CN116376415A - Preparation method of wall paint with strong antibacterial and anti-stain effects - Google Patents
Preparation method of wall paint with strong antibacterial and anti-stain effects Download PDFInfo
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- CN116376415A CN116376415A CN202310290506.XA CN202310290506A CN116376415A CN 116376415 A CN116376415 A CN 116376415A CN 202310290506 A CN202310290506 A CN 202310290506A CN 116376415 A CN116376415 A CN 116376415A
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- wall paint
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- 239000003973 paint Substances 0.000 title claims abstract description 41
- 230000000844 anti-bacterial effect Effects 0.000 title claims abstract description 24
- 230000000694 effects Effects 0.000 title claims abstract description 19
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 239000000839 emulsion Substances 0.000 claims abstract description 77
- 229920001661 Chitosan Polymers 0.000 claims abstract description 57
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims abstract description 45
- NIXOWILDQLNWCW-UHFFFAOYSA-N acrylic acid group Chemical group C(C=C)(=O)O NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims abstract description 38
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 36
- 239000004814 polyurethane Substances 0.000 claims abstract description 34
- 229920002635 polyurethane Polymers 0.000 claims abstract description 34
- 238000002156 mixing Methods 0.000 claims abstract description 25
- -1 polysiloxane Polymers 0.000 claims abstract description 20
- 229920001296 polysiloxane Polymers 0.000 claims abstract description 19
- 229920005906 polyester polyol Polymers 0.000 claims abstract description 15
- VVQNEPGJFQJSBK-UHFFFAOYSA-N Methyl methacrylate Chemical compound COC(=O)C(C)=C VVQNEPGJFQJSBK-UHFFFAOYSA-N 0.000 claims abstract description 11
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims abstract description 11
- 229920002554 vinyl polymer Polymers 0.000 claims abstract description 11
- 230000004048 modification Effects 0.000 claims abstract description 10
- 238000012986 modification Methods 0.000 claims abstract description 10
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 8
- 230000002194 synthesizing effect Effects 0.000 claims abstract description 3
- 238000003756 stirring Methods 0.000 claims description 67
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 claims description 42
- 238000006243 chemical reaction Methods 0.000 claims description 29
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 26
- 238000010438 heat treatment Methods 0.000 claims description 26
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 claims description 24
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 24
- 238000001035 drying Methods 0.000 claims description 20
- 239000007788 liquid Substances 0.000 claims description 20
- 239000003995 emulsifying agent Substances 0.000 claims description 19
- 239000003999 initiator Substances 0.000 claims description 17
- 239000000203 mixture Substances 0.000 claims description 15
- 239000002243 precursor Substances 0.000 claims description 14
- 238000000498 ball milling Methods 0.000 claims description 12
- 239000008367 deionised water Substances 0.000 claims description 12
- 229910021641 deionized water Inorganic materials 0.000 claims description 12
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 claims description 12
- 229920000909 polytetrahydrofuran Polymers 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 10
- 230000001804 emulsifying effect Effects 0.000 claims description 10
- 238000003825 pressing Methods 0.000 claims description 10
- 238000005086 pumping Methods 0.000 claims description 10
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims description 9
- 238000004321 preservation Methods 0.000 claims description 9
- 238000000034 method Methods 0.000 claims description 8
- JVYDLYGCSIHCMR-UHFFFAOYSA-N 2,2-bis(hydroxymethyl)butanoic acid Chemical compound CCC(CO)(CO)C(O)=O JVYDLYGCSIHCMR-UHFFFAOYSA-N 0.000 claims description 7
- 239000005058 Isophorone diisocyanate Substances 0.000 claims description 7
- 235000019441 ethanol Nutrition 0.000 claims description 7
- NIMLQBUJDJZYEJ-UHFFFAOYSA-N isophorone diisocyanate Chemical compound CC1(C)CC(N=C=O)CC(C)(CN=C=O)C1 NIMLQBUJDJZYEJ-UHFFFAOYSA-N 0.000 claims description 7
- 238000000926 separation method Methods 0.000 claims description 7
- 238000005406 washing Methods 0.000 claims description 7
- 239000002518 antifoaming agent Substances 0.000 claims description 5
- 230000015572 biosynthetic process Effects 0.000 claims description 5
- 239000003795 chemical substances by application Substances 0.000 claims description 5
- 210000000078 claw Anatomy 0.000 claims description 5
- 238000007599 discharging Methods 0.000 claims description 5
- 239000000706 filtrate Substances 0.000 claims description 5
- 238000003786 synthesis reaction Methods 0.000 claims description 5
- 239000002562 thickening agent Substances 0.000 claims description 5
- 239000002918 waste heat Substances 0.000 claims description 5
- 239000000654 additive Substances 0.000 claims description 3
- 230000000996 additive effect Effects 0.000 claims description 3
- 238000004945 emulsification Methods 0.000 claims description 2
- 238000011049 filling Methods 0.000 claims description 2
- 230000001105 regulatory effect Effects 0.000 claims description 2
- 239000000853 adhesive Substances 0.000 abstract description 3
- 230000001070 adhesive effect Effects 0.000 abstract description 3
- 239000011248 coating agent Substances 0.000 abstract description 2
- 238000000576 coating method Methods 0.000 abstract description 2
- 239000000126 substance Substances 0.000 description 13
- 239000000463 material Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 238000011068 loading method Methods 0.000 description 3
- 241000894006 Bacteria Species 0.000 description 1
- 239000003242 anti bacterial agent Substances 0.000 description 1
- 230000000845 anti-microbial effect Effects 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000004744 fabric Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 230000003389 potentiating effect Effects 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
- 239000004332 silver Substances 0.000 description 1
Images
Classifications
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- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F26—DRYING
- F26B—DRYING SOLID MATERIALS OR OBJECTS BY REMOVING LIQUID THEREFROM
- F26B23/00—Heating arrangements
- F26B23/001—Heating arrangements using waste heat
-
- 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
- C08F283/12—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polysiloxanes
- C08F283/124—Macromolecular compounds obtained by polymerising monomers on to polymers provided for in subclass C08G on to polysiloxanes on to polysiloxanes having carbon-to-carbon double bonds
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/30—Low-molecular-weight compounds
- C08G18/34—Carboxylic acids; Esters thereof with monohydroxyl compounds
- C08G18/348—Hydroxycarboxylic acids
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/42—Polycondensates having carboxylic or carbonic ester groups in the main chain
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/48—Polyethers
- C08G18/4854—Polyethers containing oxyalkylene groups having four carbon atoms in the alkylene group
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/40—High-molecular-weight compounds
- C08G18/64—Macromolecular compounds not provided for by groups C08G18/42 - C08G18/63
- C08G18/6484—Polysaccharides and derivatives thereof
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/28—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
- C08G18/65—Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
- C08G18/66—Compounds of groups C08G18/42, C08G18/48, or C08G18/52
- C08G18/6625—Compounds of groups C08G18/42, C08G18/48, or C08G18/52 with compounds of group C08G18/34
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/74—Polyisocyanates or polyisothiocyanates cyclic
- C08G18/75—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic
- C08G18/751—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring
- C08G18/752—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group
- C08G18/753—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group
- C08G18/755—Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group and at least one isocyanate or isothiocyanate group linked to a secondary carbon atom of the cycloaliphatic ring, e.g. isophorone diisocyanate
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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
- C09D151/085—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 on to polysiloxanes
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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
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
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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
- C09D5/14—Paints containing biocides, e.g. fungicides, insecticides or pesticides
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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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
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Abstract
The invention provides a preparation method of a wall paint with strong antibacterial and anti-stain effects. The preparation method of the wall paint with strong antibacterial and anti-stain effects comprises the following steps: citric acid acidifying chitosan, synthesizing polyurethane by using polyester polyol, adding the acidified chitosan for modification, preparing modified acrylic emulsion by using polysiloxane, and adding other auxiliary agents for mixing. According to the invention, the modified acrylic emulsion is prepared by mixing polysiloxane with active vinyl, methyl methacrylate and the like, and then the modified acrylic emulsion is mixed with the aqueous polyurethane emulsion to prepare the wall paint, so that the wall paint has a compact coating structure, and has better stain resistance, water resistance, weather resistance and stronger adhesive force.
Description
Technical Field
The invention relates to the technical field of paint, in particular to a preparation method of a wall paint with strong antibacterial and anti-stain effects.
Background
The wall paint is one of main decorative materials for the wall in the home decoration, the water-based polyurethane is widely applied to the fields of paint, adhesives, fabrics and the like due to the excellent physical and chemical properties of the water-based polyurethane, and can be used for preparing the wall paint, however, the water-based polyurethane is poor in water resistance and easy to generate bacteria, and the antibacterial property of the wall paint is usually enhanced by adding an organic antibacterial agent, silver ions or nano metals and the like at present, but the antibacterial wall paint prepared in the mode is insufficient in durability, stain resistance and safety.
The information disclosed in this background section is only for enhancement of understanding of the general background of the invention and should not be taken as an acknowledgement or any form of suggestion that this information forms the prior art already known to a person of ordinary skill in the art.
Disclosure of Invention
Aiming at the defects existing in the prior art, the invention aims to provide a preparation method of a wall paint with strong antibacterial and anti-stain effects.
A preparation method of a wall paint with strong antibacterial and anti-stain effects comprises the following steps:
s1: citric acid acidified chitosan
Adding citric acid and chitosan into an ethanol solution, stirring for reaction, performing centrifugal separation, and then washing and drying to obtain acidified chitosan;
s2: synthesis of polyurethane from polyester polyol
Under the high temperature condition, polytetrahydrofuran ether glycol, polyester polyol, isophorone diisocyanate and dimethylolbutyric acid are mixed for reaction to obtain a precursor;
s3: adding acidified chitosan for modification
Adding the acidified chitosan into the precursor, performing ball milling, performing heat preservation reaction, adding triethylamine to adjust the PH, and adding deionized water to emulsify to obtain chitosan modified polyurethane emulsion;
s4: preparation of modified acrylic emulsion with polysiloxane
Mixing methyl methacrylate, methacrylic acid, polysiloxane with active vinyl and an emulsifier, adding water for emulsification, and then adding an initiator for reaction to obtain modified acrylic emulsion;
s5: adding other auxiliary agents for mixing
Adding a defoaming agent, a leveling agent and a thickening agent into the chitosan modified polyurethane emulsion, stirring for 2-3 hours at the speed of 1200-1500r/min, uniformly mixing, adding a film forming additive and the modified acrylic emulsion, and continuously stirring for 1-1.5 hours at the speed of 800-1000r/min to obtain the wall paint.
Further, the citric acid-acidified chitosan of the step S1 specifically includes the following steps:
s1.1: adding citric acid and chitosan together into a reaction tank containing ethanol solution according to a molar ratio of 2-5:1, stirring for 0.5-1h, and reacting to obtain a solid-liquid mixture;
s1.2: starting a pressurizing pump, pressing the solid-liquid mixture into a centrifugal separator through a slide pipe, centrifuging the solid-liquid mixture for 15-30min at a speed of 5000-8000r/min by the centrifugal separator, performing solid-liquid separation, and discharging filtrate to obtain filter residues;
s1.3: washing the filter residue for 2-5 times by using absolute ethyl alcohol, and then placing the washed filter residue into a drying box for drying to obtain the acidified chitosan.
Further, the step S2 of synthesizing polyurethane by using polyester polyol specifically comprises the following steps:
s2.1: vacuum dehydrating polytetrahydrofuran ether glycol, adding the polytetrahydrofuran ether glycol and polyester polyol into a stirrer together according to the molar ratio of 1:2-3, heating to 50-70 ℃, stirring and mixing;
s2.2: adding isophorone diisocyanate into a stirrer, stirring uniformly, heating to 80-90 ℃, and reacting for 2-3h under heat preservation;
s2.3: adding the dimethylolbutyric acid into a stirrer, stirring at the speed of 200-300r/min for 1-2h, and performing chain extension reaction to obtain a precursor.
Further, the step S3 of adding the acidified chitosan for modification specifically comprises the following steps:
s3.1: adding the acidified chitosan into the precursor, ball-milling for 30-40min at a speed of 800-1200rpm by using a ball-milling device in a stirrer, keeping the temperature in the stirrer at 80-90 ℃, and continuing to react for 2-5h;
s3.2: regulating the temperature to 40-60 ℃, pumping triethylamine into a stirrer by using a hydraulic pump, stirring the triethylamine until a PH detector in the stirrer detects PH=7-8, stopping pumping the triethylamine, stopping stirring, standing and cooling to room temperature;
s3.3: and filling deionized water into a hydraulic pump of the stirrer, pressing the deionized water into the stirrer from small holes on stirring claws by the hydraulic pump, stirring at the same time, and emulsifying to obtain the chitosan modified polyurethane emulsion.
Further, the step S4 of preparing the modified acrylic emulsion by polysiloxane specifically comprises the following steps:
s4.1: adding methyl methacrylate, methacrylic acid, polysiloxane with active vinyl and an emulsifying agent into an emulsifying cylinder, adding water, and uniformly stirring to obtain a pre-emulsion;
s4.2: placing 1/5 of the pre-emulsion into a reactor, adding 1/3 of an initiator, uniformly stirring, heating to 60-70 ℃, and reacting for 1-2h;
s4.3: adding the residual pre-emulsion into a reactor, adding 1/2 of the residual initiator, heating to 70-80 ℃, and reacting for 2-3h;
s4.4: and adding all the rest initiator into the reactor, stirring for 40-50min, simultaneously carrying out heat preservation reaction, and cooling to room temperature to obtain the modified acrylic emulsion.
Further, the drying box is arranged on the inner wall of the reactor in the step S4.2, when the temperature in the reactor is raised for reaction, the temperature in the drying box is raised through the waste heat in the reactor, and the washed filter residues are dried.
Further, the emulsifier is prepared by mixing a T-02 emulsifier and an SDS emulsifier according to a volume ratio of 1-3:1.
Further, the volume ratio of the methyl methacrylate, the methacrylic acid and the polysiloxane with the active vinyl is 5-10:2-5:1.
Compared with the prior art, the invention has the advantages that:
1. according to the invention, the modified acrylic emulsion is prepared by mixing polysiloxane with active vinyl, methyl methacrylate and the like, and then the modified acrylic emulsion is mixed with the aqueous polyurethane emulsion to prepare the wall paint, so that the wall paint has a compact coating structure, and has better stain resistance, water resistance, weather resistance and stronger adhesive force.
2. According to the invention, the chitosan is acidified by citric acid to improve the water solubility of the chitosan, the polyurethane is modified by the acidified chitosan, and the wall paint prepared by taking the modified polyurethane emulsion as a raw material has strong antibacterial property, and is environment-friendly and pollution-free.
3. According to the invention, the residual heat generated during the reaction is utilized to heat the drying box, so that the filter residues are dried, the effect of fully and effectively utilizing resources is achieved, and the preparation time can be saved.
Drawings
FIG. 1 is a flow chart of a method for preparing a wall paint with potent antimicrobial and stain resistance used in an embodiment of the present invention.
Detailed Description
The present invention will be described in further detail with reference to specific examples.
Example 1
A preparation method of a wall paint with strong antibacterial and anti-stain effects is shown in figure 1, and comprises the following steps:
s1: citric acid acidified chitosan
Adding citric acid produced by the dry and Yao technology Co., ltd and chitosan produced by the Wuhan Ji chemical Co., ltd into a reaction tank containing ethanol solution according to a molar ratio of 2:1, stirring for 0.5h, reacting to obtain a solid-liquid mixture, starting a booster pump, pressing the solid-liquid mixture into a centrifugal separator through a slide tube, centrifuging the solid-liquid mixture at a speed of 5000r/min for 15min by the centrifugal separator, performing solid-liquid separation, discharging filtrate to obtain filter residues, washing the filter residues for 2 times by absolute ethanol, and then drying the washed filter residues in a drying box to obtain acidified chitosan;
s2: synthesis of polyurethane from polyester polyol
Vacuum dehydrating polytetrahydrofuran ether glycol produced by Jinan Guangyu chemical industry Co., ltd, adding the polytetrahydrofuran ether glycol and polyester polyol produced by Shandong Shuixin new material science and technology Co., ltd together in a molar ratio of 1:2 into a stirrer, heating to 50 ℃, stirring and mixing, adding isophorone diisocyanate produced by Hubei Chengfeng chemical industry Co., ltd into the stirrer, stirring uniformly, heating to 80 ℃, carrying out heat preservation and reaction for 2 hours, adding dimethylolbutyric acid produced by Cheng Mojia new material Co., ltd into the stirrer, stirring for 1 hour at a speed of 200r/min, and carrying out chain extension reaction to obtain a precursor;
s3: adding acidified chitosan for modification
Adding the acidified chitosan into the precursor, ball-milling for 30min at the speed of 800rpm by using a ball milling device in a stirrer, keeping the temperature in the stirrer at 80 ℃, continuously reacting for 2h, adjusting the temperature to 40 ℃, pumping triethylamine into the stirrer by using a hydraulic pump, stirring simultaneously until PH=7 is detected by a PH detector in the stirrer, stopping pumping triethylamine, stopping stirring, standing and cooling to room temperature, loading deionized water into the hydraulic pump of the stirrer, pressing the deionized water into the stirrer from small holes on stirring claws by using the hydraulic pump, stirring simultaneously, emulsifying to obtain chitosan modified polyurethane emulsion, modifying polyurethane by using the acidified chitosan, and preparing wall paint by using the modified polyurethane emulsion as a raw material, wherein the wall paint has strong antibacterial property, is green and environment-friendly;
s4: preparation of modified acrylic emulsion with polysiloxane
Adding methyl methacrylate produced by Jinan Runtai chemical industry Co., ltd, methacrylic acid produced by Shandong Mao national trade Co., ltd, active vinyl polysiloxane produced by Wuhan Hana white pharmaceutical chemical industry Co., ltd and an emulsifier prepared by mixing a T-02 emulsifier and an SDS emulsifier according to a volume ratio of 1:1 into an emulsifying tank together, adding water, stirring uniformly to obtain a pre-emulsion, then taking 1/5 of the pre-emulsion, placing the pre-emulsion into a reactor, adding 1/3 of an initiator, stirring uniformly, heating to 60 ℃, reacting for 1h, adding the rest of the pre-emulsion, adding 1/2 of the rest of the initiator, heating to 70 ℃, reacting for 2h, heating the drying tank by using waste heat in the reactor while heating reaction, finally adding the rest of the initiator into the reactor, stirring for 40min, cooling to room temperature, obtaining modified acrylic acid, preparing a modified acrylic acid emulsion with good weather resistance, and a high water resistance, and a modified acrylic acid emulsion, and a high weather resistance, and a modified acrylic acid emulsion, a high water resistance, and a modified acrylic acid emulsion, a modified acrylic acid emulsion, and a high-water resistance emulsion, and a high-resistance emulsion;
s5: adding other auxiliary agents for mixing
Adding a defoaming agent, a leveling agent and a thickening agent into the chitosan modified polyurethane emulsion, stirring for 2 hours at the speed of 1200r/min, uniformly mixing, adding a film forming auxiliary agent and the modified acrylic emulsion, and continuously stirring for 1 hour at the speed of 800r/min to obtain the wall paint.
Example 2
A preparation method of a wall paint with strong antibacterial and anti-stain effects is shown in figure 1, and comprises the following steps:
s1: citric acid acidified chitosan
Adding citric acid produced by the dry and Yao technology Co., ltd and chitosan produced by the Wuhan Ji chemical Co., ltd into a reaction tank containing ethanol solution according to a molar ratio of 5:1, stirring for 0.5h, reacting to obtain a solid-liquid mixture, starting a booster pump, pressing the solid-liquid mixture into a centrifugal separator through a slide tube, centrifuging the solid-liquid mixture at a speed of 8000r/min for 15min by the centrifugal separator, performing solid-liquid separation, discharging filtrate to obtain filter residues, washing the filter residues for 5 times by absolute ethanol, and then drying the washed filter residues in a drying box to obtain acidified chitosan;
s2: synthesis of polyurethane from polyester polyol
Vacuum dehydrating polytetrahydrofuran ether glycol produced by Jinan Guangyu chemical industry Co., ltd, adding the polytetrahydrofuran ether glycol and polyester polyol produced by Shandong Shuixin new material science and technology Co., ltd together in a molar ratio of 1:3 into a stirrer, heating to 70 ℃, stirring and mixing, adding isophorone diisocyanate produced by Hubei Chengfeng chemical industry Co., ltd into the stirrer, stirring uniformly, heating to 90 ℃, carrying out heat preservation and reaction for 2 hours, adding dimethylolbutyric acid produced by Cheng Mojia new material Co., ltd into the stirrer, stirring for 1 hour at a speed of 300r/min, and carrying out chain extension reaction to obtain a precursor;
s3: adding acidified chitosan for modification
Adding the acidified chitosan into the precursor, ball-milling for 30min at the speed of 1200rpm by using a ball milling device in a stirrer, keeping the temperature in the stirrer at 90 ℃, continuously reacting for 2h, adjusting the temperature to 60 ℃, pumping triethylamine into the stirrer by using a hydraulic pump, stirring simultaneously until PH=8 is detected by a PH detector in the stirrer, stopping pumping triethylamine, stopping stirring, standing and cooling to room temperature, loading deionized water into the hydraulic pump of the stirrer, pressing the deionized water into the stirrer from small holes on stirring claws by using the hydraulic pump, stirring simultaneously, emulsifying to obtain chitosan modified polyurethane emulsion, modifying polyurethane by using the acidified chitosan, and preparing wall paint by using the modified polyurethane emulsion as a raw material, wherein the wall paint has strong antibacterial property, is green and environment-friendly;
s4: preparation of modified acrylic emulsion with polysiloxane
Adding methyl methacrylate produced by Jinan Runtai chemical industry Co., ltd, methacrylic acid produced by Shandong Mao national trade Co., ltd, active vinyl polysiloxane produced by Wuhan Hana white pharmaceutical chemical industry Co., ltd and an emulsifier prepared by mixing a T-02 emulsifier and an SDS emulsifier according to a volume ratio of 3:1 into an emulsifying tank together, adding water, stirring uniformly to obtain a pre-emulsion, then taking 1/5 of the pre-emulsion, placing the pre-emulsion into a reactor, adding 1/3 of an initiator, stirring uniformly, heating to 70 ℃, reacting for 1h, adding the rest of the pre-emulsion, adding 1/2 of the rest of the initiator, heating to 80 ℃, reacting for 2h, heating the drying tank by using waste heat in the reactor while heating reaction, finally adding the rest of the initiator into the reactor, stirring for 40min, cooling to room temperature, obtaining modified acrylic acid, preparing a modified acrylic acid emulsion with good weather resistance, and a high water resistance, and a modified acrylic acid emulsion, and a high weather resistance, and a modified acrylic acid emulsion, a high water resistance, and a modified acrylic acid emulsion, a modified acrylic acid emulsion, and a high-water resistance emulsion, and a high-resistance emulsion;
s5: adding other auxiliary agents for mixing
Adding a defoaming agent, a leveling agent and a thickening agent into the chitosan modified polyurethane emulsion, stirring for 2 hours at the speed of 1500r/min, uniformly mixing, adding a film forming auxiliary agent and the modified acrylic emulsion, and continuously stirring for 1 hour at the speed of 1000r/min to obtain the wall paint.
Example 3
A preparation method of a wall paint with strong antibacterial and anti-stain effects is shown in figure 1, and comprises the following steps:
s1: citric acid acidified chitosan
Adding citric acid produced by the dry and blazed technology Co., ltd and chitosan produced by the Wuhan Ji chemical Co., ltd into a reaction tank containing ethanol solution according to a molar ratio of 2:1, stirring for 1h, reacting to obtain a solid-liquid mixture, starting a pressurizing pump, pressing the solid-liquid mixture into a centrifugal separator through a slide tube, centrifuging the solid-liquid mixture at a speed of 5000r/min for 30min by the centrifugal separator, performing solid-liquid separation, discharging filtrate to obtain filter residues, washing the filter residues for 5 times by absolute ethanol, and then drying the washed filter residues in a drying box to obtain acidified chitosan, wherein the water solubility of the chitosan is improved by using citric acid to acidify the chitosan;
s2: synthesis of polyurethane from polyester polyol
Vacuum dehydrating polytetrahydrofuran ether glycol produced by Jinan Guangyu chemical industry Co., ltd, adding the polytetrahydrofuran ether glycol and polyester polyol produced by Shandong Shuixin new material science and technology Co., ltd together in a molar ratio of 1:2 into a stirrer, heating to 50 ℃, stirring and mixing, adding isophorone diisocyanate produced by Hubei Chengfeng chemical industry Co., ltd into the stirrer, stirring uniformly, heating to 80 ℃, carrying out heat preservation reaction for 3 hours, adding dimethylolbutyric acid produced by Cheng Mojia new material Co., ltd into the stirrer, stirring for 2 hours at a speed of 200r/min, and carrying out chain extension reaction to obtain a precursor;
s3: adding acidified chitosan for modification
Adding the acidified chitosan into the precursor, ball-milling for 40min at the speed of 800rpm by using a ball milling device in a stirrer, keeping the temperature in the stirrer at 80 ℃, continuously reacting for 5h, adjusting the temperature to 40 ℃, pumping triethylamine into the stirrer by using a hydraulic pump, stirring simultaneously until PH=7 is detected by a PH detector in the stirrer, stopping pumping triethylamine, stopping stirring, standing and cooling to room temperature, loading deionized water into the hydraulic pump of the stirrer, pressing the deionized water into the stirrer from small holes on stirring claws by using the hydraulic pump, stirring simultaneously, emulsifying to obtain chitosan modified polyurethane emulsion, modifying polyurethane by using the acidified chitosan, and preparing wall paint by using the modified polyurethane emulsion as a raw material, wherein the wall paint has strong antibacterial property, is green and environment-friendly;
s4: preparation of modified acrylic emulsion with polysiloxane
Adding methyl methacrylate produced by Jinan Runtai chemical industry Co., ltd, methacrylic acid produced by Shandong Mao national trade Co., ltd, active vinyl polysiloxane produced by Wuhan Hana white pharmaceutical chemical industry Co., ltd and an emulsifier prepared by mixing a T-02 emulsifier and an SDS emulsifier according to a volume ratio of 1:1 into an emulsifying tank together, adding water, stirring uniformly to obtain a pre-emulsion, then taking 1/5 of the pre-emulsion, placing the pre-emulsion into a reactor, adding 1/3 of an initiator, stirring uniformly, heating to 60 ℃, reacting for 2h, adding the rest of the pre-emulsion, adding 1/2 of the rest of the initiator, heating to 70 ℃, reacting for 3h, heating the drying tank by using waste heat in the reactor while heating reaction, finally adding the rest of the initiator into the reactor, stirring for 50min, cooling to room temperature, obtaining modified acrylic acid, preparing a modified acrylic acid emulsion with good weather resistance, and a high water resistance, and a high weather resistance, and a modified acrylic acid emulsion, a high water resistance, a modified acrylic acid emulsion, a high-acrylic acid emulsion, and a high water resistance, and a modified acrylic acid emulsion, and a high-soluble polyurethane emulsion;
s5: adding other auxiliary agents for mixing
Adding a defoaming agent, a leveling agent and a thickening agent into the chitosan modified polyurethane emulsion, stirring for 3 hours at the speed of 1200r/min, uniformly mixing, adding a film forming additive and the modified acrylic emulsion, and continuously stirring for 1.5 hours at the speed of 800r/min to obtain the wall paint.
The above embodiments are merely illustrative of the principles of the present invention and its effectiveness, and are not intended to limit the invention. Modifications and variations may be made to the above-described embodiments by those skilled in the art without departing from the spirit and scope of the invention. Accordingly, it is intended that all equivalent modifications and variations of the invention be covered by the claims, which are within the ordinary skill of the art, be within the spirit and scope of the present disclosure.
Claims (8)
1. The preparation method of the wall paint with strong antibacterial and anti-stain effects is characterized by comprising the following steps of:
s1: citric acid acidified chitosan
Adding citric acid and chitosan into an ethanol solution, stirring for reaction, performing centrifugal separation, and then washing and drying to obtain acidified chitosan;
s2: synthesis of polyurethane from polyester polyol
Under the high temperature condition, polytetrahydrofuran ether glycol, polyester polyol, isophorone diisocyanate and dimethylolbutyric acid are mixed for reaction to obtain a precursor;
s3: adding acidified chitosan for modification
Adding the acidified chitosan into the precursor, performing ball milling, performing heat preservation reaction, adding triethylamine to adjust the PH, and adding deionized water to emulsify to obtain chitosan modified polyurethane emulsion;
s4: preparation of modified acrylic emulsion with polysiloxane
Mixing methyl methacrylate, methacrylic acid, polysiloxane with active vinyl and an emulsifier, adding water for emulsification, and then adding an initiator for reaction to obtain modified acrylic emulsion;
s5: adding other auxiliary agents for mixing
Adding a defoaming agent, a leveling agent and a thickening agent into the chitosan modified polyurethane emulsion, stirring for 2-3 hours at the speed of 1200-1500r/min, uniformly mixing, adding a film forming additive and the modified acrylic emulsion, and continuously stirring for 1-1.5 hours at the speed of 800-1000r/min to obtain the wall paint.
2. The method for preparing the wall paint with strong antibacterial and anti-stain effects according to claim 1, wherein the citric acid-acidified chitosan of the step S1 specifically comprises the following steps:
s1.1: adding citric acid and chitosan together into a reaction tank containing ethanol solution according to a molar ratio of 2-5:1, stirring for 0.5-1h, and reacting to obtain a solid-liquid mixture;
s1.2: starting a pressurizing pump, pressing the solid-liquid mixture into a centrifugal separator through a slide pipe, centrifuging the solid-liquid mixture for 15-30min at a speed of 5000-8000r/min by the centrifugal separator, performing solid-liquid separation, and discharging filtrate to obtain filter residues;
s1.3: washing the filter residue for 2-5 times by using absolute ethyl alcohol, and then placing the washed filter residue into a drying box for drying to obtain the acidified chitosan.
3. The method for preparing the wall paint with strong antibacterial and anti-stain effects according to claim 1, wherein the step S2 of synthesizing polyurethane by using polyester polyol specifically comprises the following steps:
s2.1: vacuum dehydrating polytetrahydrofuran ether glycol, adding the polytetrahydrofuran ether glycol and polyester polyol into a stirrer together according to the molar ratio of 1:2-3, heating to 50-70 ℃, stirring and mixing;
s2.2: adding isophorone diisocyanate into a stirrer, stirring uniformly, heating to 80-90 ℃, and reacting for 2-3h under heat preservation;
s2.3: adding the dimethylolbutyric acid into a stirrer, stirring at the speed of 200-300r/min for 1-2h, and performing chain extension reaction to obtain a precursor.
4. The method for preparing the wall paint with strong antibacterial and anti-stain effects according to claim 1, wherein the step S3 of adding the acidified chitosan for modification comprises the following steps:
s3.1: adding the acidified chitosan into the precursor, ball-milling for 30-40min at a speed of 800-1200rpm by using a ball-milling device in a stirrer, keeping the temperature in the stirrer at 80-90 ℃, and continuing to react for 2-5h;
s3.2: regulating the temperature to 40-60 ℃, pumping triethylamine into a stirrer by using a hydraulic pump, stirring the triethylamine until a PH detector in the stirrer detects PH=7-8, stopping pumping the triethylamine, stopping stirring, standing and cooling to room temperature;
s3.3: and filling deionized water into a hydraulic pump of the stirrer, pressing the deionized water into the stirrer from small holes on stirring claws by the hydraulic pump, stirring at the same time, and emulsifying to obtain the chitosan modified polyurethane emulsion.
5. The method for preparing the wall paint with strong antibacterial and anti-stain effects according to claim 2, wherein the step S4 of preparing the modified acrylic emulsion with polysiloxane specifically comprises the following steps:
s4.1: adding methyl methacrylate, methacrylic acid, polysiloxane with active vinyl and an emulsifying agent into an emulsifying cylinder, adding water, and uniformly stirring to obtain a pre-emulsion;
s4.2: placing 1/5 of the pre-emulsion into a reactor, adding 1/3 of an initiator, uniformly stirring, heating to 60-70 ℃, and reacting for 1-2h;
s4.3: adding the residual pre-emulsion into a reactor, adding 1/2 of the residual initiator, heating to 70-80 ℃, and reacting for 2-3h;
s4.4: and adding all the rest initiator into the reactor, stirring for 40-50min, simultaneously carrying out heat preservation reaction, and cooling to room temperature to obtain the modified acrylic emulsion.
6. The method for preparing a wall paint with strong antibacterial and anti-stain effects according to claim 5, wherein the drying box is installed on the inner wall of the reactor in the step S4.2, and when the temperature in the reactor is raised for reaction, the temperature in the drying box is raised by the waste heat in the reactor, and the washed filter residues are dried.
7. The method for preparing a wall paint with strong antibacterial and anti-stain effects according to claim 5, wherein the emulsifier is prepared by mixing a T-02 emulsifier and an SDS emulsifier according to a volume ratio of 1-3:1.
8. The method for preparing a wall paint with strong antibacterial and anti-stain effects according to claim 5, wherein the volume ratio of methyl methacrylate, methacrylic acid and polysiloxane with active vinyl is 5-10:2-5:1.
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