CN108624172A - A kind of aqueous diatom ooze liquid coating and preparation method with self-repair function - Google Patents
A kind of aqueous diatom ooze liquid coating and preparation method with self-repair function Download PDFInfo
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- CN108624172A CN108624172A CN201810522359.3A CN201810522359A CN108624172A CN 108624172 A CN108624172 A CN 108624172A CN 201810522359 A CN201810522359 A CN 201810522359A CN 108624172 A CN108624172 A CN 108624172A
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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
- C09D133/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Coating compositions based on derivatives of such polymers
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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
- C09D7/65—Additives macromolecular
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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
- C09D7/70—Additives characterised by shape, e.g. fibres, flakes or microspheres
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
Abstract
The present invention provides a kind of aqueous diatom ooze liquid coating and preparation method with self-repair function.Respectively using the dimethyl silicone polymer of ethylene functionalization and platinum catalyst mixture, Dimethicone Copolyol body as core material, two kinds of microcapsules are made by sprayed deposit cellulose acetate, in the hydrophilic film for being cross-linked to form chitosan after surface active, two kinds of modified microcapsules are made, it is finally mixed with diatomite, pure-acrylic emulsion, polyacrylate emulsion, dimethyl silicone polymer, mica powder, polyurethane thickener, water, surfactant, obtains the aqueous diatom ooze liquid coating with self-repair function.This method is by coating two kinds of microcapsules of different core materials using cellulose acetate as raw material, cause capsules break in the coating crack extension of diatom ooze coating, the selfreparing component released in core material is reacted, the reparation of fracture can efficiently be rapidly completed, and surface of microcapsule forms hydrophilic film, it is uniformly dispersed, ensure that selfreparing effect.
Description
Technical field
The present invention relates to paint fields, and in particular to the preparation of self-healing coatings having selfreparing more particularly to one kind
The aqueous diatom ooze liquid coating and preparation method of function.
Background technology
The major function material of diatom ooze is diatomite, is made of pure natural inorganic material, without any harmful substance with
And harmful additive, material sheet is as pure green environment-friendly products.With fine and smooth, loose, light, porous, water imbibition and permeability
Physical properties, unique " molecular sieve " structure and the selective absorption performance such as strong, can effectively remove the free first in air
Harmful substances such as aldehyde, benzene, ammonia and because of peculiar smell caused by pet, smoking, rubbish, essence room air can effectively adsorb sky
The harmful substances such as formaldehyde, benzene, ammonia dissociated in gas, and can purify different because of generations such as pet, smoking, rubbish in air
Taste can also adjust indoor air humidity, therefore the alternative latex of diatom ooze by absorbing and discharging the moisture in air
The tradition wall decorative material such as paint, wallpaper, thus become the new lover of decorative building material in the market, by the blueness of more and more users
It looks at.
The development of aqueous diatom ooze coating in recent years particularly attracts attention, and wall brushing can be gone up without allotment, according to
The clay pits such as different characteristics diatomite it is reasonably combined.But rehabilitation cost is higher after the damage of its coating, and self-repair technology can mould
The characteristic of biomimetic structure realizes that material carries out self healing under conditions of no extraneous participation.The self-repair technology of coating,
Self healing ability is inspired after by biological bulk damage, in the case where polymer material cracks, by being embedded in material
The release of internal the coated chemical substance of microcapsules timely automated can repair impaired coating surface, keep its surface aesthetic
With gloss, extend the materials'use service life, reduces maintenance cost.Therefore, self-repair technology answering in aqueous diatom ooze coating field
With the new highlight as development.
Chinese invention patent application number 201710999638.4 discloses a kind of low temperature resistant self-healing coatings and its preparation side
Method.The low temperature resistant self-healing coatings carry out degradation liquefaction using gutta percha as raw material, to gutta percha, then carry out epoxidation,
Finally it is grafted with aqueous epoxy resins.Under cryogenic, coating has good hardness and strength, when temperature is higher than rubber
When glue glass transition temperature, coating can repair tiny crack and bubbling automatically, while coating has good bendability, soft
Toughness and elongation percentage and impact resistance.
Chinese invention patent application number 201710458364.8 discloses a kind of synthetic method of self-repairing microcapsule, including
Following steps：（1）It emulsifies, obtains after emulsifier, urea, formaldehyde, reaction promoter, diluent, alkyd resin are mixed with water
Lotion；（2）By lotion heating, reaction, self-repairing microcapsule is obtained.The invention uses the selfreparing of one-step method fabricated in situ
Microcapsules are using alkyd resin as core material, using Lauxite as wall material.The coatings obtained by the invention self-repairing microcapsule,
When coating is damaged, microcapsules rupture therewith, and the alkyd resin core material outflow of capsule forms a film with air haptoreaction and repairs
Damaged part improves the corrosion resistance after coating is damaged, extends the military service of coating, it can be achieved that the selfreparing of coating under room temperature
Time limit.
Chinese invention patent application number 201410101557.4 discloses for self-healing coatings microcapsules, prepares and answer
With belonging to technical field of coatings.Microcapsules in the invention are using urea, formaldehyde as wall components, with fluorocarbon resin and ring
Oxygen resin is mixed into capsule-core ingredient, and particle size range can be obtained in the microcapsules of 300um ~ 400um, the microcapsules of preparation and aqueous fluorine
Carbon coating is mixed for the reparation of coating.
Chinese invention patent application number 201711000429.0 discloses a kind of wooden material surface water paint selfreparing
Microcapsules include the raw material of following parts by weight：15 ~ 30 parts of urea, 30 ~ 50 parts of formaldehyde, 10 ~ 20 parts of diethanol amine, 1 ~ 5
The fluororesin of part, 3 ~ 8 parts of epoxy resin, 7 ~ 16 parts of water-based acrylic resin, 0.1 ~ 2 part of photoinitiator, 0.005 ~ 2 part
Neopelex, 5 ~ 20 parts of distilled water.Fluororesin and ring is added using urea, formaldehyde as cyst wall raw material in the invention
Oxygen resin is to prepare modified wall material, using water-based acrylic resin as capsule-core, prepares modified polyurea formaldehyde cladding water soluble acrylic acid tree
Grease microcapsule synthesizes the material with self-repair function using microcapsules technology, is applied in water paint, repairs wooden material
The defects of expecting the slight crack on surface ensures the performance of wood product surface water paint, can make wooden to extend the coating service life
Material surface coating has low-luster and wearability, shock resistance and self-reparing capability.
According to above-mentioned, the water paint in existing scheme involves great expense, and brushes to repair after coating damage and is more troublesome, not only
Economic cost is high, and repairing effect is undesirable, and the diatom ooze coating with self-repair function there is no report at present.In view of
This, the present invention proposes a kind of aqueous diatom ooze liquid coating and preparation method with self-repair function, can effectively solve
State technical problem.
Invention content
It involves great expense using wider water paint for current, brushing reparation after coating damage is more troublesome, and not only passes through
It helps of high cost, and repairing effect is undesirable, the present invention proposes a kind of aqueous diatom ooze liquid coating with self-repair function
And preparation method, damage coating is rapidly and efficiently repaired to effectively realize, and repairing effect is good, service life is long.
Specific technical solution of the present invention is as follows：
A kind of preparation method of the aqueous diatom ooze liquid coating with self-repair function, includes the following steps：
（1）The dimethyl silicone polymer of ethylene functionalization and platinum catalyst are mixed and are used as core material, it is fine by sprayed deposit acetic acid
Dimension element is used as capsule material, and microcapsules A is made；
（2）Using Dimethicone Copolyol body as core material, capsule material is used as by sprayed deposit cellulose acetate, micro- glue is made
Capsule B；
（3）Microcapsules A, which is immersed in oxalic acid solution, makes 15 ~ 30min of surface active, is then placed in fluid bed, is warming up to 30 ~ 50
DEG C, and the acidic aqueous solution for being passed through chitosan is recycled, it is self-assembly of the hydrophily of one layer of cross-linked chitosan in surface of microcapsule
Modified microcapsule A is made in film；
（4）Microcapsules B, which is immersed in oxalic acid solution, makes 15 ~ 30min of surface active, is then placed in fluid bed, is warming up to 30 ~ 50
DEG C, and the acidic aqueous solution for being passed through chitosan is recycled, it is self-assembly of the hydrophily of one layer of cross-linked chitosan in surface of microcapsule
Modified microcapsule B is made in film；
（5）By modified microcapsule A, modified microcapsule B and diatomite, pure-acrylic emulsion, polyacrylate emulsion, polydimethylsiloxanes
Alkane, mica powder, polyurethane thickener, water, surfactant mixing, modulation obtain the aqueous diatom ooze liquid with self-repair function
State coating.
Preferably, step（1）The number-average molecular weight of the dimethyl silicone polymer of the ethylene functionalization is 3 ~ 5 × 106。
Preferably, step（1）In the microcapsules A, 79 ~ 87 parts by weight of dimethyl silicone polymer of ethylene functionalization, platinum
3 ~ 6 parts by weight of catalyst, 10 ~ 15 parts by weight of cellulose acetate.
Preferably, step（2）The number-average molecular weight of the Dimethicone Copolyol body is 2 ~ 8 × 104。
Preferably, step（2）In the microcapsules B, 85 ~ 90 parts by weight of Dimethicone Copolyol body, acetate fiber
Plain 10 ~ 15 parts by weight.Wherein, Dimethicone Copolyol body preferentially selects polyether-modified Dimethicone Copolyol body.
Preferably, the mass concentration of the oxalic acid solution is 8 ~ 12%.
Preferably, the mass concentration of the acidic aqueous solution of the chitosan is 25 ~ 30%, and pH value is 4 ~ 5.
Preferably, step（5）The surfactant is neopelex, lauryl sodium sulfate or ethoxy
At least one of sodium sulfonate.
Preferably, step（5）In the liquid coating, 4 ~ 6 parts by weight of modified microcapsule A, 4 ~ 6 weights of modified microcapsule B
Measure part, 30 ~ 35 parts by weight of diatomite, 5 ~ 8 parts by weight of pure-acrylic emulsion, 5 ~ 8 parts by weight of polyacrylate emulsion, dimethyl silicone polymer
1 ~ 2 parts by weight, 4 ~ 8 parts by weight of mica powder, 1.5 ~ 3 parts by weight of polyurethane thickener, 23 ~ 45 parts by weight of water, surfactant 0.5
~ 1 parts by weight.Wherein pure-acrylic emulsion solid content is 25wt%；Polyacrylate emulsion solid content is 18wt%.
The present invention also provides the aqueous diatom ooze liquid with self-repair function that a kind of above-mentioned preparation method is prepared
Coating.By being crosslinked one layer of hydrophilic film of self assembly in surface of microcapsule, hydrophilic modifying is carried out to microcapsules, prepares water paint
When dispersion evenly；Cause capsules break when coating crack extends, releases core material as selfreparing component, two kinds of core material hairs
Raw reaction：Active site in Dimethicone Copolyol body can be with the dimethyl silicone polymer of ethylene functionalization under platinum catalysis
It is reacted, thus fracture is repaired.
The present invention provides a kind of aqueous diatom ooze liquid coating and preparation method with self-repair function, with existing skill
Art is compared, and the feature and excellent effect protruded is：
1, propose that two kinds of microcapsules that different core materials are coated using cellulose acetate are aqueous with self-repair function as raw material preparation
The method of diatom ooze liquid coating.
2, it is split in the coating of diatom ooze coating as raw material by two kinds of microcapsules coating different core materials using cellulose acetate
Line causes capsules break when extending, and releases dimethyl silicone polymer, the dimethyl silicone polymer of the ethylene functionalization in core material
Copolymer and platinum catalyst, are reacted, and the reparation of fracture can efficiently be rapidly completed.
3, by being crosslinked one layer of hydrophilic film of self assembly in the surface of microcapsule of cladding selfreparing component, microcapsules are carried out
Hydrophilic modifying is uniformly dispersed in water paint obtained, to ensure that selfreparing effect.
Specific implementation mode
In the following, the present invention will be further described in detail by way of specific embodiments, but this should not be interpreted as to the present invention
Range be only limitted to example below.Without departing from the idea of the above method of the present invention, according to ordinary skill
The various replacements or change that knowledge and customary means are made, should be included in the scope of the present invention.
Embodiment 1
Preparation process is：
（1）The dimethyl silicone polymer of ethylene functionalization and platinum catalyst are mixed and are used as core material, it is fine by sprayed deposit acetic acid
Dimension element is used as capsule material, and microcapsules A is made；In microcapsules A, 82 parts by weight of dimethyl silicone polymer of ethylene functionalization, platinum catalysis
5 parts by weight of agent, 13 parts by weight of cellulose acetate；
（2）Using Dimethicone Copolyol body as core material, capsule material is used as by sprayed deposit cellulose acetate, micro- glue is made
Capsule B；In microcapsules B, 87 parts by weight of Dimethicone Copolyol body, 13 parts by weight of cellulose acetate；
（3）Microcapsules A, which is immersed in oxalic acid solution, makes surface active 23min, is then placed in fluid bed, is warming up to 43 DEG C, and
Cycle is passed through the acidic aqueous solution of chitosan, and modified microcapsule A is made；The mass concentration of oxalic acid solution is 9%；The acid of chitosan
Property aqueous solution mass concentration be 27%, pH value 4；
（4）Microcapsules B, which is immersed in oxalic acid solution, makes surface active 23min, is then placed in fluid bed, is warming up to 43 DEG C, and
Cycle is passed through the acidic aqueous solution of chitosan, and modified microcapsule B is made；The mass concentration of oxalic acid solution is 9%；The acid of chitosan
Property aqueous solution mass concentration be 27%, pH value 4；
（5）By modified microcapsule A, modified microcapsule B and diatomite, pure-acrylic emulsion, polyacrylate emulsion, polydimethylsiloxanes
Alkane, mica powder, polyurethane thickener, water, surfactant mixing, modulation obtain the aqueous diatom ooze liquid with self-repair function
State coating；Surfactant is neopelex；In liquid coating, 5 parts by weight of modified microcapsule A, modified microcapsule
5 parts by weight of B, 33 parts by weight of diatomite, 7 parts by weight of pure-acrylic emulsion, 7 parts by weight of polyacrylate emulsion, dimethyl silicone polymer 1
Parts by weight, 5 parts by weight of mica powder, 2 parts by weight of polyurethane thickener, 34 parts by weight of water, 1 parts by weight of surfactant.
Test method is：
By water paint even application made from embodiment 1 on the square tinplate that the length of side is 100mm, average thickness is
3mm is 25 DEG C in temperature, and relative humidity cures 7 days in the environment of being 50%, with blade in standardized scratch of coating surface, averagely
Width is 1mm, and using vernier caliper measurement scratch length, digital camera observes and records release core material reparation after microcapsules rupture and scrapes
The process of trace, while respectively scratch length, the repairing effect after the completion of observation reparation are measured in 20s, 50,100s and 150s.
The microcapsules deployment conditions of the aqueous diatom ooze liquid coating of the embodiment 1 measured by the above method, and scrape
Scratch length and repairing effect when trace is tested is as shown in table 1.
Embodiment 2
Preparation process is：
（1）The dimethyl silicone polymer of ethylene functionalization and platinum catalyst are mixed and are used as core material, it is fine by sprayed deposit acetic acid
Dimension element is used as capsule material, and microcapsules A is made；In microcapsules A, 87 parts by weight of dimethyl silicone polymer of ethylene functionalization, platinum catalysis
3 parts by weight of agent, 10 parts by weight of cellulose acetate；
（2）Using Dimethicone Copolyol body as core material, capsule material is used as by sprayed deposit cellulose acetate, micro- glue is made
Capsule B；In microcapsules B, 85 parts by weight of Dimethicone Copolyol body, 15 parts by weight of cellulose acetate；
（3）Microcapsules A, which is immersed in oxalic acid solution, makes surface active 15min, is then placed in fluid bed, is warming up to 30 DEG C, and
Cycle is passed through the acidic aqueous solution of chitosan, and modified microcapsule A is made；The mass concentration of oxalic acid solution is 8%；The acid of chitosan
Property aqueous solution mass concentration be 25%, pH value 4；
（4）Microcapsules B, which is immersed in oxalic acid solution, makes surface active 15min, is then placed in fluid bed, is warming up to 30 DEG C, and
Cycle is passed through the acidic aqueous solution of chitosan, and modified microcapsule B is made；The mass concentration of oxalic acid solution is 8%；The acid of chitosan
Property aqueous solution mass concentration be 25%, pH value 4；
（5）By modified microcapsule A, modified microcapsule B and diatomite, pure-acrylic emulsion, polyacrylate emulsion, polydimethylsiloxanes
Alkane, mica powder, polyurethane thickener, water, surfactant mixing, modulation obtain the aqueous diatom ooze liquid with self-repair function
State coating；Surfactant is lauryl sodium sulfate；In liquid coating, 4 parts by weight of modified microcapsule A, modified microcapsule B
4 parts by weight, 30 parts by weight of diatomite, 5 parts by weight of pure-acrylic emulsion, 5 parts by weight of polyacrylate emulsion, 1 weight of dimethyl silicone polymer
Measure part, 4 parts by weight of mica powder, 1.5 parts by weight of polyurethane thickener, 45 parts by weight of water, 0.5 parts by weight of surfactant.
Test method is：
By water paint even application made from embodiment 2 on the square tinplate that the length of side is 100mm, average thickness is
3mm is 25 DEG C in temperature, and relative humidity cures 7 days in the environment of being 50%, with blade in standardized scratch of coating surface, averagely
Width is 1mm, and using vernier caliper measurement scratch length, digital camera observes and records release core material reparation after microcapsules rupture and scrapes
The process of trace, while respectively scratch length, the repairing effect after the completion of observation reparation are measured in 20s, 50,100s and 150s.
The microcapsules deployment conditions of the aqueous diatom ooze liquid coating of the embodiment 2 measured by the above method, and scrape
Scratch length and repairing effect when trace is tested is as shown in table 1.
Embodiment 3
Preparation process is：
（1）The dimethyl silicone polymer of ethylene functionalization and platinum catalyst are mixed and are used as core material, it is fine by sprayed deposit acetic acid
Dimension element is used as capsule material, and microcapsules A is made；In microcapsules A, 79 parts by weight of dimethyl silicone polymer of ethylene functionalization, platinum catalysis
6 parts by weight of agent, 15 parts by weight of cellulose acetate；
（2）Using Dimethicone Copolyol body as core material, capsule material is used as by sprayed deposit cellulose acetate, micro- glue is made
Capsule B；In microcapsules B, 90 parts by weight of Dimethicone Copolyol body, 10 parts by weight of cellulose acetate；
（3）Microcapsules A, which is immersed in oxalic acid solution, makes surface active 30min, is then placed in fluid bed, is warming up to 50 DEG C, and
Cycle is passed through the acidic aqueous solution of chitosan, and modified microcapsule A is made；The mass concentration of oxalic acid solution is 12%；The acid of chitosan
Property aqueous solution mass concentration be 30%, pH value 5；
（4）Microcapsules B, which is immersed in oxalic acid solution, makes surface active 30min, is then placed in fluid bed, is warming up to 50 DEG C, and
Cycle is passed through the acidic aqueous solution of chitosan, and modified microcapsule B is made；The mass concentration of oxalic acid solution is 12%；The acid of chitosan
Property aqueous solution mass concentration be 30%, pH value 5；
（5）By modified microcapsule A, modified microcapsule B and diatomite, pure-acrylic emulsion, polyacrylate emulsion, polydimethylsiloxanes
Alkane, mica powder, polyurethane thickener, water, surfactant mixing, modulation obtain the aqueous diatom ooze liquid with self-repair function
State coating；Surfactant is sodium isethionate；In liquid coating, 6 parts by weight of modified microcapsule A, modified microcapsule B 6
Parts by weight, 35 parts by weight of diatomite, 8 parts by weight of pure-acrylic emulsion, 8 parts by weight of polyacrylate emulsion, 2 weight of dimethyl silicone polymer
Part, 8 parts by weight of mica powder, 3 parts by weight of polyurethane thickener, 23 parts by weight of water, 1 parts by weight of surfactant.
Test method is：
By water paint even application made from embodiment 3 on the square tinplate that the length of side is 100mm, average thickness is
3mm is 25 DEG C in temperature, and relative humidity cures 7 days in the environment of being 50%, with blade in standardized scratch of coating surface, averagely
Width is 1mm, and using vernier caliper measurement scratch length, digital camera observes and records release core material reparation after microcapsules rupture and scrapes
The process of trace, while respectively scratch length, the repairing effect after the completion of observation reparation are measured in 20s, 50,100s and 150s.
The microcapsules deployment conditions of the aqueous diatom ooze liquid coating of the embodiment 3 measured by the above method, and scrape
Scratch length and repairing effect when trace is tested is as shown in table 1.
Embodiment 4
Preparation process is：
（1）The dimethyl silicone polymer of ethylene functionalization and platinum catalyst are mixed and are used as core material, it is fine by sprayed deposit acetic acid
Dimension element is used as capsule material, and microcapsules A is made；In microcapsules A, 84 parts by weight of dimethyl silicone polymer of ethylene functionalization, platinum catalysis
4 parts by weight of agent, 12 parts by weight of cellulose acetate；
（2）Using Dimethicone Copolyol body as core material, capsule material is used as by sprayed deposit cellulose acetate, micro- glue is made
Capsule B；In microcapsules B, 86 parts by weight of Dimethicone Copolyol body, 14 parts by weight of cellulose acetate；
（3）Microcapsules A, which is immersed in oxalic acid solution, makes surface active 17min, is then placed in fluid bed, is warming up to 35 DEG C, and
Cycle is passed through the acidic aqueous solution of chitosan, and modified microcapsule A is made；The mass concentration of oxalic acid solution is 9%；The acid of chitosan
Property aqueous solution mass concentration be 26%, pH value 4；
（4）Microcapsules B, which is immersed in oxalic acid solution, makes surface active 18min, is then placed in fluid bed, is warming up to 38 DEG C, and
Cycle is passed through the acidic aqueous solution of chitosan, and modified microcapsule B is made；The mass concentration of oxalic acid solution is 9%；The acid of chitosan
Property aqueous solution mass concentration be 26%, pH value 4；
（5）By modified microcapsule A, modified microcapsule B and diatomite, pure-acrylic emulsion, polyacrylate emulsion, polydimethylsiloxanes
Alkane, mica powder, polyurethane thickener, water, surfactant mixing, modulation obtain the aqueous diatom ooze liquid with self-repair function
State coating；Surfactant is neopelex；In liquid coating, 5 parts by weight of modified microcapsule A, modified microcapsule
4 parts by weight of B, 31 parts by weight of diatomite, 6 parts by weight of pure-acrylic emulsion, 6 parts by weight of polyacrylate emulsion, dimethyl silicone polymer 1
Parts by weight, 5 parts by weight of mica powder, 1.5 parts by weight of polyurethane thickener, 40 parts by weight of water, 0.5 parts by weight of surfactant.
Test method is：
By water paint even application made from embodiment 4 on the square tinplate that the length of side is 100mm, average thickness is
3mm is 25 DEG C in temperature, and relative humidity cures 7 days in the environment of being 50%, with blade in standardized scratch of coating surface, averagely
Width is 1mm, and using vernier caliper measurement scratch length, digital camera observes and records release core material reparation after microcapsules rupture and scrapes
The process of trace, while respectively scratch length, the repairing effect after the completion of observation reparation are measured in 20s, 50,100s and 150s.
The microcapsules deployment conditions of the aqueous diatom ooze liquid coating of the embodiment 4 measured by the above method, and scrape
Scratch length and repairing effect when trace is tested is as shown in table 1.
Embodiment 5
Preparation process is：
（1）The dimethyl silicone polymer of ethylene functionalization and platinum catalyst are mixed and are used as core material, it is fine by sprayed deposit acetic acid
Dimension element is used as capsule material, and microcapsules A is made；In microcapsules A, 81 parts by weight of dimethyl silicone polymer of ethylene functionalization, platinum catalysis
5 parts by weight of agent, 14 parts by weight of cellulose acetate；
（2）Using Dimethicone Copolyol body as core material, capsule material is used as by sprayed deposit cellulose acetate, micro- glue is made
Capsule B；In microcapsules B, 88 parts by weight of Dimethicone Copolyol body, 12 parts by weight of cellulose acetate；
（3）Microcapsules A, which is immersed in oxalic acid solution, makes surface active 25min, is then placed in fluid bed, is warming up to 45 DEG C, and
Cycle is passed through the acidic aqueous solution of chitosan, and modified microcapsule A is made；The mass concentration of oxalic acid solution is 11%；The acid of chitosan
Property aqueous solution mass concentration be 29%, pH value 5；
（4）Microcapsules B, which is immersed in oxalic acid solution, makes surface active 26min, is then placed in fluid bed, is warming up to 44 DEG C, and
Cycle is passed through the acidic aqueous solution of chitosan, and modified microcapsule B is made；The mass concentration of oxalic acid solution is 11%；The acid of chitosan
Property aqueous solution mass concentration be 29%, pH value 5；
（5）By modified microcapsule A, modified microcapsule B and diatomite, pure-acrylic emulsion, polyacrylate emulsion, polydimethylsiloxanes
Alkane, mica powder, polyurethane thickener, water, surfactant mixing, modulation obtain the aqueous diatom ooze liquid with self-repair function
State coating；Surfactant is lauryl sodium sulfate；In liquid coating, 6 parts by weight of modified microcapsule A, modified microcapsule B
5 parts by weight, 34 parts by weight of diatomite, 6 parts by weight of pure-acrylic emulsion, 7 parts by weight of polyacrylate emulsion, 2 weight of dimethyl silicone polymer
Measure part, 7 parts by weight of mica powder, 3 parts by weight of polyurethane thickener, 29 parts by weight of water, 1 parts by weight of surfactant.
Test method is：
By water paint even application made from embodiment 5 on the square tinplate that the length of side is 100mm, average thickness is
3mm is 25 DEG C in temperature, and relative humidity cures 7 days in the environment of being 50%, with blade in standardized scratch of coating surface, averagely
Width is 1mm, and using vernier caliper measurement scratch length, digital camera observes and records release core material reparation after microcapsules rupture and scrapes
The process of trace, while respectively scratch length, the repairing effect after the completion of observation reparation are measured in 20s, 50,100s and 150s.
The microcapsules deployment conditions of the aqueous diatom ooze liquid coating of the embodiment 5 measured by the above method, and scrape
Scratch length and repairing effect when trace is tested is as shown in table 1.
Embodiment 6
Preparation process is：
（1）The dimethyl silicone polymer of ethylene functionalization and platinum catalyst are mixed and are used as core material, it is fine by sprayed deposit acetic acid
Dimension element is used as capsule material, and microcapsules A is made；In microcapsules A, 82 parts by weight of dimethyl silicone polymer of ethylene functionalization, platinum catalysis
5 parts by weight of agent, 13 parts by weight of cellulose acetate；
（2）Using Dimethicone Copolyol body as core material, capsule material is used as by sprayed deposit cellulose acetate, micro- glue is made
Capsule B；In microcapsules B, 88 parts by weight of Dimethicone Copolyol body, 12 parts by weight of cellulose acetate；
（3）Microcapsules A, which is immersed in oxalic acid solution, makes surface active 20min, is then placed in fluid bed, is warming up to 40 DEG C, and
Cycle is passed through the acidic aqueous solution of chitosan, and modified microcapsule A is made；The mass concentration of oxalic acid solution is 10%；The acid of chitosan
Property aqueous solution mass concentration be 28%, pH value 4；
（4）Microcapsules B, which is immersed in oxalic acid solution, makes surface active 20min, is then placed in fluid bed, is warming up to 40 DEG C, and
Cycle is passed through the acidic aqueous solution of chitosan, and modified microcapsule B is made；The mass concentration of oxalic acid solution is 10%；The acid of chitosan
Property aqueous solution mass concentration be 28%, pH value 4；
（5）By modified microcapsule A, modified microcapsule B and diatomite, pure-acrylic emulsion, polyacrylate emulsion, polydimethylsiloxanes
Alkane, mica powder, polyurethane thickener, water, surfactant mixing, modulation obtain the aqueous diatom ooze liquid with self-repair function
State coating；Surfactant is sodium isethionate；In liquid coating, 5 parts by weight of modified microcapsule A, modified microcapsule B 5
Parts by weight, 32 parts by weight of diatomite, 6 parts by weight of pure-acrylic emulsion, 6 parts by weight of polyacrylate emulsion, 2 weight of dimethyl silicone polymer
Part, 6 parts by weight of mica powder, 2 parts by weight of polyurethane thickener, 35 parts by weight of water, 1 parts by weight of surfactant.
Test method is：
By water paint even application made from embodiment 6 on the square tinplate that the length of side is 100mm, average thickness is
3mm is 25 DEG C in temperature, and relative humidity cures 7 days in the environment of being 50%, with blade in standardized scratch of coating surface, averagely
Width is 1mm, and using vernier caliper measurement scratch length, digital camera observes and records release core material reparation after microcapsules rupture and scrapes
The process of trace, while respectively scratch length, the repairing effect after the completion of observation reparation are measured in 20s, 50,100s and 150s.
The microcapsules deployment conditions of the aqueous diatom ooze liquid coating of the embodiment 6 measured by the above method, and scrape
Scratch length and repairing effect when trace is tested is as shown in table 1.
Comparative example 1
Preparation process is：
（1）By diatomite, pure-acrylic emulsion, polyacrylate emulsion, dimethyl silicone polymer, mica powder, polyurethane thickener, water,
Surfactant mixes, and modulation obtains the aqueous diatom ooze liquid coating with self-repair function；Surfactant is ethoxy
Sodium sulfonate；In liquid coating, 32 parts by weight of diatomite, 6 parts by weight of pure-acrylic emulsion, 6 parts by weight of polyacrylate emulsion, poly dimethyl
2 parts by weight of siloxanes, 6 parts by weight of mica powder, 2 parts by weight of polyurethane thickener, 35 parts by weight of water, 1 parts by weight of surfactant.
Test method is：
By water paint even application made from comparative example 1 on the square tinplate that the length of side is 100mm, average thickness is
3mm is 25 DEG C in temperature, and relative humidity cures 7 days in the environment of being 50%, with blade in standardized scratch of coating surface, averagely
Width is 1mm, and using vernier caliper measurement scratch length, digital camera observes and records release core material reparation after microcapsules rupture and scrapes
The process of trace, while respectively scratch length, the repairing effect after the completion of observation reparation are measured in 20s, 50,100s and 150s.
The microcapsules deployment conditions of the aqueous diatom ooze liquid coating of the comparative example 1 measured by the above method, and scrape
Scratch length and repairing effect when trace is tested is as shown in table 1.
Table 1：
Claims (10)
1. a kind of preparation method of the aqueous diatom ooze liquid coating with self-repair function, which is characterized in that including following step
Suddenly：
（1）The dimethyl silicone polymer of ethylene functionalization and platinum catalyst are mixed and are used as core material, it is fine by sprayed deposit acetic acid
Dimension element is used as capsule material, and microcapsules A is made；
（2）Using Dimethicone Copolyol body as core material, capsule material is used as by sprayed deposit cellulose acetate, micro- glue is made
Capsule B；
（3）Microcapsules A, which is immersed in oxalic acid solution, makes 15 ~ 30min of surface active, is then placed in fluid bed, is warming up to 30 ~ 50
DEG C, and the acidic aqueous solution for being passed through chitosan is recycled, it is self-assembly of the hydrophily of one layer of cross-linked chitosan in surface of microcapsule
Modified microcapsule A is made in film；
（4）Microcapsules B, which is immersed in oxalic acid solution, makes 15 ~ 30min of surface active, is then placed in fluid bed, is warming up to 30 ~ 50
DEG C, and the acidic aqueous solution for being passed through chitosan is recycled, it is self-assembly of the hydrophily of one layer of cross-linked chitosan in surface of microcapsule
Modified microcapsule B is made in film；
（5）By modified microcapsule A, modified microcapsule B and diatomite, pure-acrylic emulsion, polyacrylate emulsion, polydimethylsiloxanes
Alkane, mica powder, polyurethane thickener, water, surfactant mixing, modulation obtain the aqueous diatom ooze liquid with self-repair function
State coating.
2. a kind of preparation method of the aqueous diatom ooze liquid coating with self-repair function according to claim 1, special
Sign is：Step（1）The number-average molecular weight of the dimethyl silicone polymer of the ethylene functionalization is 3 ~ 5 × 106。
3. a kind of preparation method of the aqueous diatom ooze liquid coating with self-repair function according to claim 1, special
Sign is：Step（1）In the microcapsules A, 79 ~ 87 parts by weight of dimethyl silicone polymer of ethylene functionalization, platinum catalyst 3 ~ 6
Parts by weight, 10 ~ 15 parts by weight of cellulose acetate.
4. a kind of preparation method of the aqueous diatom ooze liquid coating with self-repair function according to claim 1, special
Sign is：Step（2）The number-average molecular weight of the Dimethicone Copolyol body is 2 ~ 8 × 104。
5. a kind of preparation method of the aqueous diatom ooze liquid coating with self-repair function according to claim 1, special
Sign is：Step（2）In the microcapsules B, 85 ~ 90 parts by weight of Dimethicone Copolyol body, 10 ~ 15 weight of cellulose acetate
Measure part.
6. a kind of preparation method of the aqueous diatom ooze liquid coating with self-repair function according to claim 1, special
Sign is：The mass concentration of the oxalic acid solution is 8 ~ 12%.
7. a kind of preparation method of the aqueous diatom ooze liquid coating with self-repair function according to claim 1, special
Sign is：The mass concentration of the acidic aqueous solution of the chitosan is 25 ~ 30%, and pH value is 4 ~ 5.
8. a kind of preparation method of the aqueous diatom ooze liquid coating with self-repair function according to claim 1, special
Sign is：Step（5）The surfactant is in neopelex, lauryl sodium sulfate or sodium isethionate
At least one.
9. a kind of preparation method of the aqueous diatom ooze liquid coating with self-repair function according to claim 1, special
Sign is：Step（5）In the liquid coating, 4 ~ 6 parts by weight of modified microcapsule A, 4 ~ 6 parts by weight of modified microcapsule B, diatom
Native 30 ~ 35 parts by weight, 5 ~ 8 parts by weight of pure-acrylic emulsion, 5 ~ 8 parts by weight of polyacrylate emulsion, 1 ~ 2 weight of dimethyl silicone polymer
Part, 4 ~ 8 parts by weight of mica powder, 1.5 ~ 3 parts by weight of polyurethane thickener, 23 ~ 45 parts by weight of water, 0.5 ~ 1 weight of surfactant
Part.
10. a kind of aqueous diatom ooze with self-repair function that any one of claim 1 ~ 9 preparation method is prepared
Liquid coating.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109505030A (en) * | 2018-11-01 | 2019-03-22 | 上海理工大学 | A kind of bi-component selfreparing nanofiber and the water paint containing the fiber |
| CN110669396A (en) * | 2019-10-05 | 2020-01-10 | 鲁东大学 | Method for constructing self-repairing aldehyde-removing coating by extracting cellulose nanocrystals |
| CN110681683A (en) * | 2019-10-10 | 2020-01-14 | 太仓该亚机器人科技有限公司 | Complexing agent microcapsule for phytoremediation soil and preparation method thereof |
| EP3685913A1 (en) * | 2019-01-23 | 2020-07-29 | Solvay Specialty Polymers Italy S.p.A. | Microcapsules-containing composition |
| CN111690318A (en) * | 2020-07-30 | 2020-09-22 | 九天起宏(江苏)检测有限公司 | Self-repairing waterborne polyurethane coating composition and coating |
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2018
- 2018-05-28 CN CN201810522359.3A patent/CN108624172A/en not_active Withdrawn
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109505030A (en) * | 2018-11-01 | 2019-03-22 | 上海理工大学 | A kind of bi-component selfreparing nanofiber and the water paint containing the fiber |
| EP3685913A1 (en) * | 2019-01-23 | 2020-07-29 | Solvay Specialty Polymers Italy S.p.A. | Microcapsules-containing composition |
| CN110669396A (en) * | 2019-10-05 | 2020-01-10 | 鲁东大学 | Method for constructing self-repairing aldehyde-removing coating by extracting cellulose nanocrystals |
| CN110681683A (en) * | 2019-10-10 | 2020-01-14 | 太仓该亚机器人科技有限公司 | Complexing agent microcapsule for phytoremediation soil and preparation method thereof |
| CN111690318A (en) * | 2020-07-30 | 2020-09-22 | 九天起宏(江苏)检测有限公司 | Self-repairing waterborne polyurethane coating composition and coating |
| CN111690318B (en) * | 2020-07-30 | 2021-10-26 | 广东嘉盛环保高新材料股份有限公司 | Self-repairing waterborne polyurethane coating composition and coating |
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Application publication date: 20181009 |