CN108587370A - A kind of emulsion paint for modifying nano-negative ion colloidal sol based on CdTe quantum - Google Patents
A kind of emulsion paint for modifying nano-negative ion colloidal sol based on CdTe quantum 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
- C09D143/00—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 containing boron, silicon, phosphorus, selenium, tellurium, or a metal; Coating compositions based on derivatives of such polymers
- C09D143/04—Homopolymers or copolymers of monomers containing silicon
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08B—POLYSACCHARIDES; DERIVATIVES THEREOF
- C08B15/00—Preparation of other cellulose derivatives or modified cellulose, e.g. complexes
- C08B15/05—Derivatives containing elements other than carbon, hydrogen, oxygen, halogens or sulfur
- C08B15/06—Derivatives containing elements other than carbon, hydrogen, oxygen, halogens or sulfur containing nitrogen, e.g. carbamates
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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
- C08F220/00—Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
- C08F220/02—Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
- C08F220/04—Acids; Metal salts or ammonium salts thereof
- C08F220/06—Acrylic acid; Methacrylic acid; Metal salts or ammonium salts thereof
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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
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/02—Emulsion paints including aerosols
- C09D5/024—Emulsion paints including aerosols characterised by the additives
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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
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/02—Emulsion paints including aerosols
- C09D5/024—Emulsion paints including aerosols characterised by the additives
- C09D5/025—Preservatives, e.g. antimicrobial agents
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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
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/02—Emulsion paints including aerosols
- C09D5/024—Emulsion paints including aerosols characterised by the additives
- C09D5/028—Pigments; Filters
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- 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
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/14—Paints containing biocides, e.g. fungicides, insecticides or pesticides
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- C09F—NATURAL RESINS; FRENCH POLISH; DRYING-OILS; DRIERS (SICCATIVES); TURPENTINE
- C09F1/00—Obtaining purification, or chemical modification of natural resins, e.g. oleo-resins
- C09F1/04—Chemical modification, e.g. esterification
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K3/00—Use of inorganic substances as compounding ingredients
- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
- C08K3/20—Oxides; Hydroxides
- C08K3/22—Oxides; Hydroxides of metals
- C08K2003/2237—Oxides; Hydroxides of metals of titanium
- C08K2003/2241—Titanium dioxide
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- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- 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 relates to a kind of emulsion paint composition for modifying nano-negative ion colloidal sol based on CdTe quantum is as follows：CdTe quantum modifies 25 80 parts of nano-negative ion colloidal sol, 250 350 parts of water, 35 parts of wetting dispersing agent, 13 parts of antifoaming agent, 0.5 1 parts of 95 multifunctional assistants of AP, unsaturated 5 10 parts of two ester type coalescents, 5 10 parts of propylene glycol, 20 80 parts of titanium dioxide, 23 parts of thickener, 80 250 parts of silicone acrylic emulsion.The present invention has synthesized the porous nano anion colloidal sol that non-setting active nucleocapsid is stabilized in aqueous dispersion for the first time；The luminous energy of the CdTe releases of selection is absorbed by Nano Titanium Oxide as Photocatalyst, increases its bactericidal effect.
Description
Technical field
The present invention relates to a kind of emulsion paint more particularly to a kind of nano-negative ion colloidal sol is modified based on CdTe quantum
Emulsion paint belongs to building coating technical field.
Technical background
In recent years, as living standards of the people are continuously improved, living environment constantly improves, and indoor decorating is increasingly bold and unconstrained
While China, beauty, the problem of indoor pollution influence health caused by finishing, is more and more.In general, people is daily
Need about 13,000,000,000 anions, and our room, office, the environment such as public place of entertainment, about 1-20 can only be provided hundred million.This
Huge contrast between kind supply and demand, tends to lead to pneumonia, the respiratory disorder of tracheitis.Central heating and air-cooling system
Air-conditioning system, anion are often purged.Synthetic fibers, carpet easily absorb anion with positive charge.Reinforcing bar, fiberboard all absorb
Anion.Therefore, indoor harmful gas is purified to high-efficient and lasting, the life of pure and fresh health, working environment is kept to be got at people
Carry out the target of more urgent pursuit.
Anion medical field be known as " air vitamin " its main function show as the nervous system to human body,
Respiratory system, metabolism, the circulatory system, treatment and health, immune system positive effect.At present building coating field by
Emulsion paint increases the content of anion in air in addition negative ion powder.For example, CN201310453843.2 be related to have bear from
Son, far infrared, except formaldehyde interiro wall latex paint and preparation method thereof, nano photo-catalytic and tourmaline anion powder are jointly used in
The production of interior wall coating is mutually excited using their collaboration, and effect enhances respective application effect；Product has in dim light
Also it can be released effectively the function of anion and far ir ray in environment, have the function of removing free formaldehyde in room air,
Also there is good elimination effect to pernicious gases such as benzene class, ammonia.
That there are negative ion powder efficiency is low for existing Negative Ion Emulsion Coatings, antibiotic property is poor, the shortcomings of having a single function.
Invention content
The shortcomings that overcome the prior art and deficiency, the present invention is intended to provide a kind of negative based on CdTe quantum modification nanometer
The emulsion paint of ion colloidal sol.
A kind of emulsion paint for modifying nano-negative ion colloidal sol based on CdTe quantum, by weight, composition is as follows：CdTe amounts
25-80 parts of nano-negative ion colloidal sol of son point modification, 250-350 parts of water, 3-5 parts of wetting dispersing agent, 1-3 parts of antifoaming agent, AP-95 are more
0.5-1 parts of function additive, unsaturated 5-10 parts of two ester type coalescents, 5-10 parts of propylene glycol, 20-80 parts of titanium dioxide, thickener
2-3 parts, 80-250 parts of silicone acrylic emulsion.
The CdTe quantum modifies nano-negative ion colloidal sol, there is following methods preparation：
(1) preparation of the porous nano anion colloidal sol of active nucleocapsid：The day of mass fraction 10-20% is prepared first
Right anion powder aqueous dispersions, then by above-mentioned dispersion liquid, account for the grinding aid of dispersion liquid total weight 0.1%-0.3%, be added
To being ground to powder median (d in nano-level grinder50) it is less than 100nm, it discharges up to nanoscale negative ion powder dispersion liquid；It takes
50 parts by weight nanoscale negative ion powder dispersion liquids, 10-20 parts by weight 0.6-1.2mol/L strong base solutions are added in reactor, are added
Heat to 80-95 DEG C of reaction 6-12h, then through cooling, be filtered to remove solid or big grain size anion powder, fully dialysis remove it is strong
Alkali is adjusted to pH after 8-9, to be able to the dispersion liquid that porous nano negative ion powder is suspended matter, as porous nano anion colloidal sol；
The ethanol solution for the titanate coupling agent that 20 parts by weight mass fractions are 3-5% is added in reactor, under stirring thereto
20-25 parts by weight porous nano anion colloidal sols are added dropwise dropwise, 1-2h is added dropwise, continues to be stirred to react 1-2h, be able to activity
Nano-titanium dioxide is shell, the sol solutions A that porous nano negative ion powder is core；
(2) preparation of CdTe quantum colloidal sol：Under inert gas shielding, by 0.2-0.3 parts by weight cadmium nitrate, 80-90 weights
Amount part deionized water, stabilizer are added in reactor and are stirred, and it is 8-9 that strong adjusting PH with base, which is added, adds 0.1-0.2 parts by weight telluriums
Sodium hydride, 90-95 DEG C is stirred to react 3-6h, obtains cadmium telluride quantum dot colloidal sol；
(3) CdTe quantum modifies nano-negative ion colloidal sol：Under the conditions of stirring at normal temperature, the colloidal sol into 40-45 parts by weight (1)
In liquid A, cadmium telluride quantum dot colloidal sol in 10-20 parts by weight (2) is added dropwise, 0.5-1h is added dropwise, and then proceedes to reaction 2-
4h obtains CdTe quantum modification nano-negative ion colloidal sol.
The wetting dispersing agent is polyocarboxy acid type anionic dispersing agents, organosilicon aqueous dispersion, nonionic high score
At least one of sub- aqueous dispersion；The antifoaming agent is preferably organic silicon antifoaming agent, polyacrylic antifoaming agent, phosphorus
At least one of esters of gallic acid antifoaming agent, silylated polyether class antifoaming agent, acetylenic diols antifoaming agent.
The preparation method of the two ester type coalescents of unsaturation, includes the following steps；
(1) rosin of 2-3 parts by weight is taken, heats and softens, is added in the diethylene glycol of 10-16 times of its weight, in 60-65
Insulated and stirred 10-20 minutes at DEG C, abienol liquid is obtained；
(2) butyl titanate for taking 20-25 parts by weight is added in above-mentioned abienol liquid, is added 45-50 parts by weight water, is stirred
Mix 3-4 hours, be added 25-30 parts by weight itaconic acids, increase temperature be 90-96 DEG C, be added 0.1-0.2 parts by weight to methylbenzene
Sulfonic acid, insulated and stirred 1-2 hours, dehydration obtain ester colloidal sol；
(3) above-mentioned ester colloidal sol is taken, is added in the dimethyl carbonate of its weight 46-50%, stirs evenly, obtains ester dispersion
Liquid；
(4) ethyl cellulose of the triethanolamine of 10-14 parts by weight, 2-3 parts by weight is mixed, is added to mixture weight
It is 1-2 hours ultrasonic in 1.8-2 times of absolute ethyl alcohol, ethyl alcohol is distilled off, the stearic acid of 20-22 parts by weight is added, stirring is equal
It is even, the p-methyl benzenesulfonic acid of 0.01-0.02 parts by weight is added, it is 180-185 DEG C to increase temperature, is stirred to react 6-7 hours, cooling
To room temperature, fiber ester amine is obtained；
(5) it takes above-mentioned ester dispersion liquid, fiber ester amine to be blended, stirs evenly, be sent in reaction kettle, be passed through nitrogen, adjust
Temperature of reaction kettle be 70-76 DEG C, react 40-46 hour, discharging cool down to get；
The degree of substitution of the ethyl cellulose is 2.3-2.5；
The grinding aid is polycarboxylic acids lubricating type grinding aid；The highly basic is sodium hydroxide, potassium hydroxide, hydroxide
At least one of barium；
The polycarboxylic acids lubricating type grinding aid has following structure：
Preparation method is：(1) by 10-20 parts by weight of acrylic acid sodium, 5-10 parts by weight list acrylic acid pentaerythritols ester,
50-100 parts by weight of deionized water stirs lower mixing, is heated to 90-100 DEG C, obtains mixed liquor a；(2) at 90-100 DEG C by 3-5
The ammonium persulfate aqueous solution of a concentration of 4-5% of parts by weight is added drop-wise to dropwise in mixed liquor a, is continued at 90-100 DEG C after being added dropwise
3-5h is reacted, mixed liquor b is obtained；(3) stop heating, 0.1-0.2 parts by weight chain terminating agents are added in mixed liquor b to tertiary butyl
Catechol, it is cooling to get to polycarboxylic acids lubricating type grinding aid.
The titanate coupling agent is at least one of butyl titanate, tetraethyl titanate, metatitanic acid orthocarbonate.
The stabilizer is sodium thioglycolate, 3- mercaptopropionic acids sodium, 3- thioacetic acid potassium, 3- mercaptobutyric acids potassium, 3- mercaptos
At least one of base sodium butyrate.
The emulsion paint that nano-negative ion colloidal sol is modified based on CdTe quantum, is prepared by following methods：
It is more that CdTe quantum modification nano-negative ion colloidal sol, water, wetting dispersing agent, AP-95 are sequentially added in dispersion cylinder
Function additive, unsaturated two ester type coalescents, propylene glycol, keep dispersion machine to be rotated with 400rpm-600rpm, fully dispersed
Then 20-30min will disperse disk center close to reactor bottom, and improve rotating speed and add to 800rpm-1200rpm, then by titanium dioxide
Enter and disperses 0.5-1h in dispersion cylinder；Rotating speed is down to 600rpm-800rpm, silicone acrylic emulsion, thickener, antifoaming agent, dispersion is added
0.5-1h, with the filter screen filtration of 300-800 mesh up to white finished product.
The present invention has the following advantages or advantageous effect：(1) it has synthesized to be stabilized in aqueous dispersion for the first time and not precipitate
Active nucleocapsid porous nano anion colloidal sol；(2) the corresponding spectrum and solar spectrum of the CdTe quantum selected are non-
Often matching, CdTe release luminous energy absorbed by Nano Titanium Oxide as Photocatalyst, increase its bactericidal effect, at the same improve bear from
The anion rate of release of sub- powder, the emulsion paint good anti-bacterial effect, without adding other antibacterials or mould proof auxiliary agent；(3) it selects
Two ester type coalescents of unsaturation while improving emulsion paint filming performance (not cracking), wherein the carbon-carbon double bond contained,
The crosslink density in silicone acrylic emulsion solidification later stage can be improved, and then improve the water resistance of emulsion paint；(4) it is prepared for porous structure
Nano-negative ion colloidal sol, due to its specific surface area bigger, effective content higher (highly basic removes a large amount of silica) and CdTe
Synergy is stronger, therefore the emulsion paint has the anion releasing effect of superelevation；(5) the polycarboxylic acids profit that the present invention is added
Slip grinding aid, in addition to containing-the COONa for generating double electrical layers in molecular structure, the also pentaerythritol with lubricant effect
Natural negative ion powder can be ground to Nano grade, to improve the integrated quality of finished product emulsion paint by monoester units；(6)
The two ester type coalescents of unsaturation that the present invention selects, first using butyl titanate as presoma, by the alcohol containing rosin
It is hydrolyzed in aqueous solution, the colloidal sol after hydrolysis is blended with itaconic acid, the catalytic esterification under p-methyl benzenesulfonic acid effect obtains insatiable hunger
It with diester colloidal sol, distributes it in dimethyl carbonate later, obtains ester dispersion liquid；Then triethanolamine is used to handle cellulose,
Again with stearic acid blending reaction, obtained fiber ester amine is blended with ester dispersion liquid, passes through the quaternary ammonium of ester amine and dimethyl carbonate
Change reaction, can not only improve dispersion compatibility of the cellulose between Organic Ingredients, enhance the film-formation result of ethyl cellulose,
It is blended with rosin, can improve film forming viscosity, enhances adhesive force intensity；And obtained quaternized products can be used as softness
Agent can play flexible, sterilization, yellowing-resistant and other effects, and to improve the quality of finished product, which also introduces titanium colloidal sol,
By modification, there is good compatibility with ester raw material, and it has good photocatalysis effect, it can be further
Improve bactericidal property.
Specific implementation mode
With reference to embodiment to a kind of emulsion paint for modifying nano-negative ion colloidal sol based on CdTe quantum of the present invention
It is further described.It is understood that specific embodiment described herein is used only for explaining related invention rather than right
The restriction of the invention.
Embodiment 1
A kind of emulsion paint for modifying nano-negative ion colloidal sol based on CdTe quantum, by weight, composition is as follows：CdTe amounts
80 parts of son point modification nano-negative ion colloidal sol, 350 parts of water, 5 parts of organosilicon aqueous dispersion, 1 part of phosphoric acid ester antifoaming agent, AP-
95 0.5 part of multifunctional assistants, unsaturated 10 parts of two ester type coalescents, 10 parts of propylene glycol, 80 parts of titanium dioxide, association type polyurethane
2 parts of thickener, 250 parts of silicone acrylic emulsion.
The CdTe quantum modifies nano-negative ion colloidal sol, there is following methods preparation：
(1) preparation of the porous nano anion colloidal sol of active nucleocapsid：The natural of mass fraction 14% is prepared first
Anion powder aqueous dispersions, then by above-mentioned dispersion liquid, account for the grinding aid of dispersion liquid total weight 0.2%, be added to nanometer and grind
Powder median (d is ground in grinding machine50) it is less than 100nm, it discharges up to nanoscale negative ion powder dispersion liquid；Take 50 parts by weight
Nanoscale negative ion powder dispersion liquid, 13 parts by weight 0.9mol/L potassium hydroxide solutions are added in reactor, are heated to 85 DEG C instead
Answer 8h, then through cooling, be filtered to remove solid or big grain size anion powder, fully dialysis remove potassium hydroxide be adjusted to pH be 8-
After 9, it is able to the dispersion liquid that porous nano negative ion powder is suspended matter, as porous nano anion colloidal sol；By 20 parts by weight matter
The ethanol solution for the tetraethyl titanate that amount score is 4% is added in reactor, and 22 parts by weight are added dropwise under stirring dropwise thereto
Porous nano anion colloidal sol, 1.5h are added dropwise, and continue to be stirred to react 1.5h, and it is shell, more to be able to active nano titanic oxide
Hole nanometer anion powder is the sol solutions A of core；
The grinding aid has following structure：
Preparation method is：(1) by 10 parts by weight of acrylic acid sodium, 5 parts by weight list acrylic acid pentaerythritol esters, 50 parts by weight
Deionized water stirs lower mixing, is heated to 90 DEG C, obtains mixed liquor a；(2) by the mistake of 3 parts by weight a concentration of 4% at 90 DEG C
Ammonium sulfate solution is added drop-wise to dropwise in mixed liquor a, the reaction was continued at 90 DEG C after being added dropwise 3h, obtains mixed liquor b；(3) stop
Only heat, 0.1 parts by weight chain terminating agent p-tert-Butylcatechol be added in mixed liquor b, stirs evenly, it is cooling to get to
Polycarboxylic acids lubricating type grinding aid.
(2) preparation of CdTe quantum colloidal sol：Under inert gas shielding, 0.22 parts by weight cadmium nitrate, 84 parts by weight are gone
Ionized water, 0.1 parts by weight 3- mercaptopropionic acid sodium be added in reactor and be stirred, it is 8-9 that potassium hydroxide tune pH, which is added, is added
0.15 parts by weight sodium hydrogen telluride, 92 DEG C are stirred to react 4h, obtain cadmium telluride quantum dot colloidal sol；
(3) CdTe quantum modifies nano-negative ion colloidal sol：Under the conditions of stirring at normal temperature, the sol solutions A into 42 parts by weight (1)
In, cadmium telluride quantum dot colloidal sol in 14 parts by weight (2) is added dropwise, 0.7h is added dropwise, and then proceedes to reaction 3h, obtains CdTe
Quantum dot modifies nano-negative ion colloidal sol, and CdTe quantum modification nano-negative ion colloidal sol places 30 days without heavy in volumetric flask
Drop.
The preparation method of the two ester type coalescents of unsaturation, includes the following steps；
(1) rosin of 2 parts by weight is taken, is heated and softened, is added in the diethylene glycol of 10 times of its weight, is kept the temperature at 60 DEG C
Stirring 10 minutes, obtains abienol liquid；
(2) butyl titanate for taking 20 parts by weight is added in above-mentioned abienol liquid, adds 45 parts by weight water, stirring 3 small
When, 25 parts by weight itaconic acids are added, it is 90 DEG C to increase temperature, and the p-methyl benzenesulfonic acid of 0.1 parts by weight is added, and insulated and stirred 1 is small
When, dehydration obtains ester colloidal sol；
(3) above-mentioned ester colloidal sol is taken, is added in the dimethyl carbonate of its weight 46%, stirs evenly, obtains ester dispersion liquid；
(4) ethyl cellulose of the triethanolamine of 10 parts by weight, 2 parts by weight is mixed, is added to 1.8 times of mixture weight
Absolute ethyl alcohol in, ultrasound 1 hour is distilled off ethyl alcohol, and the stearic acid of 20-22 parts by weight is added, stirs evenly, and is added 0.01
The p-methyl benzenesulfonic acid of parts by weight, it is 180 DEG C to increase temperature, is stirred to react 6 hours, is cooled to room temperature, obtains fiber ester amine；
(5) it takes above-mentioned ester dispersion liquid, fiber ester amine to be blended, stirs evenly, be sent in reaction kettle, be passed through nitrogen, adjust
Temperature of reaction kettle is 70 DEG C, is reacted 40 hours, discharging it is cooling to get；
The degree of substitution of the ethyl cellulose is 2.3；
The emulsion paint that nano-negative ion colloidal sol is modified based on CdTe quantum described in the present embodiment, by following methods system
It is standby：
Sequentially added in dispersion cylinder CdTe quantum modification nano-negative ion colloidal sol, water, organosilicon aqueous dispersion,
AP-95 multifunctional assistants, unsaturated two ester type coalescents, propylene glycol, keep dispersion machine to be rotated with 600rpm, fully dispersed
Then 20min will disperse disk center close to reactor bottom, and improve rotating speed to 1200rpm, then titanium dioxide is added in dispersion cylinder
Disperse 0.5h；Rotating speed is down to 800rpm, silicone acrylic emulsion, association type polyurethane thickener, phosphoric acid ester antifoaming agent, dispersion is added
0.5h, with the filter screen filtration of 300 mesh up to white finished product.
Embodiment 2
A kind of emulsion paint for modifying nano-negative ion colloidal sol based on CdTe quantum, by weight, composition is as follows：CdTe amounts
25 parts of son point modification nano-negative ion colloidal sol, 250 parts of water, 3 parts of polyocarboxy acid type anionic dispersing agents, silylated polyether class antifoaming agent 3
Part, 1 part of AP-95 multifunctional assistants, unsaturated 5 parts of two ester type coalescents, 5 parts of propylene glycol, 20 parts of titanium dioxide, modified alta-mud
3 parts of thickener, 80 parts of silicone acrylic emulsion.
The CdTe quantum modifies nano-negative ion colloidal sol, there is following methods preparation：
(1) preparation of the porous nano anion colloidal sol of active nucleocapsid：The natural of mass fraction 20% is prepared first
Anion powder aqueous dispersions, then by above-mentioned dispersion liquid, account for the grinding aid of dispersion liquid total weight 0.3%, be added to nanometer and grind
Powder median (d is ground in grinding machine50) it is less than 100nm, it discharges up to nanoscale negative ion powder dispersion liquid；Take 50 parts by weight
Nanoscale negative ion powder dispersion liquid, 20 parts by weight 0.6mol/L sodium hydroxide solutions are added in reactor, are heated to 95 DEG C instead
Answer 6h, then through cooling, be filtered to remove solid or big grain size anion powder, fully dialysis remove sodium hydroxide be adjusted to pH be 8-
After 9, it is able to the dispersion liquid that porous nano negative ion powder is suspended matter, as porous nano anion colloidal sol；By 20 parts by weight matter
The ethanol solution for the butyl titanate that amount score is 5% is added in reactor, and 25 parts by weight are added dropwise under stirring dropwise thereto
Porous nano anion colloidal sol, 2h are added dropwise, and continue to be stirred to react 2h, are able to active nano titanic oxide and are shell, porous receive
Rice negative ion powder is the sol solutions A of core；
The polycarboxylic acids lubricating type grinding aid has following structure：
Preparation method is：(1) by 20 parts by weight of acrylic acid sodium, 10 parts by weight list acrylic acid pentaerythritol esters, 100 weight
Part deionized water stirs lower mixing, is heated to 100 DEG C, obtains mixed liquor a；(2) by 5 parts by weight a concentration of 5% at 100 DEG C
Ammonium persulfate aqueous solution be added drop-wise to dropwise in mixed liquor a, the reaction was continued at 100 DEG C after being added dropwise 5h obtains mixed liquor b；
(3) stop heating, 0.2 parts by weight chain terminating agent p-tert-Butylcatechol is added in mixed liquor b, stirs evenly, it is cooling, i.e.,
Obtain polycarboxylic acids lubricating type grinding aid.
(2) preparation of CdTe quantum colloidal sol：Under inert gas shielding, by 0.3 parts by weight cadmium nitrate, 90 parts by weight go from
Sub- water, 0.2 parts by weight 3- thioacetic acid potassium be added in reactor and be stirred, it is 8 that sodium hydroxide tune pH, which is added, adds 0.2
Parts by weight sodium hydrogen telluride, 95 DEG C are stirred to react 3h, obtain cadmium telluride quantum dot colloidal sol；
(3) CdTe quantum modifies nano-negative ion colloidal sol：Under the conditions of stirring at normal temperature, the sol solutions A into 45 parts by weight (1)
In, cadmium telluride quantum dot colloidal sol in 20 parts by weight (2) is added dropwise, 1h is added dropwise, and then proceedes to reaction 4h, obtains CdTe amounts
Son point modification nano-negative ion colloidal sol, CdTe quantum modification nano-negative ion colloidal sol place 30 days without heavy in volumetric flask
Drop.
The preparation method of the two ester type coalescents of unsaturation, includes the following steps；
(1) rosin of 3 parts by weight is taken, is heated and softened, is added in the diethylene glycol of 16 times of its weight, is kept the temperature at 65 DEG C
Stirring 20 minutes, obtains abienol liquid；
(2) butyl titanate for taking 25 parts by weight is added in above-mentioned abienol liquid, adds 50 parts by weight water, stirring 4 small
When, 25-30 parts by weight itaconic acids are added, it is 96 DEG C to increase temperature, and the p-methyl benzenesulfonic acid of 0.2 parts by weight, insulated and stirred 2 is added
Hour, dehydration obtains ester colloidal sol；
(3) above-mentioned ester colloidal sol is taken, is added in the dimethyl carbonate of its weight 50%, stirs evenly, obtains ester dispersion liquid；
(4) ethyl cellulose of the triethanolamine of 14 parts by weight, 3 parts by weight is mixed, is added to 2 times of mixture weight
In absolute ethyl alcohol, ethyl alcohol is distilled off in ultrasound 2 hours, and the stearic acid of 22 parts by weight is added, stirs evenly, and 0.02 weight is added
The p-methyl benzenesulfonic acid of part, it is 185 DEG C to increase temperature, is stirred to react 7 hours, is cooled to room temperature, obtains fiber ester amine；
(5) it takes above-mentioned ester dispersion liquid, fiber ester amine to be blended, stirs evenly, be sent in reaction kettle, be passed through nitrogen, adjust
Temperature of reaction kettle is 76 DEG C, is reacted 46 hours, discharging it is cooling to get；
The degree of substitution of the ethyl cellulose is 2.5；
The emulsion paint that nano-negative ion colloidal sol is modified based on CdTe quantum described in the present embodiment, by following methods system
It is standby：
CdTe quantum modification nano-negative ion colloidal sol, water, polyocarboxy acid type anionic dispersant are sequentially added in dispersion cylinder
Agent, AP-95 multifunctional assistants, unsaturated two ester type coalescents, propylene glycol, are kept dispersion machine to be rotated with 500rpm, fully divided
24min is dissipated, then will disperse disk center close to reactor bottom, and improve rotating speed and dispersion cylinder is added to 900rpm, then by titanium dioxide
Middle dispersion 0.8h；Rotating speed is down to 700rpm, silicone acrylic emulsion, modified alta-mud thickener, silylated polyether class antifoaming agent is added, point
0.9h is dissipated, with the filter screen filtration of 500 mesh up to white finished product.
Embodiment 3
A kind of emulsion paint for modifying nano-negative ion colloidal sol based on CdTe quantum, by weight, composition is as follows：CdTe amounts
60 parts of son point modification nano-negative ion colloidal sol, 300 parts of water, 4 parts of nonionic polymer waterborne dispersant, acetylenic diols antifoaming agent
2 parts, it is 0.8 part of AP-95 multifunctional assistants, unsaturated 9 parts of two ester type coalescents, 8 parts of propylene glycol, 49 parts of titanium dioxide, modified fine
Plain 2.5 parts of the class thickener of dimension, 190 parts of silicone acrylic emulsion.
The CdTe quantum modifies nano-negative ion colloidal sol, there is following methods preparation：
(1) preparation of the porous nano anion colloidal sol of active nucleocapsid：The natural of mass fraction 10% is prepared first
Anion powder aqueous dispersions, then by above-mentioned dispersion liquid, account for the polyocarboxy acid type grinding aid of dispersion liquid total weight 0.1%, be added
To being ground to powder median (d in nano-level grinder50) it is less than 100nm, it discharges up to nanoscale negative ion powder dispersion liquid；It takes
50 parts by weight nanoscale negative ion powder dispersion liquids, 10 parts by weight 1.2mol/L sodium hydroxide solutions are added in reactor, heating
To 80 DEG C reaction 6h, then through cooling, be filtered to remove solid or big grain size anion powder, fully dialysis remove sodium hydroxide tune
After being 8-9 to pH, it is able to the dispersion liquid that porous nano negative ion powder is suspended matter, as porous nano anion colloidal sol；By 20
The ethanol solution for the metatitanic acid orthocarbonate that parts by weight mass fraction is 3% is added in reactor, is added dropwise dropwise thereto under stirring
20 parts by weight porous nano anion colloidal sols, 1h are added dropwise, continue to be stirred to react 1h, and being able to active nano titanic oxide is
Shell, the sol solutions A that porous nano negative ion powder is core；
The polycarboxylic acids lubricating type grinding aid has following structure：
Preparation method is：(1) by 15 parts by weight of acrylic acid sodium, 7 parts by weight list acrylic acid pentaerythritol esters, 70 parts by weight
Deionized water stirs lower mixing, is heated to 95 DEG C, obtains mixed liquor a；(2) by the mistake of 4 parts by weight a concentration of 4% at 96 DEG C
Ammonium sulfate solution is added drop-wise to dropwise in mixed liquor a, the reaction was continued at 93 DEG C after being added dropwise 4h, obtains mixed liquor b；(3) stop
Only heat, 0.13 parts by weight chain terminating agent p-tert-Butylcatechol be added in mixed liquor b, stirs evenly, it is cooling to get to
Polycarboxylic acids lubricating type grinding aid.
(2) preparation of CdTe quantum colloidal sol：Under inert gas shielding, by 0.2 parts by weight cadmium nitrate, 80 parts by weight go from
Sub- water, 0.15 parts by weight 3- mercaptobutyric acid sodium be added in reactor and be stirred, it is 9 that sodium hydroxide tune pH, which is added, adds 0.1
Parts by weight sodium hydrogen telluride, 90 DEG C are stirred to react 6h, obtain cadmium telluride quantum dot colloidal sol；
(3) CdTe quantum modifies nano-negative ion colloidal sol：Under the conditions of stirring at normal temperature, the sol solutions A into 40 parts by weight (1)
In, cadmium telluride quantum dot colloidal sol in 10 parts by weight (2) is added dropwise, 0.5h is added dropwise, and then proceedes to reaction 2h, obtains CdTe
Quantum dot modifies nano-negative ion colloidal sol, and CdTe quantum modification nano-negative ion colloidal sol places 30 days without heavy in volumetric flask
Drop.
The preparation method of the two ester type coalescents of unsaturation, includes the following steps；
(1) rosin of 2 parts by weight is taken, is heated and softened, is added in the diethylene glycol of 12 times of its weight, is kept the temperature at 62 DEG C
Stirring 13 minutes, obtains abienol liquid；
(2) butyl titanate for taking 22 parts by weight is added in above-mentioned abienol liquid, adds 47 parts by weight water, stirring 3 small
When, 28 parts by weight itaconic acids are added, it is 92 DEG C to increase temperature, and the p-methyl benzenesulfonic acid of 0.14 parts by weight is added, and insulated and stirred 1 is small
When, dehydration obtains ester colloidal sol；
(3) above-mentioned ester colloidal sol is taken, is added in the dimethyl carbonate of its weight 46-50%, stirs evenly, obtains ester dispersion
Liquid；
(4) ethyl cellulose of the triethanolamine of 12 parts by weight, 2 parts by weight is mixed, is added to 1.9 times of mixture weight
Absolute ethyl alcohol in, ultrasound 1 hour is distilled off ethyl alcohol, and the stearic acid of 21 parts by weight is added, stirs evenly, and 0.014 weight is added
The p-methyl benzenesulfonic acid of part is measured, it is 183 DEG C to increase temperature, is stirred to react 6 hours, is cooled to room temperature, obtains fiber ester amine；
(5) it takes above-mentioned ester dispersion liquid, fiber ester amine to be blended, stirs evenly, be sent in reaction kettle, be passed through nitrogen, adjust
Temperature of reaction kettle is 73 DEG C, is reacted 43 hours, discharging it is cooling to get；
The degree of substitution of the ethyl cellulose is 2.4；
The emulsion paint that nano-negative ion colloidal sol is modified based on CdTe quantum described in the present embodiment, by following methods system
It is standby：
CdTe quantum modification nano-negative ion colloidal sol, water, nonionic polymer waterborne are sequentially added in dispersion cylinder
Dispersant, AP-95 multifunctional assistants, unsaturated two ester type coalescents, propylene glycol, are kept dispersion machine to be rotated with 400rpm, filled
Then dispersion 30min will disperse disk center close to reactor bottom, and improve rotating speed and be added to 800rpmrpm, then by titanium dioxide
Disperse 1h in dispersion cylinder；Rotating speed is down to 600rpmrpm, silicone acrylic emulsion, modified cellulose class thickener, acetylenic diols are added and disappear
Infusion, dispersion dispersion 1h, with the filter screen filtration of 800 mesh up to white finished product.
By the emulsion paint and Fujian product for modifying nano-negative ion colloidal sol based on CdTe quantum of the embodiment of the present invention
Board anion release type white interior wall latex finishing coat (comparative example) imposes on metope under the same conditions, is examined under the same terms
It surveys, test data is as shown in the table：
Although the present invention has been explained in detail and has referred to embodiment, for those of ordinary skill in the art, show
Various schemes, modification and the change that can so make as specified above, should be construed as being included within the scope of the claims.
Claims (7)
1. a kind of emulsion paint for modifying nano-negative ion colloidal sol based on CdTe quantum, which is characterized in that described based on CdTe
Quantum dot modifies the emulsion paint of nano-negative ion colloidal sol, and by weight, composition is as follows：It is molten that CdTe quantum modifies nano-negative ion
25-80 parts of glue, 250-350 parts of water, 3-5 parts of wetting dispersing agent, 1-3 parts of antifoaming agent, 0.5-1 parts of AP-95 multifunctional assistants, insatiable hunger
With 5-10 parts of two ester type coalescents, 5-10 parts of propylene glycol, 2-3 parts of thickener, 80-250 parts of silicone acrylic emulsion；
Wherein, the CdTe quantum modifies nano-negative ion colloidal sol, is prepared by following methods：
(1) preparation of the porous nano anion colloidal sol of active nucleocapsid：The natural negative of mass fraction 10-20% is prepared first
Ion powder aqueous dispersions, then by above-mentioned natural negative ion powder aqueous dispersions, to account for natural negative ion powder aqueous dispersions total
The grinding aid of weight 0.1%-0.3% is added and is ground to powder median (d into nano-level grinder50) it is less than 100nm, go out
Expect up to nanoscale negative ion powder dispersion liquid；Take 50 parts by weight nanoscale negative ion powder dispersion liquids, 10-20 parts by weight 0.6-
1.2mol/L strong base solutions are added in reactor, be heated to 80-95 DEG C reaction 6-12h, then through cooling, be filtered to remove it is solid
Or it is suspended matter that big grain size anion powder, removing highly basic of fully dialysing, which are adjusted to pH after 8-9, to be able to porous nano negative ion powder,
Dispersion liquid, as porous nano anion colloidal sol；By the ethyl alcohol for the titanate coupling agent that 20 parts by weight mass fractions are 3-5%
Solution is added in reactor, and 20-25 parts by weight porous nano anion colloidal sols are added dropwise under stirring dropwise thereto, and 1-2h is added dropwise
It finishes, continues to be stirred to react 1-2h, it is shell, the sol solutions A that porous nano negative ion powder is core to be able to active nano titanic oxide；
(2) preparation of CdTe quantum colloidal sol：Under inert gas shielding, by 0.2-0.3 parts by weight cadmium nitrate, 80-90 parts by weight
Deionized water, 0.1-0.2 parts by weight stabilizer be added in reactor and be stirred, it is 8-9 that strong adjusting PH with base, which is added, adds 0.1-
0.2 parts by weight sodium hydrogen telluride, 90-95 DEG C is stirred to react 3-6h, obtains cadmium telluride quantum dot colloidal sol；
(3) CdTe quantum modifies nano-negative ion colloidal sol：Under the conditions of stirring at normal temperature, the sol solutions A into 40-45 parts by weight (1)
In, cadmium telluride quantum dot colloidal sol in 10-20 parts by weight (2) is added dropwise, 0.5-1h is added dropwise, and then proceedes to reaction 2-4h,
Obtain CdTe quantum modification nano-negative ion colloidal sol.
2. the emulsion paint according to claim 1 for modifying nano-negative ion colloidal sol based on CdTe quantum, which is characterized in that
The wetting dispersing agent is polyocarboxy acid type anionic dispersing agents, organosilicon aqueous dispersion, nonionic polymer waterborne point
At least one of powder；The antifoaming agent is preferably that organic silicon antifoaming agent, polyacrylic antifoaming agent, phosphoric acid ester disappear
At least one of infusion, silylated polyether class antifoaming agent, acetylenic diols antifoaming agent.
3. the emulsion paint according to claim 1 for modifying nano-negative ion colloidal sol based on CdTe quantum, which is characterized in that
The preparation method of the two ester type coalescents of unsaturation, includes the following steps；
(1) rosin of 2-3 parts by weight is taken, heats and softens, is added in the diethylene glycol of 10-16 times of its weight, at 60-65 DEG C
Insulated and stirred 10-20 minutes, obtains abienol liquid；
(2) butyl titanate for taking 20-25 parts by weight is added in above-mentioned abienol liquid, adds 45-50 parts by weight water, stirs 3-4
Hour, 25-30 parts by weight itaconic acids are added, it is 90-96 DEG C to increase temperature, and the p-methyl benzenesulfonic acid of 0.1-0.2 parts by weight is added,
Insulated and stirred 1-2 hours, dehydration, obtains ester colloidal sol；
(3) above-mentioned ester colloidal sol is taken, is added in the dimethyl carbonate of its weight 46-50%, stirs evenly, obtains ester dispersion liquid；
(4) ethyl cellulose of the triethanolamine of 10-14 parts by weight, 2-3 parts by weight is mixed, is added to mixture weight 1.8-
It is 1-2 hours ultrasonic in 2 times of absolute ethyl alcohol, ethyl alcohol is distilled off, the stearic acid of 20-22 parts by weight is added, stirs evenly, adds
Enter the p-methyl benzenesulfonic acid of 0.01-0.02 parts by weight, it is 180-185 DEG C to increase temperature, is stirred to react 6-7 hours, is cooled to often
Temperature obtains fiber ester amine；
(5) it takes above-mentioned ester dispersion liquid, fiber ester amine to be blended, stirs evenly, be sent in reaction kettle, be passed through nitrogen, adjust reaction
Kettle temperature degree be 70-76 DEG C, react 40-46 hour, discharging cool down to get；
The degree of substitution of the ethyl cellulose is 2.3-2.5；
It is poly- that the thickener is preferably modified cellulose class thickener, hydrophobically-modified alkali is swollen acrylic thickener, association type
At least one of urethane thickener, modified alta-mud thickener.
4. the emulsion paint according to claim 1 for modifying nano-negative ion colloidal sol based on CdTe quantum, which is characterized in that
The grinding aid is polycarboxylic acids lubricating type grinding aid；The highly basic is sodium hydroxide, potassium hydroxide, in barium hydroxide extremely
Few one kind；
The polycarboxylic acids lubricating type grinding aid has following structure：
Preparation method is：(1) by 10-20 parts by weight of acrylic acid sodium, 5-10 parts by weight list acrylic acid pentaerythritols ester, 50-100
Parts by weight of deionized water stirs lower mixing, is heated to 90-100 DEG C, obtains mixed liquor a；(2) by 3-5 weight at 90-100 DEG C
The ammonium persulfate aqueous solution of a concentration of 4-5% of part is added drop-wise to dropwise in mixed liquor a, and at 90-100 DEG C, the reaction was continued after being added dropwise
3-5h obtains mixed liquor b；(3) stop heating, 0.1-0.2 parts by weight chain terminating agent is added in mixed liquor b to tert-butyl o benzene
Diphenol stirs evenly, cooling to get to polycarboxylic acids lubricating type grinding aid.
5. the emulsion paint according to claim 1 for modifying nano-negative ion colloidal sol based on CdTe quantum, which is characterized in that
The titanate coupling agent is at least one of butyl titanate, tetraethyl titanate, metatitanic acid orthocarbonate.
6. the emulsion paint according to claim 1 for modifying nano-negative ion colloidal sol based on CdTe quantum, which is characterized in that
The stabilizer is sodium thioglycolate, 3- mercaptopropionic acids sodium, 3- thioacetic acid potassium, 3- mercaptobutyric acids potassium, 3- mercaptobutyric acid sodium
At least one of.
7. a kind of emulsion paint according to claim 1 for modifying nano-negative ion colloidal sol based on CdTe quantum, feature
It is, is prepared by following steps：
It is multi-functional that CdTe quantum modification nano-negative ion colloidal sol, water, wetting dispersing agent, AP-95 are sequentially added in dispersion cylinder
Auxiliary agent, unsaturated two ester type coalescents, propylene glycol, keep dispersion machine to be rotated with 400rpm-600rpm, fully dispersed 20-
Then 30min will disperse disk center close to reactor bottom, and improve rotating speed to 800rpm-1200rpm, silicone acrylic emulsion be added, increases
Thick dose, antifoaming agent disperse 0.5-1h, with the filter screen filtration of 300-800 mesh up to white finished product.
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