CN114316656A - Self-repairing flame-retardant water-based paint - Google Patents
Self-repairing flame-retardant water-based paint Download PDFInfo
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- CN114316656A CN114316656A CN202111575248.7A CN202111575248A CN114316656A CN 114316656 A CN114316656 A CN 114316656A CN 202111575248 A CN202111575248 A CN 202111575248A CN 114316656 A CN114316656 A CN 114316656A
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- 239000003063 flame retardant Substances 0.000 title claims abstract description 58
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 title claims abstract description 53
- 239000003973 paint Substances 0.000 title claims abstract description 36
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 36
- 238000000576 coating method Methods 0.000 claims abstract description 58
- 239000011248 coating agent Substances 0.000 claims abstract description 57
- 241001312219 Amorphophallus konjac Species 0.000 claims abstract description 25
- 235000001206 Amorphophallus rivieri Nutrition 0.000 claims abstract description 25
- 229920002752 Konjac Polymers 0.000 claims abstract description 25
- 229920000180 alkyd Polymers 0.000 claims abstract description 25
- 235000010485 konjac Nutrition 0.000 claims abstract description 25
- 239000000252 konjac Substances 0.000 claims abstract description 25
- 238000007605 air drying Methods 0.000 claims abstract description 20
- 239000003094 microcapsule Substances 0.000 claims abstract description 12
- 239000000839 emulsion Substances 0.000 claims abstract description 10
- 229920002635 polyurethane Polymers 0.000 claims abstract description 10
- 239000004814 polyurethane Substances 0.000 claims abstract description 10
- 239000002270 dispersing agent Substances 0.000 claims abstract description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 54
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 32
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 30
- 238000006243 chemical reaction Methods 0.000 claims description 28
- 238000003756 stirring Methods 0.000 claims description 27
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 24
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 24
- JUJWROOIHBZHMG-UHFFFAOYSA-N Pyridine Chemical compound C1=CC=NC=C1 JUJWROOIHBZHMG-UHFFFAOYSA-N 0.000 claims description 20
- 229910019142 PO4 Inorganic materials 0.000 claims description 18
- 150000001263 acyl chlorides Chemical class 0.000 claims description 18
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 claims description 18
- 239000010452 phosphate Substances 0.000 claims description 18
- 229910052757 nitrogen Inorganic materials 0.000 claims description 16
- 238000005406 washing Methods 0.000 claims description 16
- 238000000967 suction filtration Methods 0.000 claims description 15
- 238000004519 manufacturing process Methods 0.000 claims description 13
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 claims description 12
- 235000013312 flour Nutrition 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 12
- FYSNRJHAOHDILO-UHFFFAOYSA-N thionyl chloride Chemical compound ClS(Cl)=O FYSNRJHAOHDILO-UHFFFAOYSA-N 0.000 claims description 12
- 238000001291 vacuum drying Methods 0.000 claims description 12
- 238000001035 drying Methods 0.000 claims description 10
- UMJSCPRVCHMLSP-UHFFFAOYSA-N pyridine Natural products COC1=CC=CN=C1 UMJSCPRVCHMLSP-UHFFFAOYSA-N 0.000 claims description 10
- ARVGPHNSEONSQH-UHFFFAOYSA-N 7,9-dihydro-3h-purine-2,6,8-trione;phosphoric acid Chemical compound OP(O)(O)=O.N1C(=O)NC(=O)C2=C1NC(=O)N2 ARVGPHNSEONSQH-UHFFFAOYSA-N 0.000 claims description 6
- 230000010933 acylation Effects 0.000 claims description 6
- 238000005917 acylation reaction Methods 0.000 claims description 6
- 229910000147 aluminium phosphate Inorganic materials 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- 230000004048 modification Effects 0.000 claims description 6
- 238000012986 modification Methods 0.000 claims description 6
- 238000004806 packaging method and process Methods 0.000 claims description 6
- 239000000758 substrate Substances 0.000 claims description 6
- 108010010803 Gelatin Proteins 0.000 claims description 5
- SXRSQZLOMIGNAQ-UHFFFAOYSA-N Glutaraldehyde Chemical compound O=CCCCC=O SXRSQZLOMIGNAQ-UHFFFAOYSA-N 0.000 claims description 5
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 5
- 238000001816 cooling Methods 0.000 claims description 5
- 229920000159 gelatin Polymers 0.000 claims description 5
- 239000008273 gelatin Substances 0.000 claims description 5
- 235000019322 gelatine Nutrition 0.000 claims description 5
- 235000011852 gelatine desserts Nutrition 0.000 claims description 5
- 239000005457 ice water Substances 0.000 claims description 5
- 238000002360 preparation method Methods 0.000 claims description 5
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 5
- 235000011152 sodium sulphate Nutrition 0.000 claims description 5
- 238000005507 spraying Methods 0.000 claims description 5
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 4
- 239000004202 carbamide Substances 0.000 claims description 4
- 230000000087 stabilizing effect Effects 0.000 claims description 4
- 230000008961 swelling Effects 0.000 claims description 4
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 2
- 238000007766 curtain coating Methods 0.000 claims description 2
- 238000003618 dip coating Methods 0.000 claims description 2
- 238000007590 electrostatic spraying Methods 0.000 claims description 2
- 229910052710 silicon Inorganic materials 0.000 claims description 2
- 239000010703 silicon Substances 0.000 claims description 2
- 238000004528 spin coating Methods 0.000 claims description 2
- 229920005830 Polyurethane Foam Polymers 0.000 claims 1
- 239000011496 polyurethane foam Substances 0.000 claims 1
- 239000002023 wood Substances 0.000 abstract description 10
- 239000000853 adhesive Substances 0.000 abstract description 3
- 230000001070 adhesive effect Effects 0.000 abstract description 3
- 230000002035 prolonged effect Effects 0.000 abstract description 3
- 230000008439 repair process Effects 0.000 abstract description 3
- LUEWUZLMQUOBSB-FSKGGBMCSA-N (2s,3s,4s,5s,6r)-2-[(2r,3s,4r,5r,6s)-6-[(2r,3s,4r,5s,6s)-4,5-dihydroxy-2-(hydroxymethyl)-6-[(2r,4r,5s,6r)-4,5,6-trihydroxy-2-(hydroxymethyl)oxan-3-yl]oxyoxan-3-yl]oxy-4,5-dihydroxy-2-(hydroxymethyl)oxan-3-yl]oxy-6-(hydroxymethyl)oxane-3,4,5-triol Chemical compound O[C@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1O[C@@H]1[C@@H](CO)O[C@@H](O[C@@H]2[C@H](O[C@@H](OC3[C@H](O[C@@H](O)[C@@H](O)[C@H]3O)CO)[C@@H](O)[C@H]2O)CO)[C@H](O)[C@H]1O LUEWUZLMQUOBSB-FSKGGBMCSA-N 0.000 abstract 1
- 229920002581 Glucomannan Polymers 0.000 abstract 1
- 239000002518 antifoaming agent Substances 0.000 abstract 1
- 229940046240 glucomannan Drugs 0.000 abstract 1
- 239000008213 purified water Substances 0.000 abstract 1
- 239000000047 product Substances 0.000 description 38
- 230000000694 effects Effects 0.000 description 5
- 238000009413 insulation Methods 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 3
- 229910052736 halogen Inorganic materials 0.000 description 3
- 150000002367 halogens Chemical class 0.000 description 3
- 239000000779 smoke Substances 0.000 description 3
- 239000002341 toxic gas Substances 0.000 description 3
- 239000000945 filler Substances 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- 239000000049 pigment Substances 0.000 description 2
- 230000002265 prevention Effects 0.000 description 2
- 229920005989 resin Polymers 0.000 description 2
- 239000011347 resin Substances 0.000 description 2
- 238000006748 scratching Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000004566 building material Substances 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000005034 decoration Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 230000002393 scratching effect Effects 0.000 description 1
- 239000011265 semifinished product Substances 0.000 description 1
- 230000007480 spreading Effects 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000001629 suppression Effects 0.000 description 1
Landscapes
- Paints Or Removers (AREA)
Abstract
The invention provides a self-repairing flame-retardant water-based paint which comprises the following components in percentage by weight: 25-40% of polyurethane emulsion, 20-35% of halogen-free intumescent konjac glucomannan flame retardant, 5-10% of air-drying alkyd self-repairing microcapsule, 5-10% of dispersing agent, 5-15% of vitrified micro bubbles, 1-5% of defoaming agent and the balance of purified water. The polyurethane emulsion is adopted, so that the adhesive force and the impact resistance of a wood product paint film are improved, the air-drying alkyd resin repair microcapsule is adopted, when the cured coating is slightly worn, the air-drying alkyd resin seeps out to react with air to form a film, microscopic damage parts are repaired in time, the broken parts of the coating cannot continue to extend, the subsequent breakage and peeling of the coating are avoided, and the service life of the flame-retardant coating is prolonged.
Description
Technical Field
The invention relates to the field of building coatings, in particular to a self-repairing flame-retardant water-based coating.
Background
At present, the use of the coating is closely related to the interface, and the coating is a multi-component system and comprises resin (base material), pigments, fillers, solvents, auxiliaries and the like. A plurality of interfaces exist in the system, and particularly, a certain interface exists among the pigment, the filler, the resin and the solvent; meanwhile, the coating is a semi-finished product and can provide protection, decoration, functions and the like only by being coated on workpieces, products and structures, so that certain interface states inevitably exist, and certain requirements are provided for the use of the coating. In addition, after the coating is applied, there is a drying and curing process in which the contact between the (wet) surface of the coating film and air is necessarily taken into consideration to ensure that a good appearance of the coating film is provided and the occurrence of surface defects is prevented.
The wood product is easy to cause fire because of the characteristic of low burning point and flammability, and in order to avoid the disadvantage, the method adopted at present mainly adds flame-retardant liquid medicine into the wood or coats flame-retardant coating. However, the existing flame retardant coating can not effectively insulate and protect wood, has no smoke-proof effect, and even some flame retardant materials can release toxic gases containing halogen when decomposed. And the coating is damaged when the flame-retardant coating building material is coated, and the flame-retardant effect is invalid due to stripping. Meanwhile, the existing flame-retardant coating cannot meet the production requirements on a production line. Therefore, in order to ensure and improve the adhesion and impact resistance of a paint film, the production requirement of fireproof wood products on a production line is met, and the wood products have heat insulation and smoke prevention effects. Improvements in the prior art are necessary.
Disclosure of Invention
The technical problem to be solved is as follows: the invention aims to solve the problem that the conventional flame-retardant material can release toxic gas containing halogen when decomposed. The invention adopts polyurethane emulsion to improve the adhesive force and impact resistance of a wood product paint film, and adopts air-drying alkyd resin to repair microcapsules, so that when the cured coating is slightly worn, the air-drying alkyd resin seeps out to react with air to form a film, the microscopic damaged part of the coating is repaired in time, the continuous extension of the broken part of the coating is avoided, the subsequent breakage and peeling of the coating are avoided, and the service life of the flame-retardant coating is prolonged.
The technical scheme is as follows: a self-repairing flame-retardant water-based paint is prepared from polyurethane emulsion, a halogen-free intumescent konjac fire retardant and air-drying alkyd resin self-repairing microcapsules.
The self-repairing flame-retardant water-based paint comprises the following components in percentage by weight:
the polyurethane emulsion is organic silicon modified polyurethane emulsion.
Preferably, the steps of the halogen-free intumescent konjac fire retardant are as follows:
s1: modification of konjac flour into a phosphate: under the reaction condition of 40-60 ℃, the weight portions are as follows: adding konjac flour into phosphoric acid, (1-2) mechanically stirring and reacting for 2-4 h under a nitrogen protection environment, washing with dimethylformamide after the reaction is finished, performing suction filtration, and performing vacuum drying for 12-24 h at 60-80 ℃ to obtain a phosphate;
s2: acylation of the phosphorylate: adding a phosphate (toluene (1-2): 10) into toluene, then respectively adding 1-2 parts by weight of thionyl chloride and 5-6 parts by weight of ethanol, stirring and reacting at 25-55 ℃ for 2-6 h, carrying out the whole reaction under the condition of nitrogen, washing the obtained acyl chloride product with toluene and ethanol, carrying out suction filtration, and carrying out vacuum drying at 60-80 ℃ for 12-24 h to obtain an acyl chloride product;
s3: uric acid phosphate: adding an acyl chloride product of pyridine (1-2): 5 in parts by weight into pyridine for swelling, under the protection of nitrogen, then dripping 1-2 parts by weight of urea solution, reacting for 2-6 h, cooling to room temperature after the reaction is finished, washing with N, N-dimethylformamide and methanol in sequence, carrying out suction filtration, drying, dissolving the product with methanol, and then stabilizing the product with a rotary evaporator to obtain the konjac flame retardant.
Preferably, the preparation method of the air-drying alkyd resin self-repairing microcapsule comprises the following steps: adding 10g of gelatin solution and 20g of air-drying alkyd resin into a reaction kettle, stirring for 90min at the rotation speed of 400r/min and the temperature of 60 ℃, adding 3g of sodium sulfate solution, continuously stirring for 30min under the condition of ice-water bath, adding 3g of glutaraldehyde, continuously stirring for 3min, standing for 10min, filtering and drying to obtain the gelatin-modified alkyd resin.
Preferably, the dispersant is BYK-192.
The using method of the self-repairing flame-retardant water-based paint comprises the following steps:
step 1: coating the self-repairing flame-retardant water-based coating on the surface of a wooden product;
step 2: curing by using a hot air blower;
and step 3: continuously coating the ultraviolet curing coating on the substrate, and then curing;
and 4, step 4: and packaging finished products on the production line.
Preferably, the coating means includes roll coating, electrostatic spraying, vacuum spraying, curtain coating, dip coating, spin coating, and draw coating.
Preferably, the curing temperature in the step 2 is 50-70 ℃, and the curing time is 20-40 s.
Preferably, the ultraviolet curing conditions in step 3 are as follows: the ultraviolet curing conditions are as follows: the curing energy is 100-2。
Has the advantages that:
1. the coating disclosed by the invention uses the polyurethane emulsion, so that the adhesive force and the impact resistance of a wooden product paint film can be improved.
2. The coating has good heat insulation effect, can delay or prevent fire from diffusing, and when the surface temperature of the coating is below 400 ℃, the hollow glass can obstruct heat conduction and prevent the coating from cracking caused by water vapor or other substances in the wood so as to prevent the internal wood from contacting a heat source; when the surface temperature of the coating exceeds 400 ℃, the coating begins to liquefy and continuously expands to form a thicker heat insulation protective layer, and the heat insulation effect is improved.
3. The coating disclosed by the invention adopts the tough heat-insulating layer and the continuously generated expansion layer to block heat conduction, does not adopt the volatilization heat absorption cooling fire prevention principle of halogen-containing materials, avoids the generation of toxic gas and smoke, has a smoke suppression effect while preventing the fire from spreading, and obtains better escape conditions for personnel in a fire scene.
4. The invention adopts the air-drying alkyd resin to repair the microcapsule, so that when the cured coating is slightly worn, the air-drying alkyd resin seeps out to react with air to form a film, and the microscopic damaged part is repaired in time, so that the broken part of the coating cannot continue to extend, the subsequent breakage and peeling of the coating are avoided, and the service life of the flame-retardant coating is prolonged.
5. The coating can be used on a production line to prepare a wood product with fireproof performance, is suitable for quick production, and greatly improves the production efficiency.
Detailed Description
Example 1
The self-repairing flame-retardant water-based paint comprises the following components in percentage by weight:
all the components are mixed and stirred to obtain the self-repairing flame-retardant water-based paint.
The halogen-free intumescent konjac flame retardant comprises the following steps:
s1: modification of konjac flour into a phosphate: under the reaction condition of 40 ℃, according to the weight portion: adding konjac flour into phosphoric acid at a ratio of 10:1, mechanically stirring under nitrogen protection for reaction for 2h, washing with dimethylformamide after the reaction is finished, performing suction filtration, and vacuum drying at 60 ℃ for 12h to obtain phosphate;
s2: acylation of the phosphorylate: adding a phosphate with the weight portion of toluene being 1:10 into toluene, then respectively adding 1 part of thionyl chloride and 5 parts of ethanol with the weight portion, stirring and reacting for 2 hours at 25 ℃, carrying out the whole reaction under the condition of nitrogen, washing the obtained acyl chloride product with toluene and ethanol, carrying out suction filtration, and carrying out vacuum drying for 12 hours at 60 ℃ to obtain an acyl chloride product;
s3: uric acid phosphate: adding an acyl chloride product of which the weight part is that the weight part is that the weight is that the weight of the weight is that the weight of the.
The preparation method of the air-drying alkyd resin self-repairing microcapsule comprises the following steps: adding 10g of gelatin solution and 20g of air-drying alkyd resin into a reaction kettle, stirring for 90min at the rotation speed of 400r/min and the temperature of 60 ℃, adding 3g of sodium sulfate solution, continuously stirring for 30min under the condition of ice-water bath, adding 3g of glutaraldehyde, continuously stirring for 3min, standing for 10min, filtering and drying to obtain the gelatin-modified alkyd resin. The using method of the self-repairing flame-retardant water-based paint comprises the following steps:
step 1: coating the self-repairing flame-retardant water-based paint on the surface of a wooden product by a roller;
step 2: curing by using an air heater at 50 ℃ for 40 s;
and step 3: continuously coating the ultraviolet curing coating on the substrate, and then curing, wherein the ultraviolet curing conditions are as follows: the ultraviolet curing conditions are as follows: the curing energy is 100-2；
And 4, step 4: and packaging finished products on the production line.
Example 2
The self-repairing flame-retardant water-based paint comprises the following components in percentage by weight:
all the components are mixed and stirred to obtain the self-repairing flame-retardant water-based paint.
The halogen-free intumescent konjac flame retardant comprises the following steps:
s1: modification of konjac flour into a phosphate: under the reaction condition of 50 ℃, according to the weight portion: adding konjac flour into phosphoric acid at a ratio of 10:1.5, mechanically stirring under nitrogen protection for 3h, washing with dimethylformamide after reaction, vacuum-filtering, and vacuum-drying at 70 deg.C for 18h to obtain phosphate;
s2: acylation of the phosphorylate: adding a phosphate with the weight portion of toluene being 1.5:10 into toluene, then respectively adding 1.5 parts of thionyl chloride and 5.5 parts of ethanol with the weight portions, stirring and reacting for 4 hours at 40 ℃, carrying out the whole reaction under the condition of nitrogen, washing the obtained acyl chloride product with toluene and ethanol, carrying out suction filtration, and carrying out vacuum drying for 18 hours at 70 ℃ to obtain an acyl chloride product;
s3: uric acid phosphate: adding an acyl chloride product of which the weight part is that the weight of the.
The preparation method of the air-drying alkyd resin self-repairing microcapsule comprises the following steps: adding 10g of gelatin solution and 20g of air-drying alkyd resin into a reaction kettle, stirring for 90min at the rotation speed of 400r/min and the temperature of 60 ℃, adding 3g of sodium sulfate solution, continuously stirring for 30min under the condition of ice-water bath, adding 3g of glutaraldehyde, continuously stirring for 3min, standing for 10min, filtering and drying to obtain the gelatin-modified alkyd resin. The using method of the self-repairing flame-retardant water-based paint comprises the following steps:
step 1: electrostatically spraying the self-repairing flame-retardant water-based paint on the surface of the wooden product;
step 2: curing by using an air heater at the curing temperature of 60 ℃ for 30 s;
and step 3: continuously coating the ultraviolet curing coating on the substrate, and then curing, wherein the ultraviolet curing conditions are as follows: the ultraviolet curing conditions are as follows: the curing energy is 100-2；
And 4, step 4: and packaging finished products on the production line.
Example 3
The self-repairing flame-retardant water-based paint comprises the following components in percentage by weight:
all the components are mixed and stirred to obtain the self-repairing flame-retardant water-based paint.
The halogen-free intumescent konjac flame retardant comprises the following steps:
s1: modification of konjac flour into a phosphate: under the reaction condition of 60 ℃, according to the weight portion: adding konjac flour into phosphoric acid at a ratio of 10:2, mechanically stirring under nitrogen protection for 4h, washing with dimethylformamide after the reaction is finished, performing suction filtration, and vacuum drying at 80 ℃ for 24h to obtain phosphate;
s2: acylation of the phosphorylate: adding a phosphate with the weight portion of toluene being 2:10 into toluene, then respectively adding 2 parts by weight of thionyl chloride and 6 parts by weight of ethanol, stirring and reacting for 6 hours at 55 ℃, carrying out the whole reaction under the condition of nitrogen, washing the obtained acyl chloride product with toluene and ethanol, carrying out suction filtration, and carrying out vacuum drying for 24 hours at 80 ℃ to obtain an acyl chloride product;
s3: uric acid phosphate: adding an acyl chloride product of which the weight part is 2:5 pyridine into pyridine for swelling, dripping a urea solution of which the weight part is 2 into the pyridine under the protection of nitrogen, reacting for 6 hours, cooling to room temperature after the reaction is finished, washing with N, N-dimethylformamide and methanol, performing suction filtration, drying, dissolving the product with methanol, and stabilizing the product with a rotary evaporator to obtain the konjac fire retardant.
The preparation method of the air-drying alkyd resin self-repairing microcapsule comprises the following steps: adding 10g of gelatin solution and 20g of air-drying alkyd resin into a reaction kettle, stirring for 90min at the rotation speed of 400r/min and the temperature of 60 ℃, adding 3g of sodium sulfate solution, continuously stirring for 30min under the condition of ice-water bath, adding 3g of glutaraldehyde, continuously stirring for 3min, standing for 10min, filtering and drying to obtain the gelatin-modified alkyd resin. The using method of the self-repairing flame-retardant water-based paint comprises the following steps:
step 1: vacuum spraying the self-repairing flame-retardant water-based paint on the surface of a wooden product;
step 2: curing by using an air heater at the curing temperature of 70 ℃ for 20 s;
and step 3: continuously coating the ultraviolet curing coating on the substrate, and then curing, wherein the ultraviolet curing conditions are as follows: the ultraviolet curing conditions are as follows: the curing energy is 100-2；
And 4, step 4: and packaging finished products on the production line.
Comparative example 1
The difference between the comparative example and the example 3 is that the air-drying alkyd resin self-repairing microcapsule is not contained, and the details are as follows:
the flame-retardant water-based paint comprises the following components in percentage by weight:
all the components are mixed and stirred to obtain the self-repairing flame-retardant water-based paint.
The halogen-free intumescent konjac flame retardant comprises the following steps:
s1: modification of konjac flour into a phosphate: under the reaction condition of 60 ℃, according to the weight portion: adding konjac flour into phosphoric acid at a ratio of 10:2, mechanically stirring under nitrogen protection for 4h, washing with dimethylformamide after the reaction is finished, performing suction filtration, and vacuum drying at 80 ℃ for 24h to obtain phosphate;
s2: acylation of the phosphorylate: adding a phosphate with the weight portion of toluene being 2:10 into toluene, then respectively adding 2 parts by weight of thionyl chloride and 6 parts by weight of ethanol, stirring and reacting for 6 hours at 55 ℃, carrying out the whole reaction under the condition of nitrogen, washing the obtained acyl chloride product with toluene and ethanol, carrying out suction filtration, and carrying out vacuum drying for 24 hours at 80 ℃ to obtain an acyl chloride product;
s3: uric acid phosphate: adding an acyl chloride product of which the weight part is 2:5 pyridine into pyridine for swelling, dripping a urea solution of which the weight part is 2 into the pyridine under the protection of nitrogen, reacting for 6 hours, cooling to room temperature after the reaction is finished, washing with N, N-dimethylformamide and methanol, performing suction filtration, drying, dissolving the product with methanol, and stabilizing the product with a rotary evaporator to obtain the konjac fire retardant.
The using method of the self-repairing flame-retardant water-based paint comprises the following steps:
step 1: vacuum spraying the self-repairing flame-retardant water-based paint on the surface of a wooden product;
step 2: curing by using an air heater at the curing temperature of 70 ℃ for 20 s;
and step 3: continuously coating the ultraviolet curing coating on the substrate, and then curing, wherein the ultraviolet curing conditions are as follows: the ultraviolet curing conditions are as follows: the curing energy is 100-2；
And 4, step 4: and packaging finished products on the production line.
The performance indexes of the embodiment of the invention are as follows:
TABLE 1
| Technical index | Standard of merit | Example 1 | Example 2 | Example 3 | Comparative example 1 |
| Adhesion force | ASTMD3359 | B5 | B5 | B5 | B5 |
| Scratch resistance | ISO1518 | 2500g | 2500g | 2500g | 2500g |
| Micro-scratch | EN16094 | A4 | A4 | A4 | A4 |
| Initial gloss | ASTMD-523 | 60 | 60 | 60 | 60 |
| Gloss within 5min after micro-scratching | ASTMD-523 | 50 | 52 | 55 | 45 |
| Gloss after 24h of micro scratching | ASTMD-523 | 55 | 57 | 58 | 45 |
Claims (9)
1. A self-repairing flame-retardant water-based paint is characterized in that: the self-repairing polyurethane foam is prepared from polyurethane emulsion, a halogen-free intumescent konjac fire retardant and air-drying alkyd resin self-repairing microcapsules.
2. The self-repairing flame-retardant water-based paint as claimed in claim 1, wherein: the paint consists of the following components in percentage by weight:
the polyurethane emulsion is organic silicon modified polyurethane emulsion.
3. The self-repairing flame-retardant water-based paint as claimed in claim 1, wherein: the halogen-free intumescent konjac flame retardant comprises the following steps:
s1: modification of konjac flour into a phosphate: under the reaction condition of 40-60 ℃, the weight portions are as follows: adding konjac flour into phosphoric acid, (1-2) mechanically stirring and reacting for 2-4 h under a nitrogen protection environment, washing with dimethylformamide after the reaction is finished, performing suction filtration, and performing vacuum drying for 12-24 h at 60-80 ℃ to obtain a phosphate;
s2: acylation of the phosphorylate: adding a phosphate (toluene (1-2): 10) into toluene, then respectively adding 1-2 parts by weight of thionyl chloride and 5-6 parts by weight of ethanol, stirring and reacting at 25-55 ℃ for 2-6 h, carrying out the whole reaction under the condition of nitrogen, washing the obtained acyl chloride product with toluene and ethanol, carrying out suction filtration, and carrying out vacuum drying at 60-80 ℃ for 12-24 h to obtain an acyl chloride product;
s3: uric acid phosphate: adding an acyl chloride product of pyridine (1-2): 5 in parts by weight into pyridine for swelling, under the protection of nitrogen, then dripping 1-2 parts by weight of urea solution, reacting for 2-6 h, cooling to room temperature after the reaction is finished, washing with N, N-dimethylformamide and methanol in sequence, carrying out suction filtration, drying, dissolving the product with methanol, and then stabilizing the product with a rotary evaporator to obtain the konjac flame retardant.
4. The self-repairing flame-retardant water-based paint as claimed in claim 1, wherein: the preparation method of the air-drying alkyd resin self-repairing microcapsule comprises the following steps: adding 10g of gelatin solution and 20g of air-drying alkyd resin into a reaction kettle, stirring for 90min at the rotation speed of 400r/min and the temperature of 60 ℃, adding 3g of sodium sulfate solution, continuously stirring for 30min under the condition of ice-water bath, adding 3g of glutaraldehyde, continuously stirring for 3min, standing for 10min, filtering and drying to obtain the gelatin-modified alkyd resin.
5. The self-repairing flame-retardant water-based paint as claimed in claim 2, wherein: the dispersant is BYK-192.
6. The use method of the self-repairing flame-retardant water-based paint, according to claim 2, is characterized in that: the method comprises the following steps:
step 1: coating the self-repairing flame-retardant water-based coating on the surface of a wooden product;
step 2: curing by using a hot air blower;
and step 3: continuously coating the ultraviolet curing coating on the substrate, and then curing;
and 4, step 4: and packaging finished products on the production line.
7. The use method of the self-repairing flame-retardant water-based paint, according to claim 6, is characterized in that: the coating modes comprise roll coating, electrostatic spraying, vacuum spraying, curtain coating, dip coating, spin coating and pump coating.
8. The use method of the self-repairing flame-retardant water-based paint, according to claim 6, is characterized in that: in the step 2, the curing temperature is 50-70 ℃, and the curing time is 20-40 s.
9. The use method of the self-repairing flame-retardant water-based paint, according to claim 6, is characterized in that: the ultraviolet curing conditions in the step 3 are as follows: the curing energy is 100-2。
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|---|---|---|---|---|
| CN104927468A (en) * | 2015-05-27 | 2015-09-23 | 叶氏化工研发（上海）有限公司 | Microcapsule type additive for corrosion-resistant coating and preparation method thereof |
| CN111298729A (en) * | 2018-12-11 | 2020-06-19 | 中国船舶重工集团公司第七二五研究所 | Self-repairing microcapsule and preparation and application methods thereof |
| CN112646472A (en) * | 2020-12-18 | 2021-04-13 | 东周化学工业（昆山）有限公司 | Flame-retardant water-based paint and preparation method thereof |
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2021
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| CN111298729A (en) * | 2018-12-11 | 2020-06-19 | 中国船舶重工集团公司第七二五研究所 | Self-repairing microcapsule and preparation and application methods thereof |
| CN112646472A (en) * | 2020-12-18 | 2021-04-13 | 东周化学工业（昆山）有限公司 | Flame-retardant water-based paint and preparation method thereof |
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