CN108384421A - A kind of accumulation of heat aqueous polyurethane coating - Google Patents
A kind of accumulation of heat aqueous polyurethane coating Download PDFInfo
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- CN108384421A CN108384421A CN201810241025.9A CN201810241025A CN108384421A CN 108384421 A CN108384421 A CN 108384421A CN 201810241025 A CN201810241025 A CN 201810241025A CN 108384421 A CN108384421 A CN 108384421A
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- parts
- lignin
- aqueous polyurethane
- accumulation
- polyurethane coating
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- 239000011527 polyurethane coating Substances 0.000 title claims abstract description 33
- 238000009825 accumulation Methods 0.000 title claims abstract description 30
- 229920005610 lignin Polymers 0.000 claims abstract description 74
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 38
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 19
- 239000002270 dispersing agent Substances 0.000 claims abstract description 15
- 238000009736 wetting Methods 0.000 claims abstract description 15
- 229920003009 polyurethane dispersion Polymers 0.000 claims abstract description 10
- 239000005056 polyisocyanate Substances 0.000 claims abstract description 9
- 229920001228 polyisocyanate Polymers 0.000 claims abstract description 9
- 239000002518 antifoaming agent Substances 0.000 claims abstract description 7
- 239000002994 raw material Substances 0.000 claims abstract description 3
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 78
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 38
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 32
- 235000008331 Pinus X rigitaeda Nutrition 0.000 claims description 29
- 235000011613 Pinus brutia Nutrition 0.000 claims description 29
- 241000018646 Pinus brutia Species 0.000 claims description 29
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 20
- 239000000843 powder Substances 0.000 claims description 18
- 239000008367 deionised water Substances 0.000 claims description 16
- 229910021641 deionized water Inorganic materials 0.000 claims description 16
- 125000004836 hexamethylene group Chemical group [H]C([H])([*:2])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[*:1] 0.000 claims description 16
- 229910052757 nitrogen Inorganic materials 0.000 claims description 16
- 238000003756 stirring Methods 0.000 claims description 15
- 239000007788 liquid Substances 0.000 claims description 10
- 238000007605 air drying Methods 0.000 claims description 9
- 238000003851 corona treatment Methods 0.000 claims description 9
- 238000012545 processing Methods 0.000 claims description 9
- 102000004190 Enzymes Human genes 0.000 claims description 8
- 108090000790 Enzymes Proteins 0.000 claims description 8
- -1 acrylic ester Chemical class 0.000 claims description 8
- 239000012298 atmosphere Substances 0.000 claims description 8
- 238000005119 centrifugation Methods 0.000 claims description 8
- 238000001035 drying Methods 0.000 claims description 8
- 239000000706 filtrate Substances 0.000 claims description 8
- 238000002390 rotary evaporation Methods 0.000 claims description 8
- 239000000284 extract Substances 0.000 claims description 7
- 238000002360 preparation method Methods 0.000 claims description 6
- FENFUOGYJVOCRY-UHFFFAOYSA-N 1-propoxypropan-2-ol Chemical compound CCCOCC(C)O FENFUOGYJVOCRY-UHFFFAOYSA-N 0.000 claims description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 2
- CUVLMZNMSPJDON-UHFFFAOYSA-N 1-(1-butoxypropan-2-yloxy)propan-2-ol Chemical compound CCCCOCC(C)OCC(C)O CUVLMZNMSPJDON-UHFFFAOYSA-N 0.000 claims 1
- KZHHZKKPQWMHHM-UHFFFAOYSA-N 4-methylhept-2-yne Chemical group CCCC(C)C#CC KZHHZKKPQWMHHM-UHFFFAOYSA-N 0.000 claims 1
- 239000011248 coating agent Substances 0.000 abstract description 18
- 238000000576 coating method Methods 0.000 abstract description 18
- 238000005338 heat storage Methods 0.000 abstract description 8
- 239000002253 acid Substances 0.000 abstract description 2
- QQONPFPTGQHPMA-UHFFFAOYSA-N propylene Natural products CC=C QQONPFPTGQHPMA-UHFFFAOYSA-N 0.000 abstract description 2
- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 abstract description 2
- 239000004814 polyurethane Substances 0.000 description 8
- 238000001914 filtration Methods 0.000 description 7
- MLRKYSNODSLPAB-UHFFFAOYSA-N hex-1-yn-1-ol Chemical group CCCCC#CO MLRKYSNODSLPAB-UHFFFAOYSA-N 0.000 description 7
- 229920002635 polyurethane Polymers 0.000 description 7
- 239000003973 paint Substances 0.000 description 6
- 230000008859 change Effects 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 230000007613 environmental effect Effects 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- IDQBJILTOGBZCR-UHFFFAOYSA-N 1-butoxypropan-1-ol Chemical compound CCCCOC(O)CC IDQBJILTOGBZCR-UHFFFAOYSA-N 0.000 description 2
- 239000000853 adhesive Substances 0.000 description 2
- 230000001070 adhesive effect Effects 0.000 description 2
- 230000007797 corrosion Effects 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 239000003063 flame retardant Substances 0.000 description 2
- 230000006872 improvement Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000011159 matrix material Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000000178 monomer Substances 0.000 description 2
- 231100000252 nontoxic Toxicity 0.000 description 2
- 230000003000 nontoxic effect Effects 0.000 description 2
- 150000003254 radicals Chemical class 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 230000010148 water-pollination Effects 0.000 description 2
- POAOYUHQDCAZBD-UHFFFAOYSA-N 2-butoxyethanol Chemical compound CCCCOCCO POAOYUHQDCAZBD-UHFFFAOYSA-N 0.000 description 1
- 244000248349 Citrus limon Species 0.000 description 1
- 235000005979 Citrus limon Nutrition 0.000 description 1
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 description 1
- 241000196324 Embryophyta Species 0.000 description 1
- JOYRKODLDBILNP-UHFFFAOYSA-N Ethyl urethane Chemical compound CCOC(N)=O JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 description 1
- 229920002488 Hemicellulose Polymers 0.000 description 1
- 239000001913 cellulose Substances 0.000 description 1
- 229920002678 cellulose Polymers 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 238000004132 cross linking Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- POLCUAVZOMRGSN-UHFFFAOYSA-N dipropyl ether Chemical compound CCCOCCC POLCUAVZOMRGSN-UHFFFAOYSA-N 0.000 description 1
- SZXQTJUDPRGNJN-UHFFFAOYSA-N dipropylene glycol Chemical group OCCCOCCCO SZXQTJUDPRGNJN-UHFFFAOYSA-N 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004945 emulsification Methods 0.000 description 1
- 230000009970 fire resistant effect Effects 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 231100001261 hazardous Toxicity 0.000 description 1
- 238000000034 method Methods 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000000049 pigment Substances 0.000 description 1
- 238000004321 preservation Methods 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 239000000057 synthetic resin Substances 0.000 description 1
- 239000002562 thickening agent Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Classifications
-
- 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
-
- 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
- C08F289/00—Macromolecular compounds obtained by polymerising monomers on to macromolecular compounds not provided for in groups C08F251/00 - C08F287/00
-
- 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
- C09D7/60—Additives non-macromolecular
- C09D7/63—Additives non-macromolecular organic
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Paints Or Removers (AREA)
Abstract
The present invention provides a kind of accumulation of heat aqueous polyurethane coating, counts in parts by weight, the accumulation of heat aqueous polyurethane coating includes following raw material：100 parts of aqueous polyurethane dispersion, 0.5 1 parts of wetting dispersing agent, 30 40 parts of water, 1 1.5 parts of antifoaming agent, 0.1 0.6 parts of levelling agent, 35 parts of coalescents, 10 15 parts of propylene acid soluble lignin graft, 24 parts of aqueous polyisocyanates.The coating that the present invention prepares has good heat storage performance.
Description
The application is application No. is 2016101651297, and the applying date is on 03 22nd, 2016, and invention and created name is
A kind of divisional application of the patent of " preparation method of accumulation of heat aqueous polyurethane coating ".
Technical field
The present invention relates to a kind of polyurethane coatings, more particularly to a kind of preparation method of accumulation of heat aqueous polyurethane coating.
Background technology
Polyurethane (PU) coating is the high-grade durable synthetic resin coating to grow up the 1960s, is had excellent
Adhesive force, chemicals-resistant, dicoration and wear-resisting property, be widely used in wooden furniture paint, floor paint, car refinishing paint, anti-
Rotten coating and sapecial coating.Domestic production quotient is concentrated mainly on East China and Central-South coastal cities, the wherein increment of Jiangsu-zhejiang Shanghai Area yield most
Soon, East China PU coating yield accounts for about the 80% of national PU coating yield.
With the improvement of people's life quality, environmental regulation is also increasingly stringenter, various environmental regulations are organic to volatility
Discharge capacity, the content of hazardous solvent of compound (VOC) have stringent limitation.Aqueous polyurethane coating is by the hard of polyurethane coating film
Degree height, strong adhesive force, it is corrosion-resistant, solvent resistant is good the advantages that be combined with the low VOC content of water paint, simultaneously because it is with water
For decentralized medium, so having many advantages, such as nontoxic, nonflammable, free from environmental pollution, energy saving, safe and reliable thus in recent years wide
It is general to be used in all kinds of common coating and functional coating.Aqueous polyurethane coating includes water-soluble type, water emulsification type, water-dispersed
Type can be divided into line style and cross-linking type by molecular structure, all there are two kinds of systems of one-component and two-component.
Publication No. CN102746784B, publication date 2014.11.19, the artificial Jiangsu Rui Feng science and technology industry of application are limited
The Chinese patent of company discloses " a kind of energy-saving heat preserving fire-resistant waterproof anti-corrosion function coating and preparation method thereof ", the functional paint
With aqueous polyurethane dispersion, fire retardant, fire-proof smoke suppressor, hollow glass micropearl, wetting dispersing agent, anti-settling agent, thickener,
Water, levelling agent and antifoaming agent are prepared as a raw material；The functional paint has the function of heat preservation, fire-retardant, waterproof and corrosion-resistant etc., makes
Used time be not easy xanthochromia, safe and reliable, function admirable, with the compatibility of pigment dye it is good, not easy damaged by coating surface, be easy to change
Property, it is nontoxic, safe to use, free from environmental pollution, be suitble to inner-outer wall application, pipeline application, wood furniture application, finishing application, change
Learn the fields such as anticorrosive coating.But, which limits its scope of application there are the undesirable defect of heat storage performance.
Invention content
The technical problem to be solved in the present invention is to provide a kind of preparation methods of accumulation of heat aqueous polyurethane coating, prepare
Coating has good heat storage performance.
In order to solve the above technical problems, the technical scheme is that：
A kind of preparation method of accumulation of heat aqueous polyurethane coating, its step are as follows：
(1) pine nut shell is crushed with pulverizer, crosses 60 mesh sieve, is extracted 40 hours with hexamethylene, ball grinder is used after drying
200rpm rotating speeds are ground 48 hours, obtain pine nut shell powder, will be hydrolyzed 40 hours at 40 DEG C of carboxymethylcelluloenzyme enzyme of pine nut shell powder,
Rinsed with deionized water after centrifugation, it is cold it is dry after obtain enzymolysis lignin；
(2) enzymolysis lignin for obtaining step (1) is added in citric acid solution, flows back under logical nitrogen protection, extracting 3 is small
When, filtered filtration residue is washed with citric acid solution, and concentrated by rotary evaporation after filtrate neutralizes is centrifuged after standing 1 day, washed with hexamethylene
It is dried in vacuo at room temperature after washing, obtains lignin；
(3) lignin that step (2) obtains is put into plasma processing chamber, air atmosphere, vacuum degree 10Pa, electric discharge
Power is corona treatment 4 minutes under 350W, is taken out after closing radio-frequency power supply, vacuum pump successively, it is molten to be immediately placed in acrylic acid
In liquid, lead to nitrogen protection, stirring in water bath 3 hours, is washed after taking-up with deionized water repeatedly at 70 DEG C, and propylene is obtained after air-drying
Acid-lignin graft；
(4) will polyurethane be added blender in, under rotating speed 300rpm be added wetting dispersing agent, water, antifoaming agent, levelling agent,
Coalescents adjust rotating speed and are stirred 20 minutes to 800rpm, acrylic acid-lignin graft that step (3) obtains is added, adjust and turn
Speed stirs 30 minutes to 2400rpm, reduces rotating speed to 400rpm, is stirred 15 minutes after curing agent is added, it is aqueous poly- to obtain accumulation of heat
Urethane coating.
Preferably, in step (2) of the present invention, a concentration of 0.1mol/L of citric acid solution, enzymolysis lignin and lemon
The mass volume ratio of acid solution is 1:20.
Preferably, in step (3) of the present invention, the volume fraction of acrylic acid solution is 16%, and lignin is molten with acrylic acid
The weight ratio of liquid is 1:10.
Preferably, it in step (4) of the present invention, counts in parts by weight, 100 parts of polyurethane, wetting dispersing agent 0.5-1
Part, 30-40 parts of water, 1-1.5 parts of antifoaming agent, 0.1-0.6 parts of levelling agent, 3-5 parts of coalescents, acrylic acid-lignin graft 10-
15 parts, 2-4 parts of curing agent.
Preferably, in step (4) of the present invention, polyurethane is aqueous polyurethane dispersion.
Preferably, in step (4) of the present invention, wetting dispersing agent is nonionic wetting dispersing agent.
Preferably, in step (4) of the present invention, antifoaming agent is dimethylated hexynol.
Preferably, in step (4) of the present invention, levelling agent is acrylic ester type levelling agent.
Preferably, in step (4) of the present invention, coalescents are dipropylene or propylene glycol propyl ether.
Preferably, in step (4) of the present invention, curing agent is aqueous polyisocyanates.
Compared with prior art, the invention has the advantages that：
Pine nut shell is a plant material, and containing a large amount of lignins, cellulose, hemicellulose, wherein lignin can effectively absorb
Infra-red radiation is simultaneously converted to heat, therefore has good heat storage capacity, and the present invention digests after powder is made in pine nut shell, then leads to
It crosses citric acid acidolysis and isolates the higher lignin of purity from pine nut shell powder, but lignin is in hydrophily, and polyurethane matrix is in
Hydrophobicity causes compatibility between the two bad, so lignin of the present invention carries out corona treatment, lignin surface after processing
Free radical is produced, while increasing surface area, free radical produces peroxy radical in air, is put into acrylic acid solution
Graft reaction has occurred with acrylic monomers, since acrylic monomers is in hydrophobicity, its hydrophily becomes after lignin grafting
Compatibility between hydrophobicity, with polyurethane matrix has obtained larger improvement, therebetween forms stronger interface knot
It closes so that the heat storage performance of coating is greatly improved；The discarded of pine nut generation later is eaten in addition, pine nut shell is people
Object, it is cheap and easy to get, manufacturing cost is reduced, and turn waste into wealth, there is good economic value and the value of environmental protection.
Specific implementation mode
Below in conjunction with specific embodiment, the present invention will be described in detail, herein illustrative examples and explanation of the invention
For explaining the present invention, but it is not as a limitation of the invention.
Embodiment 1
Accumulation of heat aqueous polyurethane coating is prepared according to the following steps：
(1) pine nut shell is crushed with pulverizer, crosses 60 mesh sieve, is extracted 40 hours with hexamethylene, ball grinder is used after drying
200rpm rotating speeds are ground 48 hours, obtain pine nut shell powder, will be hydrolyzed 40 hours at 40 DEG C of carboxymethylcelluloenzyme enzyme of pine nut shell powder,
Rinsed with deionized water after centrifugation, it is cold it is dry after obtain enzymolysis lignin；
(2) enzymolysis lignin that step (1) obtains is added in the citric acid solution of a concentration of 0.1mol/L, enzymolysis lignin with
The mass volume ratio of citric acid solution is 1:20, lead under nitrogen protection and flow back, extracts 3 hours, filtered filtration residue citric acid is molten
Liquid washs, and concentrated by rotary evaporation after filtrate neutralizes centrifuges after standing 1 day, is dried in vacuo, obtains at room temperature after being washed with hexamethylene
Lignin；
(3) lignin that step (2) obtains is put into plasma processing chamber, air atmosphere, vacuum degree 10Pa, electric discharge
Power is corona treatment 4 minutes under 350W, is taken out after closing radio-frequency power supply, vacuum pump successively, is immediately placed in volume fraction
For in 16% acrylic acid solution, the weight ratio of lignin and acrylic acid solution is 1:10, lead to nitrogen protection, stirring in water bath at 70 DEG C
It 3 hours, is washed repeatedly with deionized water after taking-up, acrylic acid-lignin graft is obtained after air-drying；
(4) it counts in parts by weight, 100 parts of aqueous polyurethane dispersion is added in blender, are added under rotating speed 300rpm
0.5 part of nonionic wetting dispersing agent, 40 parts of water, 1.2 parts of dimethylated hexynols, 0.5 part of acrylic ester type levelling agent, 3.5 parts
Propylene glycol propyl ether adjusts rotating speed and is stirred 20 minutes to 800rpm, acrylic acid-lignin graft that 11 parts of steps (3) obtain is added,
It adjusts rotating speed to stir 30 minutes to 2400rpm, reduces rotating speed to 400rpm, 15 points are stirred after 3 parts of aqueous polyisocyanates are added
Clock obtains accumulation of heat aqueous polyurethane coating.
Embodiment 2
Accumulation of heat aqueous polyurethane coating is prepared according to the following steps：
(1) pine nut shell is crushed with pulverizer, crosses 60 mesh sieve, is extracted 40 hours with hexamethylene, ball grinder is used after drying
200rpm rotating speeds are ground 48 hours, obtain pine nut shell powder, will be hydrolyzed 40 hours at 40 DEG C of carboxymethylcelluloenzyme enzyme of pine nut shell powder,
Rinsed with deionized water after centrifugation, it is cold it is dry after obtain enzymolysis lignin；
(2) enzymolysis lignin that step (1) obtains is added in the citric acid solution of a concentration of 0.1mol/L, enzymolysis lignin with
The mass volume ratio of citric acid solution is 1:20, lead under nitrogen protection and flow back, extracts 3 hours, filtered filtration residue citric acid is molten
Liquid washs, and concentrated by rotary evaporation after filtrate neutralizes centrifuges after standing 1 day, is dried in vacuo, obtains at room temperature after being washed with hexamethylene
Lignin；
(3) lignin that step (2) obtains is put into plasma processing chamber, air atmosphere, vacuum degree 10Pa, electric discharge
Power is corona treatment 4 minutes under 350W, is taken out after closing radio-frequency power supply, vacuum pump successively, is immediately placed in volume fraction
For in 16% acrylic acid solution, the weight ratio of lignin and acrylic acid solution is 1:10, lead to nitrogen protection, stirring in water bath at 70 DEG C
It 3 hours, is washed repeatedly with deionized water after taking-up, acrylic acid-lignin graft is obtained after air-drying；
(4) it counts in parts by weight, 100 parts of aqueous polyurethane dispersion is added in blender, are added under rotating speed 300rpm
0.7 part of nonionic wetting dispersing agent, 32 parts of water, 1 part of dimethylated hexynol, 0.6 part of acrylic ester type levelling agent, 4 parts of dipropyls
Glycol butyl ether adjusts rotating speed and is stirred 20 minutes to 800rpm, acrylic acid-lignin graft that 13 parts of steps (3) obtain is added, adjusts
It saves rotating speed to stir 30 minutes to 2400rpm, reduces rotating speed to 400rpm, 15 points are stirred after 2.5 parts of aqueous polyisocyanates are added
Clock obtains accumulation of heat aqueous polyurethane coating.
Embodiment 3
Accumulation of heat aqueous polyurethane coating is prepared according to the following steps：
(1) pine nut shell is crushed with pulverizer, crosses 60 mesh sieve, is extracted 40 hours with hexamethylene, ball grinder is used after drying
200rpm rotating speeds are ground 48 hours, obtain pine nut shell powder, will be hydrolyzed 40 hours at 40 DEG C of carboxymethylcelluloenzyme enzyme of pine nut shell powder,
Rinsed with deionized water after centrifugation, it is cold it is dry after obtain enzymolysis lignin；
(2) enzymolysis lignin that step (1) obtains is added in the citric acid solution of a concentration of 0.1mol/L, enzymolysis lignin with
The mass volume ratio of citric acid solution is 1:20, lead under nitrogen protection and flow back, extracts 3 hours, filtered filtration residue citric acid is molten
Liquid washs, and concentrated by rotary evaporation after filtrate neutralizes centrifuges after standing 1 day, is dried in vacuo, obtains at room temperature after being washed with hexamethylene
Lignin；
(3) lignin that step (2) obtains is put into plasma processing chamber, air atmosphere, vacuum degree 10Pa, electric discharge
Power is corona treatment 4 minutes under 350W, is taken out after closing radio-frequency power supply, vacuum pump successively, is immediately placed in volume fraction
For in 16% acrylic acid solution, the weight ratio of lignin and acrylic acid solution is 1:10, lead to nitrogen protection, stirring in water bath at 70 DEG C
It 3 hours, is washed repeatedly with deionized water after taking-up, acrylic acid-lignin graft is obtained after air-drying；
(4) it counts in parts by weight, 100 parts of aqueous polyurethane dispersion is added in blender, are added under rotating speed 300rpm
0.9 part of nonionic wetting dispersing agent, 35 parts of water, 1.5 parts of dimethylated hexynols, 0.1 part of acrylic ester type levelling agent, 4.8 parts
Propylene glycol propyl ether adjusts rotating speed and is stirred 20 minutes to 800rpm, acrylic acid-lignin graft that 12 parts of steps (3) obtain is added,
It adjusts rotating speed to stir 30 minutes to 2400rpm, reduces rotating speed to 400rpm, 15 points are stirred after 4 parts of aqueous polyisocyanates are added
Clock obtains accumulation of heat aqueous polyurethane coating.
Embodiment 4
Accumulation of heat aqueous polyurethane coating is prepared according to the following steps：
(1) pine nut shell is crushed with pulverizer, crosses 60 mesh sieve, is extracted 40 hours with hexamethylene, ball grinder is used after drying
200rpm rotating speeds are ground 48 hours, obtain pine nut shell powder, will be hydrolyzed 40 hours at 40 DEG C of carboxymethylcelluloenzyme enzyme of pine nut shell powder,
Rinsed with deionized water after centrifugation, it is cold it is dry after obtain enzymolysis lignin；
(2) enzymolysis lignin that step (1) obtains is added in the citric acid solution of a concentration of 0.1mol/L, enzymolysis lignin with
The mass volume ratio of citric acid solution is 1:20, lead under nitrogen protection and flow back, extracts 3 hours, filtered filtration residue citric acid is molten
Liquid washs, and concentrated by rotary evaporation after filtrate neutralizes centrifuges after standing 1 day, is dried in vacuo, obtains at room temperature after being washed with hexamethylene
Lignin；
(3) lignin that step (2) obtains is put into plasma processing chamber, air atmosphere, vacuum degree 10Pa, electric discharge
Power is corona treatment 4 minutes under 350W, is taken out after closing radio-frequency power supply, vacuum pump successively, is immediately placed in volume fraction
For in 16% acrylic acid solution, the weight ratio of lignin and acrylic acid solution is 1:10, lead to nitrogen protection, stirring in water bath at 70 DEG C
It 3 hours, is washed repeatedly with deionized water after taking-up, acrylic acid-lignin graft is obtained after air-drying；
(4) it counts in parts by weight, 100 parts of aqueous polyurethane dispersion is added in blender, are added under rotating speed 300rpm
0.6 part of nonionic wetting dispersing agent, 36 parts of water, 1.4 parts of dimethylated hexynols, 0.2 part of acrylic ester type levelling agent, 3 part two
Propandiol butyl ether adjusts rotating speed and is stirred 20 minutes to 800rpm, acrylic acid-lignin graft that 15 parts of steps (3) obtain is added,
It adjusts rotating speed to stir 30 minutes to 2400rpm, reduces rotating speed to 400rpm, 15 points are stirred after 2 parts of aqueous polyisocyanates are added
Clock obtains accumulation of heat aqueous polyurethane coating.
Embodiment 5
Accumulation of heat aqueous polyurethane coating is prepared according to the following steps：
(1) pine nut shell is crushed with pulverizer, crosses 60 mesh sieve, is extracted 40 hours with hexamethylene, ball grinder is used after drying
200rpm rotating speeds are ground 48 hours, obtain pine nut shell powder, will be hydrolyzed 40 hours at 40 DEG C of carboxymethylcelluloenzyme enzyme of pine nut shell powder,
Rinsed with deionized water after centrifugation, it is cold it is dry after obtain enzymolysis lignin；
(2) enzymolysis lignin that step (1) obtains is added in the citric acid solution of a concentration of 0.1mol/L, enzymolysis lignin with
The mass volume ratio of citric acid solution is 1:20, lead under nitrogen protection and flow back, extracts 3 hours, filtered filtration residue citric acid is molten
Liquid washs, and concentrated by rotary evaporation after filtrate neutralizes centrifuges after standing 1 day, is dried in vacuo, obtains at room temperature after being washed with hexamethylene
Lignin；
(3) lignin that step (2) obtains is put into plasma processing chamber, air atmosphere, vacuum degree 10Pa, electric discharge
Power is corona treatment 4 minutes under 350W, is taken out after closing radio-frequency power supply, vacuum pump successively, is immediately placed in volume fraction
For in 16% acrylic acid solution, the weight ratio of lignin and acrylic acid solution is 1:10, lead to nitrogen protection, stirring in water bath at 70 DEG C
It 3 hours, is washed repeatedly with deionized water after taking-up, acrylic acid-lignin graft is obtained after air-drying；
(4) it counts in parts by weight, 100 parts of aqueous polyurethane dispersion is added in blender, are added under rotating speed 300rpm
0.8 part of nonionic wetting dispersing agent, 39 parts of water, 1.1 parts of dimethylated hexynols, 0.4 part of acrylic ester type levelling agent, 5 part two
Propandiol butyl ether adjusts rotating speed and is stirred 20 minutes to 800rpm, acrylic acid-lignin graft that 10 parts of steps (3) obtain is added,
It adjusts rotating speed to stir 30 minutes to 2400rpm, reduces rotating speed to 400rpm, 15 are stirred after 3.5 parts of aqueous polyisocyanates are added
Minute, obtain accumulation of heat aqueous polyurethane coating.
Embodiment 6
Accumulation of heat aqueous polyurethane coating is prepared according to the following steps：
(1) pine nut shell is crushed with pulverizer, crosses 60 mesh sieve, is extracted 40 hours with hexamethylene, ball grinder is used after drying
200rpm rotating speeds are ground 48 hours, obtain pine nut shell powder, will be hydrolyzed 40 hours at 40 DEG C of carboxymethylcelluloenzyme enzyme of pine nut shell powder,
Rinsed with deionized water after centrifugation, it is cold it is dry after obtain enzymolysis lignin；
(2) enzymolysis lignin that step (1) obtains is added in the citric acid solution of a concentration of 0.1mol/L, enzymolysis lignin with
The mass volume ratio of citric acid solution is 1:20, lead under nitrogen protection and flow back, extracts 3 hours, filtered filtration residue citric acid is molten
Liquid washs, and concentrated by rotary evaporation after filtrate neutralizes centrifuges after standing 1 day, is dried in vacuo, obtains at room temperature after being washed with hexamethylene
Lignin；
(3) lignin that step (2) obtains is put into plasma processing chamber, air atmosphere, vacuum degree 10Pa, electric discharge
Power is corona treatment 4 minutes under 350W, is taken out after closing radio-frequency power supply, vacuum pump successively, is immediately placed in volume fraction
For in 16% acrylic acid solution, the weight ratio of lignin and acrylic acid solution is 1:10, lead to nitrogen protection, stirring in water bath at 70 DEG C
It 3 hours, is washed repeatedly with deionized water after taking-up, acrylic acid-lignin graft is obtained after air-drying；
(4) it counts in parts by weight, 100 parts of aqueous polyurethane dispersion is added in blender, 1 is added under rotating speed 300rpm
Part nonionic wetting dispersing agent, 30 parts of water, 1.3 parts of dimethylated hexynols, 0.3 part of acrylic ester type levelling agent, 4.5 parts the third two
Alcohol propyl ether adjusts rotating speed and is stirred 20 minutes to 800rpm, acrylic acid-lignin graft that 14 parts of steps (3) obtain is added, adjusts
Rotating speed stirs 30 minutes to 2400rpm, reduces rotating speed to 400rpm, is stirred 15 minutes after 2.8 parts of aqueous polyisocyanates are added,
Obtain accumulation of heat aqueous polyurethane coating.
Coating made from embodiment 1-6 and the heat storage performance of comparative example are tested, wherein comparative example is publication number
For the Chinese patent of CN102746784B, heat storage performance test process is：Each coating is coated on substrate surface, is put into after air-drying
It being equipped in the chamber of infrared lamp, for infrared lamp apart from substrate 20cm, thermal detector, which is fixed, makes it be contacted with base lower surface,
It opens infrared lamp to be irradiated, the temperature of base material under different time sections is recorded by thermal detector, as a result see the table below：
As seen from the above table, it is apparent high in the temperature of each period after coating produced by the present invention is coated on substrate
In comparative example, good heat storage performance is shown.
The above-described embodiments merely illustrate the principles and effects of the present invention, and is not intended to limit the present invention.It is any ripe
The personage for knowing this technology can all carry out modifications and changes to above-described embodiment without violating the spirit and scope of the present invention.Cause
This, institute is complete without departing from the spirit and technical ideas disclosed in the present invention by those of ordinary skill in the art such as
At all equivalent modifications or change, should by the present invention claim be covered.
Claims (8)
1. a kind of accumulation of heat aqueous polyurethane coating, which is characterized in that count in parts by weight, the accumulation of heat aqueous polyurethane coating packet
Include following raw material：100 parts of aqueous polyurethane dispersion, 0.5-1 parts of wetting dispersing agent, 30-40 parts of water, 1-1.5 parts of antifoaming agent, stream
Flat agent 0.1-0.6 parts, 3-5 parts of coalescents, acrylic acid -10-15 parts of lignin graft, aqueous polyisocyanates 2-4 parts.
2. accumulation of heat aqueous polyurethane coating according to claim 1, which is characterized in that the acrylic acid-lignin graft
Preparation method, include the following steps：
(1) pine nut shell is crushed with pulverizer, crosses 60 mesh sieve, extracted 40 hours with hexamethylene, ball grinder 200rpm is used after drying
Rotating speed is ground 48 hours, obtains pine nut shell powder, will hydrolyze 40 hours at 40 DEG C of carboxymethylcelluloenzyme enzyme of pine nut shell powder, centrifugation divides
Rinsed with deionized water from rear, it is cold it is dry after obtain enzymolysis lignin；
(2) enzymolysis lignin for obtaining step (1) is added in citric acid solution, flows back, extracts 3 hours, mistake under logical nitrogen protection
Filter residue is washed with citric acid solution after filter, and concentrated by rotary evaporation after filtrate neutralizes centrifuges after standing 1 day, after being washed with hexamethylene
It is dried in vacuo at room temperature, obtains lignin；
(3) lignin that step (2) obtains is put into plasma processing chamber, air atmosphere, vacuum degree 10Pa, discharge power
For corona treatment under 350W 4 minutes, takes out, is immediately placed in acrylic acid solution after closing radio-frequency power supply, vacuum pump successively,
Logical nitrogen protection, stirring in water bath 3 hours, is washed after taking-up with deionized water, acrylic acid-lignin is obtained after air-drying repeatedly at 70 DEG C
Graft.
3. accumulation of heat aqueous polyurethane coating according to claim 2, it is characterised in that：In the step (2), citric acid is molten
The mass volume ratio of a concentration of 0.1mol/L of liquid, enzymolysis lignin and citric acid solution is 1:20.
4. accumulation of heat aqueous polyurethane coating according to claim 2, it is characterised in that：In the step (3), acrylic acid is molten
The volume fraction of liquid is 16%, and the weight ratio of lignin and acrylic acid solution is 1:10.
5. accumulation of heat aqueous polyurethane coating according to claim 1, it is characterised in that：The wetting dispersing agent is nonionic
Type wetting dispersing agent.
6. accumulation of heat aqueous polyurethane coating according to claim 1, which is characterized in that the antifoaming agent is dimethylhexyne
Alcohol.
7. accumulation of heat aqueous polyurethane coating according to claim 1, which is characterized in that the levelling agent is acrylic ester type
Levelling agent.
8. accumulation of heat aqueous polyurethane coating according to claim 1, it is characterised in that：The coalescents are dipropylene glycol
Butyl ether or propylene glycol propyl ether.
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| CN201810241025.9A CN108384421A (en) | 2016-03-22 | 2016-03-22 | A kind of accumulation of heat aqueous polyurethane coating |
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| CN201610165129.7A CN105670479B (en) | 2016-03-22 | 2016-03-22 | A kind of preparation method of water storage polyurethane coating |
| CN201810241025.9A CN108384421A (en) | 2016-03-22 | 2016-03-22 | A kind of accumulation of heat aqueous polyurethane coating |
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| CN113881010A (en) * | 2021-09-09 | 2022-01-04 | 上海鹤城高分子科技有限公司 | A kind of high-strength yellowing-resistant polyurethane floor lamp cover and preparation method thereof |
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| CN105670479A (en) | 2016-06-15 |
| CN105670479B (en) | 2018-04-10 |
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Application publication date: 20180810 |