyl alcohol mixing to get.
The preparation method of mechanical strength enhancer:
It takes raw polyol 80:2 in mass ratio that potassium hydroxide is added, 20min is kept under 30 DEG C, -0.095MPa state, it is former that alcohol is added
The ethylene oxide of 10 times of quality of material, in 110 DEG C of heat preservation 1h, vacuum distillation obtains vacuum distillation object, takes vacuum distillation object in mass ratio
Dimethyl carbonate is added in 100:2, is passed through nitrogen protection, and the epoxychloropropane of 20 times of amount of substance of vacuum distillation is added, stirs in 140 DEG C
Mixing 2h is mixed, is evaporated under reduced pressure to get mechanical strength enhancer.
Solvent are as follows: take dimethylbenzene 7:1 in mass ratio be added isopropanol mixing to get.
Associate additive the preparation method comprises the following steps:
Take mechanical strength enhancer 2:3 in mass ratio that solvent is added, be stirred 20min, be added solvent quality 3% without water beetle
Benzene is warming up to 100 DEG C and is stirred 2h, then is cooled to 70 DEG C and is stirred 20min, must stir mixture a, take stirring mixture
Octadecylisocyanate is added in a 5:2 in mass ratio, adds the isooctyl acid bismuth of stirring mixture a mass 1%, stirs in 80 DEG C
3h is mixed, vacuum distillation must be evaporated under reduced pressure object a, take and be stirred a deionized water of 1:5 in mass ratio, be stirred 20min,
Up to association additive.
Complex additive are as follows: take carbomer 10:2:3 in mass ratio be added stearic acid, glucose mixing to get.
Emulsifier are as follows: take dodecyl sodium sulfonate calcium 3:2:5 in mass ratio be added 2- acrylamide-2-methylpro panesulfonic acid,
Polyisobutene succinimide mixing to get.
A kind of pigment anti-settling agent, according to the mass fraction, including 20 parts of anti-settling additives, 5 parts of association additives, 3 parts of compoundings
Additive, 1 part of emulsifier, 20 parts of water.
Activity gel raw material are as follows: take guar gum 8:5 in mass ratio be added carragheen mixing to get.
Anti-settling additive the preparation method comprises the following steps:
(1) it takes activity gel raw material 5:10 in mass ratio that chlorination (1- butyl -3- methylimidazole) mixing is added, obtains mixture, take four
Ammonium hydroxide 3:15 in mass ratio is added water and is stirred 30min, obtains mixed liquor, and mixed liquor 5:50 in mass ratio is taken to be added
In mixture, it is stirred 40min in 5 DEG C, obtains stirring mixture；
(2) it takes stirring mixture 20:3 in mass ratio that dodecenylsuccinic anhydride is added, the N for being stirred amount of substance 5% is added,
N- diisopropylethylamine, is passed through nitrogen protection, is stirred 3h in 30 DEG C, must stir mixture a, takes stirring mixture a by matter
Acetic acid is added than 20:5 in amount, is stirred 30min, filters, filter residue is taken to wash through dehydrated alcohol, dry to get anti-settling additive.
Raw polyol are as follows: take sorbierite 5:4:3 in mass ratio be added mannitol, laruyl alcohol mixing to get.
The preparation method of mechanical strength enhancer:
It takes raw polyol 100:5 in mass ratio that potassium hydroxide is added, 30min is kept under 40 DEG C, -0.095MPa state, alcohol is added
The ethylene oxide that 15 times of material quality, in 120 DEG C of heat preservation 3h, vacuum distillation obtains vacuum distillation object, takes vacuum distillation object by quality
Dimethyl carbonate is added than 150:7, is passed through nitrogen protection, the epoxychloropropane of 30 times of amount of substance of vacuum distillation is added, in 150 DEG C
It is stirred 4h, is evaporated under reduced pressure to get mechanical strength enhancer.
Solvent are as follows: take dimethylbenzene 9:3 in mass ratio be added isopropanol mixing to get.
Associate additive the preparation method comprises the following steps:
Take mechanical strength enhancer 5:9 in mass ratio that solvent is added, be stirred 30min, be added solvent quality 8% without water beetle
Benzene is warming up to 110 DEG C and is stirred 4h, then is cooled to 80 DEG C and is stirred 40min, must stir mixture a, take stirring mixture
Octadecylisocyanate is added in a 10:5 in mass ratio, adds the isooctyl acid bismuth of stirring mixture a mass 3%, stirs in 90 DEG C
Mixing 5h is mixed, vacuum distillation must be evaporated under reduced pressure object a, take and be stirred a deionized water of 4:10 in mass ratio, be stirred
40min is to get association additive.
Complex additive are as follows: take carbomer 15:5:7 in mass ratio be added stearic acid, glucose mixing to get.
Emulsifier are as follows: take dodecyl sodium sulfonate calcium 5:7:10 in mass ratio be added 2- acrylamide-2-methylpro panesulfonic acid,
Polyisobutene succinimide mixing to get.
A kind of pigment anti-settling agent, according to the mass fraction, including 30 parts of anti-settling additives, 10 parts of association additives, 7 parts of compoundings
Additive, 3 parts of emulsifiers, 30 parts of water.
Activity gel raw material are as follows: take guar gum 6:3 in mass ratio be added carragheen mixing to get.
Anti-settling additive the preparation method comprises the following steps:
(1) it takes activity gel raw material 3:7 in mass ratio that chlorination (1- butyl -3- methylimidazole) mixing is added, obtains mixture, take tetramethyl
Base ammonium hydroxide 2:13 in mass ratio is added water and is stirred 25min, obtains mixed liquor, takes mixed liquor 3:40 to be in mass ratio added mixed
It closes in object, is stirred 30min in 3 DEG C, obtains stirring mixture；
(2) it takes stirring mixture 15:2 in mass ratio that dodecenylsuccinic anhydride is added, the N for being stirred amount of substance 4% is added,
N- diisopropylethylamine, is passed through nitrogen protection, is stirred 2h in 27 DEG C, must stir mixture a, takes stirring mixture a by matter
Acetic acid is added than 15:3 in amount, is stirred 25min, filters, filter residue is taken to wash through dehydrated alcohol, dry to get anti-settling additive.
Raw polyol are as follows: take sorbierite 4:3:2 in mass ratio be added mannitol, laruyl alcohol mixing to get.
The preparation method of mechanical strength enhancer:
It takes raw polyol 90:4 in mass ratio that potassium hydroxide is added, 25min is kept under 35 DEG C, -0.095MPa state, it is former that alcohol is added
The ethylene oxide of 13 times of quality of material, in 115 DEG C of heat preservation 2h, vacuum distillation obtains vacuum distillation object, takes vacuum distillation object in mass ratio
Dimethyl carbonate is added in 130:5, is passed through nitrogen protection, and the epoxychloropropane of 25 times of amount of substance of vacuum distillation is added, stirs in 145 DEG C
Mixing 3h is mixed, is evaporated under reduced pressure to get mechanical strength enhancer.
Solvent are as follows: take dimethylbenzene 8:2 in mass ratio be added isopropanol mixing to get.
Associate additive the preparation method comprises the following steps:
Take mechanical strength enhancer 3:4 in mass ratio that solvent is added, be stirred 25min, be added solvent quality 6% without water beetle
Benzene is warming up to 105 DEG C and is stirred 3h, then is cooled to 75 DEG C and is stirred 30min, must stir mixture a, take stirring mixture
Octadecylisocyanate is added in a 7:3 in mass ratio, adds the isooctyl acid bismuth of stirring mixture a mass 2%, stirs in 85 DEG C
4h is mixed, vacuum distillation must be evaporated under reduced pressure object a, take and be stirred a deionized water of 3:7 in mass ratio, be stirred 30min,
Up to association additive.
Complex additive are as follows: take carbomer 13:3:4 in mass ratio be added stearic acid, glucose mixing to get.
Emulsifier are as follows: take dodecyl sodium sulfonate calcium 4:5:7 in mass ratio be added 2- acrylamide-2-methylpro panesulfonic acid,
Polyisobutene succinimide mixing to get.
A kind of pigment anti-settling agent, according to the mass fraction, including 25 parts of anti-settling additives, 7 parts of association additives, 5 parts of compoundings
Additive, 2 parts of emulsifiers, 25 parts of water.
Comparative example 1: it is essentially identical with the preparation method of embodiment 1, it has only the difference is that lacking anti-settling additive.
Comparative example 2: it is essentially identical with the preparation method of embodiment 1, it has only the difference is that lacking association additive.
Comparative example 3: the anti-settling agent of company, Yuhang city production.
The anti-settling agent that above-described embodiment is obtained with comparative example is detected, the pigment that anti-settling agent is added is scratched poly- four
On vinyl fluoride plate, the film of 1.5mm thickness is made, is placed on standard test conditions: (23 ± 2) DEG C, relative humidity (50 ± 10) %, maintenance
After 7d, correlated performance is tested in sample preparation.The tensile strength of coating, elongation at break press GB/T 16777-2008 " buildings waterproof material
Material test method " it is tested；Tearing strength presses the GB/T 529-2008 " survey of vulcanized rubber or thermoplastic elastomer tearing strength
It is fixed " in square test specimen tested, obtain that the results are shown in Table 1, prepared coating sample and deionized water pressed 1:
16 are diluted, and the sample after dilution, which is stored in be placed in 50 DEG C of baking ovens in 1000mL tool plug graduated cylinder, stands observation precipitating, precipitating
The corresponding calibration gauge of precipitating generated with graduated cylinder bottom is measured, specific result of prevention is shown in Table 2.
Table 1:
Table 2:
In summary, it can be seen that anti-settling agent effect of the invention is more preferable from table 1, table 2, be worth of widely use, the above is only
For preferred mode of the invention, it is not intended to limit the invention, it is all within the spirits and principles of the present invention, made any to repair
Change, equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.
Claims (9)
1. a kind of pigment anti-settling agent, according to parts by weight, including 3 ~ 7 parts of complex additives, 1 ~ 3 part of emulsifier, 20 ~ 30 parts of water,
It is characterized in that, further including 20 ~ 30 parts of anti-settling additives, 5 ~ 10 parts of association additives.
2. pigment anti-settling agent according to claim 1, which is characterized in that the anti-settling additive the preparation method comprises the following steps:
(1) it takes activity gel raw material 2 ~ 5:5 in mass ratio ~ 10 that chlorination (1- butyl -3- methylimidazole) mixing is added, obtains mixture,
It takes tetramethylammonium hydroxide 1 ~ 3:10 in mass ratio ~ 15 that water is added to be stirred, obtains mixed liquor, take mixed liquor in mass ratio 2 ~ 5:
It is stirred in 30 ~ 50 addition mixtures, obtains stirring mixture；
(2) take stirring mixture 10 ~ 20:1 in mass ratio ~ 3 be added dodecenylsuccinic anhydride, addition be stirred amount of substance 3 ~
5% n,N-diisopropylethylamine, is passed through nitrogen protection, is stirred, and must stir mixture a, takes stirring mixture a by quality
Acetic acid is added than 10 ~ 20:2 ~ 5 to be stirred, filters, filter residue is taken to wash through dehydrated alcohol, it is dry to get anti-settling additive.
3. pigment anti-settling agent according to claim 2, which is characterized in that the activity gel raw material in the step (1) are as follows: take
Guar gum 4 ~ 8:2 in mass ratio ~ 5 be added carragheen mixing to get.
4. pigment anti-settling agent according to claim 1, which is characterized in that it is described association additive the preparation method comprises the following steps: taking
Stirring solvent mixing is added in mechanical strength enhancer 2 ~ 5:3 in mass ratio ~ 9, and the dry toluene stirring of solvent quality 3 ~ 8% is added
Mixing, then be cooled to 70 ~ 80 DEG C and be stirred, mixture a must be stirred, stirring mixture a 5 ~ 10:2 in mass ratio ~ 5 is taken to be added
Octadecylisocyanate, the isooctyl acid bismuth for adding stirring mixture a mass 1 ~ 3% are stirred, are evaporated under reduced pressure, must depressurize
Distillation a takes the deionized water for being stirred 1 ~ 4:5 ~ 10 in mass ratio a to be stirred to get association additive.
5. pigment anti-settling agent according to claim 4, which is characterized in that the preparation method of the mechanical strength enhancer:
It takes raw polyol 80 ~ 100:2 in mass ratio ~ 5 that potassium hydroxide is added, is kept under 30 ~ 40 DEG C, -0.095MPa state, it is former that alcohol is added
10 ~ 15 times of quality of ethylene oxide of material, keeps the temperature in 110 ~ 120 DEG C, and vacuum distillation obtains vacuum distillation object, take vacuum distillation object by
Dimethyl carbonate is added in 100 ~ 150:2 of mass ratio ~ 7, is passed through nitrogen protection, and the epoxy of 20 ~ 30 times of amount of substance of vacuum distillation is added
Chloropropane is stirred, and is evaporated under reduced pressure to get mechanical strength enhancer.
6. pigment anti-settling agent according to claim 5, which is characterized in that the raw polyol are as follows: take sorbierite in mass ratio 3
~ 5:1 ~ 4:1 ~ 3 be added mannitol, laruyl alcohol mixing to get.
7. pigment anti-settling agent according to claim 4, which is characterized in that the solvent are as follows: take dimethylbenzene in mass ratio 7 ~
9:1 ~ 3 be added isopropanol mixing to get.
8. pigment anti-settling agent according to claim 1, which is characterized in that the complex additive are as follows: take carbomer by matter
Amount than 10 ~ 15:2 ~ 5:3 ~ 7 be added stearic acid, glucose mixing to get.
9. pigment anti-settling agent according to claim 1, which is characterized in that the emulsifier are as follows: take dodecyl sodium sulfonate calcium
2- acrylamide-2-methylpro panesulfonic acid, polyisobutene succinimide mixing is added in 3 ~ 5:2 in mass ratio ~ 7:5 ~ 10, i.e.,
?.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910181288.XA CN109971237A (en) | 2019-03-11 | 2019-03-11 | A kind of pigment anti-settling agent |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910181288.XA CN109971237A (en) | 2019-03-11 | 2019-03-11 | A kind of pigment anti-settling agent |
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| Publication Number | Publication Date |
|---|---|
| CN109971237A true CN109971237A (en) | 2019-07-05 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201910181288.XA Withdrawn CN109971237A (en) | 2019-03-11 | 2019-03-11 | A kind of pigment anti-settling agent |
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| Country | Link |
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| CN (1) | CN109971237A (en) |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102167944A (en) * | 2011-05-31 | 2011-08-31 | 苏州市金近涂料有限公司 | Water-based dipping lacquer and preparation method thereof |
| CN107216707A (en) * | 2017-05-04 | 2017-09-29 | 明光市飞洲新材料有限公司 | A kind of special anti-settling thickener of building coating and preparation method thereof |
-
2019
- 2019-03-11 CN CN201910181288.XA patent/CN109971237A/en not_active Withdrawn
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102167944A (en) * | 2011-05-31 | 2011-08-31 | 苏州市金近涂料有限公司 | Water-based dipping lacquer and preparation method thereof |
| CN107216707A (en) * | 2017-05-04 | 2017-09-29 | 明光市飞洲新材料有限公司 | A kind of special anti-settling thickener of building coating and preparation method thereof |
Non-Patent Citations (3)
| Title |
|---|
| 刘文主编: "《药用高分子材料学》", 30 June 2017, 中国中医药出版社 * |
| 李楠: "《琥珀酸瓜尔胶酯在BMIMCl离子液体中的合成及应用》", 《中国优秀硕士学位论文全文数据库 工程科技I缉》 * |
| 申小龙等: "《异山梨醇基生物高分子材料的研究进展》", 《石油化工》 * |
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Application publication date: 20190705 |