CN106046273B - A kind of associative thickening vac-veova emulsion and preparation method thereof - Google Patents
A kind of associative thickening vac-veova emulsion and preparation method thereof Download PDFInfo
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- CN106046273B CN106046273B CN201610673902.0A CN201610673902A CN106046273B CN 106046273 B CN106046273 B CN 106046273B CN 201610673902 A CN201610673902 A CN 201610673902A CN 106046273 B CN106046273 B CN 106046273B
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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
- C08F283/00—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G
- C08F283/06—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals
- C08F283/065—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polyethers, polyoxymethylenes or polyacetals on to unsaturated polyethers, polyoxymethylenes or polyacetals
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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
- C08F218/00—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 an acyloxy radical of a saturated carboxylic acid, of carbonic acid or of a haloformic acid
- C08F218/02—Esters of monocarboxylic acids
- C08F218/04—Vinyl esters
- C08F218/08—Vinyl acetate
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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
- C09D131/00—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 an acyloxy radical of a saturated carboxylic acid, of carbonic acid, or of a haloformic acid; Coating compositions based on derivatives of such polymers
- C09D131/02—Homopolymers or copolymers of esters of monocarboxylic acids
- C09D131/04—Homopolymers or copolymers of vinyl acetate
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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
- C09D151/00—Coating compositions based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Coating compositions based on derivatives of such polymers
- C09D151/08—Coating compositions based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Coating compositions based on derivatives of such polymers grafted on to macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
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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
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Abstract
The invention discloses a kind of associative thickening vac-veova emulsions and preparation method thereof, belong to building coating research and development technology field, it include each component of following mass percentage: water 40-50% in the vac-veova emulsion, emulsifier 1-3%, vinylacetate 30-40%, butyl acrylate 5-15%, tertiary carbonic ester VV-10 5-15%, acrylic acid 0-1%, associative thickening monomer 1-20%, persulfate 0.5-2%.It include: that a part of water and emulsifier and remaining component in addition to persulfate are subjected to pre-emulsification in this method step；A part of persulfate is dissolved with water；The water of remainder amount, which is added with emulsifier into reaction kettle, to be put into emulsion as seed again and reacts；The persulfate of a part of surplus is added, while remaining persulfate and emulsion, temperature control heat preservation is added dropwise；It post-processes to obtain the final product.Vac-veova emulsion produced by the present invention is capable of forming finer and close association networks, effectively improves high cut and paste degree in coating.
Description
Technical field
The invention belongs to building coating research and development technology field, it is related to a kind of associative thickening vac-veova emulsion and preparation method thereof.
Background technique
For a long time, improving high cut and paste degree, balance levelling and sagging is always the insoluble problem of building coating, this is straight
Connect the application property for being related to coating.General lotion can not form firm associative thickening network structure in coating system, in height
It is easy to be destroyed rapidly under shear rate, viscosity declines rapidly, is unfavorable for the construction of water based paint, easy sagging.It is asked to solve this
Topic would generally be by the way of increasing thickener additive amount, but this mode will cause low cut and paste again and spend height, be unfavorable for coating
Levelling.In addition, excessive thickener gives whole coating products to introduce other small molecule substances, to other property of paint film again
Can, such as scrubbing resistance and water-fast can have a negative impact.Therefore, how thickening efficiency is improved, effectively improves height in coating and cuts
The relationship of viscosity, balance levelling and sagging is current urgent problem to be solved.
Summary of the invention
In order to solve the above-mentioned technical problem the present invention, devises a kind of associative thickening vac-veova emulsion and preparation method thereof, this
Lotion prepared by preparation method can efficiently carry out thickening response with thickener, form finer and close association network knot
Structure effectively improves high cut and paste degree in coating, be easy to construct etc..
The technical solution adopted by the present invention is that: a kind of associative thickening vac-veova emulsion, key are: in the vac-veova emulsion
Each component including following mass percentage:
Wherein, the emulsifier be sodium vinyl sulfonate,3- allyloxy -2- hydroxyl -1- propane sulfonic acid sodium saltOr allyl
Base polyoxyethylene ether ammonium sulfate any of them or two or more mixtures.
Wherein, the associative thickening monomer is any one in CBH, BEM or SEM or two or more mixtures.
Preferably, the mass percentage of the associative thickening monomer is 3-10%.
It is further preferred that the mass percentage of the associative thickening monomer is 2-5%.
Wherein, the persulfate be ammonium persulfate, potassium peroxydisulfate or sodium peroxydisulfate any of them or two kinds with
On mixture.
A kind of preparation method of associative thickening vac-veova emulsion as described above, it is characterised in that: include: in this method step
(1) water of 1/3-1/2 and emulsifier are placed in a beaker stirring, add vinylacetate, butyl acrylate, third
Olefin(e) acid, tertiary carbonic ester VV-10 and associative thickening monomer carry out pre-emulsification, emulsification times 15-25 minutes, are configured to emulsion, standby
With；
(2) persulfate of 1/3-1/2 is sufficiently dissolved with water, it is spare；
(3) water and emulsifier for taking surplus are added into reaction kettle, are heated to 80-84 DEG C, to temperature be stable at 80 DEG C-
Emulsion obtained by the step of mass percent is 3%-5% (1) is put into after 84 DEG C to be reacted as seed；
(4) persulfate of 1/3-1/2 surplus is added after 3-10 minutes into reaction kettle, sufficiently reaction 18-25 minutes；
(5) remaining persulfate and remaining emulsion are added dropwise simultaneously, time for adding is 2-3 hours；
(6) after completion of dropwise addition, controlled at 84 DEG C -86 DEG C, 1-2 hours are kept the temperature；
(7) after keeping the temperature, controlled at 70 DEG C to 65 DEG C, tert-butyl hydroperoxide and L-AA are added,
It discharges after cooling, filtering.
Preferably, the emulsification times in step (1) are 20 minutes.
Preferably, in step (4), the persulfate of 1/3-1/2 surplus is added after five minutes into reaction kettle, it is sufficiently anti-
It answers 20 minutes.
The beneficial effects of the present invention are: the 1, present invention is crucial to joined associative thickening list in the synthesizing formula of vac-veova emulsion
Body can not only form chain hydrophobic association unit with tertiary carbonic ester, improve lotion thickening efficiency and water resistance；It can also apply
Association tridimensional network is formed in material with thickener, the group of special construction can adsorb pigments and fillers particle again at the same time,
Enhance associative structure.On the other hand, there is no as conventional polymerization process, hydroxylated cellulose is added, and introduces hydrophobic association
Monomer, so that the selection of thickener is more extensive in final formulation for coating material, and other thickeners have preferable compatibility.
It is polymerisable emulsifier used in the present invention, the reactivity of vinylacetate can be improved, significantly improve vinyl acetate
The monomer conversion of ester improves the comprehensive performance of lotion.It 2, can be with using vac-veova emulsion obtained by preparation method of the present invention
Thickener efficiently carries out thickening response, forms finer and close association networks, effectively improves high cut and paste degree in coating,
Make final product that there is unique rheological property, be easy to construct etc..
Specific embodiment
The following describes the present invention in detail with reference to examples.
Embodiment 1:
Vinylacetate 32% (weight percent, similarly hereinafter), butyl acrylate 10%, tertiary carbonic ester 6%, acrylic acid
0.2%, allyl polyethenoxy ether ammonium sulfate 2%, ammonium persulfate 1.8%, associative thickening monomer CBH 3%, water 45%.
Embodiment 2:
Vinylacetate 38% (weight percent, similarly hereinafter), butyl acrylate 5%, tertiary carbonic ester 7%, acrylic acid
0.2%, sodium vinyl sulfonate 2%, ammonium persulfate 1.8%, associative thickening monomer BEM 1%, water 45%.
Embodiment 3:
Vinylacetate 30% (weight percent, similarly hereinafter), butyl acrylate 10%, tertiary carbonic ester 10%, acrylic acid
0.2%, sodium vinyl sulfonate 1.5%,3- allyloxy -2- hydroxyl -1- propane sulfonic acid sodium salt0.5%, potassium peroxydisulfate 1.3% is formed
Close thickening monomer SEM 1.5%, water 45%.
Embodiment 4:
Vinylacetate 40% (weight percent, similarly hereinafter), butyl acrylate 5%, tertiary carbonic ester 5%, acrylic acid
0.5%, sodium vinyl sulfonate 1.5%, potassium peroxydisulfate 1.5%, associative thickening monomer CD559 1%, associative thickening monomer BEM
5%, water 45%.
Embodiment 5:
Vinylacetate 33% (weight percent, similarly hereinafter), butyl acrylate 8%, tertiary carbonic ester 5%, acrylic acid
0.5%, sodium vinyl sulfonate 3%, sodium peroxydisulfate 2.5%, associative thickening monomer BEM 1.5%, associative thickening monomer SEM
1.5%, water 45%.
After above-mentioned each way of example feeding, with the preparation of following preparation methods:
(1) water of 1/3-1/2 and emulsifier are placed in a beaker stirring, add vinylacetate, butyl acrylate, third
Olefin(e) acid, tertiary carbonic ester VV-10 and associative thickening monomer carry out pre-emulsification, emulsification times 20 minutes, are configured to emulsion, spare；
(2) persulfate of 1/3-1/2 is sufficiently dissolved with water, it is spare；
(3) water and emulsifier for taking surplus are added into reaction kettle, are heated to 82 DEG C, after temperature is stable at 82 DEG C
Emulsion obtained by the step of disposably investment mass percent is 3%-5% after five minutes (1) is reacted as seed；
(4) persulfate of 1/3-1/2 surplus is added after five minutes into reaction kettle, sufficiently reaction 20 minutes；
(5) after reaction, while remaining persulfate and remaining emulsion is added dropwise in seed, and time for adding is 3 small
When；
(6) after completion of dropwise addition, controlled at 84 DEG C -86 DEG C, 1 hour is kept the temperature；
(7) after keeping the temperature, controlled at 70 DEG C to 65 DEG C, tert-butyl hydroperoxide and L-AA are added,
It discharges after cooling, filtering.
The vac-veova emulsion that above-mentioned several examples are allotted is equipped with coating by table 1, and compared with prior art, lotion can be more effective
Rate it is corresponding to thickener progress, form fine and close associative thickening network structure, improve the service efficiency of thickener, effectively improve painting
High cut and paste degree in material is easy to construct (table 2).
Table 1
Table 2
| Embodiment 1 | Embodiment 2 | Embodiment 3 | Embodiment 4 | Embodiment 5 | Competing product | |
| Middle cut and paste degree (KU) | 109 | 112 | 115 | 110 | 113 | 90 |
| High cut and paste degree (mpas) | 285 | 288 | 293 | 290 | 291 | 248 |
| Application property | ★★★★ | ★★★★★ | ★★★★★ | ★★★★ | ★★★★★ | ★★★ |
| It is water-fast | It is unchanged | It is unchanged | It is unchanged | It is unchanged | It is unchanged | Blistering |
| Scrubbing resistance | > 10000 | > 10000 | 8500 | 8000 | 9000 | 3500 |
Claims (6)
1. a kind of preparation method of associative thickening vac-veova emulsion, it is characterised in that: include following quality in the vac-veova emulsion
The each component of percentage composition:
The associative thickening monomer is the mixture of any one or two kinds in BEM or SEM；
Include: in this method step
(1) water of 1/3-1/2 and emulsifier are placed in a beaker stirring, add vinylacetate, butyl acrylate, propylene
Acid, tertiary carbonic ester VV-10 and associative thickening monomer carry out pre-emulsification, emulsification times 15-25 minutes, are configured to emulsion, spare；
(2) persulfate of 1/3-1/2 is sufficiently dissolved with water, it is spare；
(3) water and emulsifier for taking surplus are added into reaction kettle, are heated to 80-84 DEG C, are stable at 80 DEG C -84 DEG C to temperature
Emulsion obtained by the step of investment mass percent is 3%-5% afterwards (1) is reacted as seed；
(4) persulfate of 1/3-1/2 surplus is added after 3-10 minutes into reaction kettle, sufficiently reaction 18-25 minutes；
(5) remaining persulfate and remaining emulsion are added dropwise simultaneously, time for adding is 2-3 hours；
(6) after completion of dropwise addition, controlled at 84 DEG C -86 DEG C, 1-2 hours are kept the temperature；
(7) after keeping the temperature, controlled at 70 DEG C to 65 DEG C, tert-butyl hydroperoxide and L-AA are added, cool down,
It discharges after filtering.
2. a kind of preparation method of associative thickening vac-veova emulsion according to claim 1, it is characterised in that: the emulsification
Agent is that sodium vinyl sulfonate, 3- allyloxy -2- hydroxyl -1- propane sulfonic acid sodium salt or allyl polyethenoxy ether ammonium sulfate are wherein appointed
The mixture for one or more of anticipating.
3. a kind of preparation method of associative thickening vac-veova emulsion according to claim 1, it is characterised in that: the association
The mass percentage for thickening monomer is 3-10%.
4. a kind of preparation method of associative thickening vac-veova emulsion according to claim 1, it is characterised in that: the over cure
Hydrochlorate is ammonium persulfate, potassium peroxydisulfate or sodium peroxydisulfate any of them or two or more mixtures.
5. a kind of preparation method of associative thickening vac-veova emulsion according to claim 1, it is characterised in that: in step (1)
Emulsification times be 20 minutes.
6. a kind of preparation method of associative thickening vac-veova emulsion according to claim 1, it is characterised in that: in step (4),
The persulfate of 1/3-1/2 surplus is added after five minutes into reaction kettle, sufficiently reaction 20 minutes.
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Denomination of invention: Associative thickened vinegar tert lotion and its preparation method Effective date of registration: 20230506 Granted publication date: 20190212 Pledgee: Agricultural Bank of China Limited Nanxiong Sub branch Pledgor: GUANGDONG HENGGUANG NEW MATERIAL TECHNOLOGY CO.,LTD. Registration number: Y2023980039881 |