CN105038571B - Heat resistant type vegetable oil based polyurethane floor coatings and preparation method thereof - Google Patents
Heat resistant type vegetable oil based polyurethane floor coatings and preparation method thereof Download PDFInfo
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- 235000015112 vegetable and seed oil Nutrition 0.000 title claims abstract description 90
- 239000008158 vegetable oil Substances 0.000 title claims abstract description 90
- 238000000576 coating method Methods 0.000 title claims abstract description 53
- 239000004814 polyurethane Substances 0.000 title claims abstract description 46
- 229920002635 polyurethane Polymers 0.000 title claims abstract description 46
- 238000002360 preparation method Methods 0.000 title claims abstract description 46
- 239000002994 raw material Substances 0.000 claims abstract description 43
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 35
- 239000008367 deionised water Substances 0.000 claims abstract description 34
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 34
- 239000000843 powder Substances 0.000 claims abstract description 33
- 239000011248 coating agent Substances 0.000 claims abstract description 32
- 229910021536 Zeolite Inorganic materials 0.000 claims abstract description 22
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims abstract description 22
- 239000010457 zeolite Substances 0.000 claims abstract description 22
- 239000000203 mixture Substances 0.000 claims abstract description 17
- 239000005995 Aluminium silicate Substances 0.000 claims abstract description 13
- 235000012211 aluminium silicate Nutrition 0.000 claims abstract description 13
- 239000012948 isocyanate Substances 0.000 claims abstract description 13
- 150000002513 isocyanates Chemical class 0.000 claims abstract description 13
- NLYAJNPCOHFWQQ-UHFFFAOYSA-N kaolin Chemical compound O.O.O=[Al]O[Si](=O)O[Si](=O)O[Al]=O NLYAJNPCOHFWQQ-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000003607 modifier Substances 0.000 claims abstract description 13
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000000049 pigment Substances 0.000 claims abstract description 12
- 239000003054 catalyst Substances 0.000 claims abstract description 9
- 239000003995 emulsifying agent Substances 0.000 claims abstract description 9
- 150000005846 sugar alcohols Polymers 0.000 claims abstract description 5
- 229920005862 polyol Polymers 0.000 claims description 41
- 150000003077 polyols Chemical class 0.000 claims description 41
- 238000003756 stirring Methods 0.000 claims description 38
- WMFOQBRAJBCJND-UHFFFAOYSA-M Lithium hydroxide Chemical compound [Li+].[OH-] WMFOQBRAJBCJND-UHFFFAOYSA-M 0.000 claims description 24
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 17
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 15
- MTHSVFCYNBDYFN-UHFFFAOYSA-N diethylene glycol Chemical compound OCCOCCO MTHSVFCYNBDYFN-UHFFFAOYSA-N 0.000 claims description 15
- 239000004359 castor oil Substances 0.000 claims description 12
- 235000019438 castor oil Nutrition 0.000 claims description 12
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 claims description 12
- 239000010453 quartz Substances 0.000 claims description 10
- 125000001931 aliphatic group Chemical group 0.000 claims description 9
- 239000000839 emulsion Substances 0.000 claims description 9
- RNMDNPCBIKJCQP-UHFFFAOYSA-N 5-nonyl-7-oxabicyclo[4.1.0]hepta-1,3,5-trien-2-ol Chemical compound C(CCCCCCCC)C1=C2C(=C(C=C1)O)O2 RNMDNPCBIKJCQP-UHFFFAOYSA-N 0.000 claims description 8
- RSWGJHLUYNHPMX-UHFFFAOYSA-N Abietic-Saeure Natural products C12CCC(C(C)C)=CC2=CCC2C1(C)CCCC2(C)C(O)=O RSWGJHLUYNHPMX-UHFFFAOYSA-N 0.000 claims description 8
- KHPCPRHQVVSZAH-HUOMCSJISA-N Rosin Natural products O(C/C=C/c1ccccc1)[C@H]1[C@H](O)[C@@H](O)[C@@H](O)[C@@H](CO)O1 KHPCPRHQVVSZAH-HUOMCSJISA-N 0.000 claims description 8
- -1 polyoxyethylene nonylphenol Polymers 0.000 claims description 8
- KHPCPRHQVVSZAH-UHFFFAOYSA-N trans-cinnamyl beta-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OCC=CC1=CC=CC=C1 KHPCPRHQVVSZAH-UHFFFAOYSA-N 0.000 claims description 8
- 125000003118 aryl group Chemical group 0.000 claims description 7
- 238000009924 canning Methods 0.000 claims description 7
- 239000000945 filler Substances 0.000 claims description 7
- 239000011261 inert gas Substances 0.000 claims description 7
- 238000004806 packaging method and process Methods 0.000 claims description 7
- LGRFSURHDFAFJT-UHFFFAOYSA-N Phthalic anhydride Natural products C1=CC=C2C(=O)OC(=O)C2=C1 LGRFSURHDFAFJT-UHFFFAOYSA-N 0.000 claims description 6
- JHIWVOJDXOSYLW-UHFFFAOYSA-N butyl 2,2-difluorocyclopropane-1-carboxylate Chemical compound CCCCOC(=O)C1CC1(F)F JHIWVOJDXOSYLW-UHFFFAOYSA-N 0.000 claims description 6
- KXGFMDJXCMQABM-UHFFFAOYSA-N 2-methoxy-6-methylphenol Chemical compound [CH]OC1=CC=CC([CH])=C1O KXGFMDJXCMQABM-UHFFFAOYSA-N 0.000 claims description 5
- 239000005058 Isophorone diisocyanate Substances 0.000 claims description 5
- 235000019482 Palm oil Nutrition 0.000 claims description 5
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 5
- ZJCCRDAZUWHFQH-UHFFFAOYSA-N Trimethylolpropane Chemical compound CCC(CO)(CO)CO ZJCCRDAZUWHFQH-UHFFFAOYSA-N 0.000 claims description 5
- 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 5
- 239000000944 linseed oil Substances 0.000 claims description 5
- 235000021388 linseed oil Nutrition 0.000 claims description 5
- 239000002540 palm oil Substances 0.000 claims description 5
- 239000003549 soybean oil Substances 0.000 claims description 5
- 235000012424 soybean oil Nutrition 0.000 claims description 5
- 239000002202 Polyethylene glycol Substances 0.000 claims description 4
- 229920001568 phenolic resin Polymers 0.000 claims description 4
- 239000005011 phenolic resin Substances 0.000 claims description 4
- 229920001223 polyethylene glycol Polymers 0.000 claims description 4
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 4
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 4
- 229920003987 resole Polymers 0.000 claims description 4
- 229920000538 Poly[(phenyl isocyanate)-co-formaldehyde] Polymers 0.000 claims description 3
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 3
- 239000003973 paint Substances 0.000 claims description 3
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 claims description 3
- 239000013638 trimer Substances 0.000 claims description 3
- HIFVAOIJYDXIJG-UHFFFAOYSA-N benzylbenzene;isocyanic acid Chemical group N=C=O.N=C=O.C=1C=CC=CC=1CC1=CC=CC=C1 HIFVAOIJYDXIJG-UHFFFAOYSA-N 0.000 claims description 2
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims description 2
- 229920000642 polymer Polymers 0.000 claims description 2
- 150000008064 anhydrides Chemical group 0.000 claims 1
- 235000013312 flour Nutrition 0.000 abstract 1
- 239000000377 silicon dioxide Substances 0.000 abstract 1
- 230000015572 biosynthetic process Effects 0.000 description 8
- 239000000463 material Substances 0.000 description 7
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 235000011187 glycerol Nutrition 0.000 description 5
- 239000001056 green pigment Substances 0.000 description 5
- 239000002304 perfume Substances 0.000 description 4
- 239000011527 polyurethane coating Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 238000009408 flooring Methods 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 3
- UPMLOUAZCHDJJD-UHFFFAOYSA-N 4,4'-Diphenylmethane Diisocyanate Chemical group C1=CC(N=C=O)=CC=C1CC1=CC=C(N=C=O)C=C1 UPMLOUAZCHDJJD-UHFFFAOYSA-N 0.000 description 2
- 241001596784 Pegasus Species 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- NJTGANWAUPEOAX-UHFFFAOYSA-N molport-023-220-454 Chemical compound OCC(O)CO.OCC(O)CO NJTGANWAUPEOAX-UHFFFAOYSA-N 0.000 description 2
- 229920002565 Polyethylene Glycol 400 Polymers 0.000 description 1
- 125000004018 acid anhydride group Chemical group 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000006115 industrial coating Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229930014626 natural product Natural products 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 125000003367 polycyclic group Chemical group 0.000 description 1
- 230000008092 positive effect Effects 0.000 description 1
- 238000003847 radiation curing Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
Landscapes
- Polyurethanes Or Polyureas (AREA)
- Paints Or Removers (AREA)
Abstract
Description
技术领域technical field
本发明涉及涂料技术领域,尤其涉及地坪涂料技术领域,具体的是一种耐热型植物油基聚氨酯地坪涂料及其制备方法。The invention relates to the technical field of coatings, in particular to the technical field of floor coatings, in particular to a heat-resistant vegetable oil-based polyurethane floor coating and a preparation method thereof.
技术背景technical background
随着化石资源的日益枯竭以及人们环保意识的日益增强,社会需求已经对涂料行业提出了新的要求,即发展环保、高性能、水性无溶剂、高固体份、粉末和辐射固化的新型涂料。而在目前的涂料中聚氨酯涂料的应用是非常广泛的,有普通涂料,有特种涂料,有工业涂料,有建筑涂料,几乎到处都有聚氨酯涂料的痕迹。在聚氨酯涂料的制造中,植物油由于是可再生资源,其来源广泛,将含羟基的植物油或者羟基化的植物油作为多元醇来制备聚氨酯涂料已经受到人们的关注。由于植物油基多元醇具有多羟基结构,能形成三维交联结构,将其用来制备聚氨酯地坪涂料应该具有良好的物理化学性能。With the depletion of fossil resources and the increasing awareness of environmental protection, social needs have put forward new requirements for the coatings industry, namely the development of new coatings with environmental protection, high performance, water-based solvent-free, high solids, powder and radiation curing. The application of polyurethane coatings in current coatings is very extensive. There are common coatings, special coatings, industrial coatings, and architectural coatings. There are traces of polyurethane coatings almost everywhere. In the manufacture of polyurethane coatings, vegetable oil is a renewable resource with a wide range of sources. The use of hydroxyl-containing vegetable oils or hydroxylated vegetable oils as polyols to prepare polyurethane coatings has attracted people's attention. Since vegetable oil-based polyols have a multi-hydroxyl structure and can form a three-dimensional cross-linked structure, they should have good physical and chemical properties when used to prepare polyurethane floor coatings.
中国专利201210267256.X和201210291182.3公开了:将植物油作为原料以制备聚氨酯地坪材料。但是,由于植物油的长链结构为脂肪族直链,柔性较强,因此,用其制备的聚氨酯材料的力学性能和耐热性能不够理想。Chinese patents 201210267256.X and 201210291182.3 disclose: using vegetable oil as a raw material to prepare polyurethane flooring materials. However, since the long-chain structure of vegetable oil is aliphatic straight chain and has strong flexibility, the mechanical properties and heat resistance of polyurethane materials prepared with it are not ideal.
为了提高植物油基聚氨酯地坪的耐热性,中国专利200810036486.9和200810036487.3公开了:在植物油基聚氨酯地坪涂料中引入苯酐与多元醇的缩合物。由于它们采用的是物理混合法,所以对植物油基聚氨酯地坪涂料耐热性的提升不理想。In order to improve the heat resistance of vegetable oil-based polyurethane flooring, Chinese patents 200810036486.9 and 200810036487.3 disclose the introduction of condensates of phthalic anhydride and polyols into vegetable oil-based polyurethane flooring coatings. Because they use the physical mixing method, they are not ideal for improving the heat resistance of vegetable oil-based polyurethane floor coatings.
美国专利US19750567074和US19760704945公开了:植物油基聚氨酯混凝土地坪的组成和制备方法,其通过物理混合法引入了松香改性的酚醛树脂,对混凝土地坪的耐热性有了一定的改善,但提升效果不明显。U.S. Patents US19750567074 and US19760704945 disclosed: the composition and preparation method of vegetable oil-based polyurethane concrete floor, which introduces rosin-modified phenolic resin through physical mixing method, and the heat resistance of concrete floor has been improved to a certain extent, but the improvement no significant effect.
发明内容Contents of the invention
本发明的目的在于克服现有技术的不足,提供一种耐热型植物油基聚氨酯地坪涂料,它通过采用具有芳环或者多元环结构的改性剂对植物油基多元醇进行改性,能提高链段的刚性,使所制备的聚氨酯地坪涂料具有良好的耐热性和力学性能。本发明的第二目的是,提供所述耐热型植物油基聚氨酯地坪涂料的制备方法。The purpose of the present invention is to overcome the deficiencies in the prior art, and to provide a heat-resistant vegetable oil-based polyurethane floor coating, which is modified by using a modifier with an aromatic ring or a polycyclic ring structure to modify the vegetable oil-based polyol, which can improve The rigidity of the chain segment makes the prepared polyurethane floor coating have good heat resistance and mechanical properties. The second object of the present invention is to provide a preparation method of the heat-resistant vegetable oil-based polyurethane floor coating.
为实现上述发明目的,本发明采用了以下技术方案。In order to realize the purpose of the above invention, the present invention adopts the following technical solutions.
一种耐热型植物油基聚氨酯地坪涂料,其特征在于,含有A、B、C三个组份,A heat-resistant vegetable oil-based polyurethane floor coating is characterized in that it contains three components A, B and C,
所述A组份为植物油基多元醇乳液,其中各原料的重量份组成为:The A component is a vegetable oil-based polyol emulsion, wherein the parts by weight of each raw material are composed of:
植物油:100重量份;Vegetable oil: 100 parts by weight;
多元醇:5~20重量份;Polyol: 5-20 parts by weight;
耐热改性剂:10~30重量份;Heat-resistant modifier: 10-30 parts by weight;
催化剂:0.3~1重量份;Catalyst: 0.3 to 1 part by weight;
乳化剂:3~5重量份;Emulsifier: 3 to 5 parts by weight;
去离子水:60~120重量份;Deionized water: 60-120 parts by weight;
所述B组分为具有刚性链段的异氰酸酯;The B component is an isocyanate with a rigid segment;
所述C组分中各原料的重量份组成为:The parts by weight of each raw material in the C component consist of:
颜料:1~5重量份;Pigment: 1 to 5 parts by weight;
沸石粉:5~10重量份;Zeolite powder: 5-10 parts by weight;
高岭土或石英粉:20~30重量份;Kaolin or quartz powder: 20-30 parts by weight;
去离子水:30~60重量份;Deionized water: 30-60 parts by weight;
所述A组份、B组份与C组份按重量比A:B:C=2:1~3:0.5~1配合使用。The components A, B and C are used together in a weight ratio of A:B:C=2:1-3:0.5-1.
进一步,所述植物油为蓖麻油、大豆油、亚麻油或棕榈油的一种。Further, the vegetable oil is one of castor oil, soybean oil, linseed oil or palm oil.
进一步,所述多元醇为脂肪族多元醇,为乙二醇、一缩二乙二醇、丙三醇或三羟甲基丙烷的一种。Further, the polyhydric alcohol is an aliphatic polyhydric alcohol, which is one of ethylene glycol, diethylene glycol, glycerol or trimethylolpropane.
进一步,所述耐热改性剂为拥有芳环或脂肪环结构并含有羟基、羧基或酸酐基团的化合物或者低分子聚合物。Further, the heat-resistant modifier is a compound or a low-molecular polymer having an aromatic ring or aliphatic ring structure and containing a hydroxyl group, a carboxyl group or an acid anhydride group.
进一步,所述耐热改性剂为甲阶酚醛树脂、松香或苯酐的一种。Further, the heat-resistant modifier is one of resole phenolic resin, rosin or phthalic anhydride.
进一步,所述催化剂为钛酸酯或氢氧化锂的一种。Further, the catalyst is one of titanate or lithium hydroxide.
进一步,所述乳化剂为聚氧化乙烯壬基酚醚、聚乙二醇双油酸酯、蓖麻油聚氧乙烯醚的一种或两种。Further, the emulsifier is one or two of polyoxyethylene nonylphenol ether, polyethylene glycol dioleate, and castor oil polyoxyethylene ether.
进一步,所述异氰酸酯为含有芳环或脂肪环刚性结构的异氰酸酯。Further, the isocyanate is an isocyanate containing an aromatic ring or an aliphatic ring rigid structure.
进一步,所述异氰酸酯为为改性二苯基甲烷二异氰酸酯、甲苯二异氰酸酯三聚体、异氟尔酮二异氰酸酯或聚甲撑聚苯基异氰酸酯的一种。Further, the isocyanate is one of modified diphenylmethane diisocyanate, toluene diisocyanate trimer, isophorone diisocyanate or polymethylene polyphenylisocyanate.
为实现上述第二目的,本发明采用了以下技术方案。In order to achieve the above-mentioned second purpose, the present invention adopts the following technical solutions.
一种耐热型植物油基聚氨酯地坪涂料的制备方法,其特征在于,包含以下步骤:A preparation method of heat-resistant vegetable oil-based polyurethane floor coating, is characterized in that, comprises the following steps:
(1)原料准备(1) Raw material preparation
①所述耐热型植物油基聚氨酯地坪涂料含有A、B、C三个组份,①The heat-resistant vegetable oil-based polyurethane floor coating contains three components A, B, and C,
所述A组份中各原料的重量份组成为:The parts by weight of each raw material in the described A component consist of:
植物油:100重量份;Vegetable oil: 100 parts by weight;
多元醇:5~20重量份;Polyol: 5-20 parts by weight;
耐热改性剂:10~30重量份;Heat-resistant modifier: 10-30 parts by weight;
催化剂:0.3~1重量份;Catalyst: 0.3 to 1 part by weight;
乳化剂:3~5重量份;Emulsifier: 3 to 5 parts by weight;
去离子水:60~120重量份;Deionized water: 60-120 parts by weight;
所述B组分为具有刚性链段的异氰酸酯;The B component is an isocyanate with a rigid segment;
所述C组分填料中各原料的重量份组成为:The parts by weight of each raw material in the C component filler consist of:
颜料:1~5重量份;Pigment: 1 to 5 parts by weight;
沸石粉:5~10重量份;Zeolite powder: 5-10 parts by weight;
高岭土或石英粉:20~30重量份;Kaolin or quartz powder: 20-30 parts by weight;
去离子水:30~60重量份;Deionized water: 30-60 parts by weight;
② 按原料的重量份准备原料;② Prepare raw materials according to the weight of raw materials;
(2)各组份的制备(2) Preparation of each component
① A组份的制备① Preparation of component A
Ⅰ、将植物油、多元醇、耐热改性剂、催化剂按照重量份的比例加入反应釜,抽真空,通入惰性气体保护;Ⅰ. Add vegetable oil, polyol, heat-resistant modifier, and catalyst to the reactor according to the proportion of parts by weight, vacuumize, and pass inert gas protection;
Ⅱ、升温至200~230℃反应2~3小时,而后冷却至室温,得到植物油基多元醇,出料待用;Ⅱ. Raise the temperature to 200-230°C and react for 2-3 hours, and then cool to room temperature to obtain vegetable oil-based polyol, which is discharged for use;
Ⅲ、将乳化剂、去离子水按照重量份的比例加入上述反应釜中,在室温下快速搅拌,在搅拌中缓慢滴加步骤Ⅱ得到的植物油基多元醇,应控制在0.5~1小时滴加完所述的植物油基多元醇;Ⅲ. Add the emulsifier and deionized water into the above reaction kettle according to the proportion of parts by weight, stir rapidly at room temperature, and slowly add the vegetable oil-based polyol obtained in step Ⅱ dropwise while stirring, and the dropwise addition should be controlled within 0.5 to 1 hour Complete described vegetable oil-based polyol;
Ⅳ、继续搅拌0.5~2小时,获得植物油基多元醇乳液;Ⅳ. Continue to stir for 0.5 to 2 hours to obtain vegetable oil-based polyol emulsion;
② B组分直接采用现有的异氰酸酯产品;② Component B directly adopts existing isocyanate products;
③ C组份的制备③ Preparation of component C
按步骤(1)① C组份的重量份组成依次将颜料、沸石粉、高岭土或石英粉、去离子水投入拉缸中,启动分散机,按400~800转/分钟的转速搅拌15~30分钟进行分散,获得分散均匀的C组份混合料;Put the pigment, zeolite powder, kaolin or quartz powder, and deionized water into the tank in turn according to the weight composition of component C in step (1), start the disperser, and stir at a speed of 400-800 rpm for 15-30 Disperse in minutes to obtain a uniformly dispersed component C mixture;
④ 将所述A组份与C组分分开配料和分散;④ Separately batch and disperse the A component and the C component;
(3)包装(3) Packaging
将步骤(2)制备的A组份和C组分通过罐装、分装设备分开包装。The components A and C prepared in step (2) are packaged separately through canning and dispensing equipment.
本发明的积极效果是:The positive effect of the present invention is:
(1)采用植物油制备聚氨酯地坪涂料,既利用了植物油良好的物理化学性能,又利用了植物油为天然产物,来源广、低成本、可再生的优势。(1) The use of vegetable oil to prepare polyurethane floor coatings not only utilizes the good physical and chemical properties of vegetable oil, but also utilizes the advantages of vegetable oil as a natural product, wide source, low cost, and renewable.
(2)采用了具有芳环或者脂肪环结构的改性剂,通过反应接枝到多元醇组分中,有效提高了植物油基聚氨酯软段的刚性;选用含有芳环或脂肪环刚性结构的异氰酸酯,有效提高了硬段的刚性;通过上述两者的协同作用,能有效改善植物油基聚氨酯地坪涂料的耐热性能和力学性能。(2) A modifier with an aromatic ring or aliphatic ring structure is used, which is grafted into the polyol component through reaction, which effectively improves the rigidity of the soft segment of vegetable oil-based polyurethane; an isocyanate with an aromatic ring or aliphatic ring rigid structure is selected , effectively improving the rigidity of the hard segment; through the synergistic effect of the above two, the heat resistance and mechanical properties of vegetable oil-based polyurethane floor coatings can be effectively improved.
(3)制备方法简便科学,能进行规模化生产。(3) The preparation method is simple and scientific, and large-scale production can be carried out.
具体实施方式detailed description
以下进一步介绍本发明耐热型植物油基聚氨酯地坪涂料及其制备方法的具体实施方式,提供4个实施例和1个比较例。但是需要指出,本发明的实施不限于以下的实施方式。The specific implementation of the heat-resistant vegetable oil-based polyurethane floor coating of the present invention and its preparation method will be further introduced below, and 4 examples and 1 comparative example will be provided. However, it should be noted that implementation of the present invention is not limited to the following embodiments.
实施例1 一种耐热型植物油基聚氨酯地坪涂料的制备方法,包含以下步骤:Embodiment 1 A kind of preparation method of heat-resistant vegetable oil-based polyurethane floor paint, comprises the following steps:
(1)原料准备(1) Raw material preparation
①所述耐热型植物油基聚氨酯地坪涂料包含A、B、C三个组份。① The heat-resistant vegetable oil-based polyurethane floor coating includes three components A, B and C.
所述A组份中各原料的重量份组成为:The parts by weight of each raw material in the described A component consist of:
蓖麻油:100重量份,采用广州成倍化工有限公司生产的精制蓖麻油;Castor oil: 100 parts by weight, adopt the refined castor oil produced by Guangzhou Chengbei Chemical Co., Ltd.;
丙三醇:16重量份,采用上海石化公司生产的甘油(丙三醇);Glycerol: 16 parts by weight, adopt the glycerol (glycerol) produced by Shanghai Petrochemical Company;
松香:25重量份,采用武汉市黑飞马化工原料有限责任公司生产的一级松香;Rosin: 25 parts by weight, adopt the first-grade rosin produced by Wuhan Black Pegasus Chemical Raw Materials Co., Ltd.;
钛酸酯:0.5重量份,采用上海德榜化工有限公司生产的钛酸丁酯;Titanate: 0.5 parts by weight, using butyl titanate produced by Shanghai Debang Chemical Co., Ltd.;
聚氧化乙烯壬基酚醚:4重量份,采用江苏省海安石化公司生产的、型号为TX-10的产品;Polyoxyethylene nonylphenol ether: 4 parts by weight, adopting the product produced by Jiangsu Haian Petrochemical Company, the model is TX-10;
去离子水:120重量份。Deionized water: 120 parts by weight.
所述B组分为二苯基甲烷二异氰酸酯:采用烟台万华公司生产的、型号为MDI-100的产品。The B component is diphenylmethane diisocyanate: a product of the model MDI-100 produced by Yantai Wanhua Company.
所述C组分填料中各原料的重量份组成为:The parts by weight of each raw material in the C component filler consist of:
绿色颜料:3重量份,采用德国巴斯夫公司生产的、型号为K8740的产品;Green pigment: 3 parts by weight, the product that adopts German BASF company to produce, the model is K8740;
沸石粉:8重量份,采用宁波嘉和新材料科技有限公司生产的沸石粉;Zeolite powder: 8 parts by weight, adopts the zeolite powder produced by Ningbo Jiahe New Material Technology Co., Ltd.;
高岭土:25重量份,采用淮安市汇江钛白粉有限公司生产的1250目产品;Kaolin: 25 parts by weight, using the 1250 mesh product produced by Huaian Huijiang Titanium Dioxide Co., Ltd.;
去离子水:40重量份。Deionized water: 40 parts by weight.
② 按原料的重量份准备原料。② Prepare the raw materials according to the weight of the raw materials.
(2)各组份的制备(2) Preparation of each component
① A组份的制备① Preparation of component A
Ⅰ、将蓖麻油、丙三醇、松香、钛酸丁酯按照重量份的比例加入反应釜,抽真空,通入惰性气体保护。Ⅰ. Add castor oil, glycerol, rosin, and butyl titanate to the reaction kettle in proportions by weight, vacuumize, and pass in an inert gas for protection.
Ⅱ、升温至220℃反应3小时,而后冷却至室温,得到植物油基多元醇,出料待用。II. Raise the temperature to 220° C. for 3 hours and then cool to room temperature to obtain vegetable oil-based polyol, which is discharged for use.
Ⅲ、将4重量份聚氧化乙烯壬基酚醚、100重量份去离子水加入上述反应釜中,在室温下快速搅拌,在搅拌中缓慢滴加步骤Ⅱ得到的植物油基多元醇,控制在0.5小时滴加完所述的植物油基多元醇。Ⅲ. Add 4 parts by weight of polyoxyethylene nonylphenol ether and 100 parts by weight of deionized water into the above reaction kettle, stir rapidly at room temperature, and slowly add the vegetable oil-based polyol obtained in step Ⅱ during the stirring, and control it at 0.5 Add the vegetable oil-based polyol dropwise in hours.
Ⅳ、继续搅拌2小时,获得植物油基多元醇乳液。Ⅳ. Stirring was continued for 2 hours to obtain vegetable oil-based polyol emulsion.
② B组分直接采用烟台万华公司生产的型号为MDI-100的产品。② Component B directly adopts the product of model MDI-100 produced by Yantai Wanhua Company.
③ C组份的制备③ Preparation of component C
将3重量份颜料、8重量份沸石粉、25重量份高岭土、40重量份去离子水投入拉缸中,启动分散机,按500转/分钟的转速搅拌20分钟进行分散,获得分散均匀的C组份混合料。Put 3 parts by weight of pigments, 8 parts by weight of zeolite powder, 25 parts by weight of kaolin, and 40 parts by weight of deionized water into the tank, start the disperser, stir for 20 minutes at a speed of 500 rpm to disperse, and obtain evenly dispersed C Component mix.
④ 将所述A组份与C组分分开配料和分散。④ Separately mix and disperse the components A and C.
(3)包装(3) Packaging
将步骤(2)制备的A组份和C组分通过罐装、分装设备分开包装。The components A and C prepared in step (2) are packaged separately through canning and dispensing equipment.
涂覆前,将所述A组份、B组份与C组份按重量比A:B:C=2:2:0.7配合使用:在搅拌状态下,先将C组分加入A组份;再将B组分缓慢加入A组份与C组份的混合组分中,搅拌5分钟,用馒刀刮涂,后用消泡滚筒消泡处理,在室温下固化14天成膜。Before coating, use the A component, B component and C component in a weight ratio of A:B:C=2:2:0.7: under stirring, first add C component to A component; Then slowly add component B into the mixed component of component A and component C, stir for 5 minutes, scrape it with a steamed knife, and then use a defoaming roller for defoaming treatment, and cure it at room temperature for 14 days to form a film.
实施例1制备的耐热型植物油基聚氨酯地坪涂料成膜后的耐热性能和力学性能的测试结果见表1。Table 1 shows the test results of heat resistance and mechanical properties of the heat-resistant vegetable oil-based polyurethane floor coating prepared in Example 1 after film formation.
实施例2 一种耐热型植物油基聚氨酯地坪涂料的制备方法,包含以下步骤:Embodiment 2 A preparation method of heat-resistant vegetable oil-based polyurethane floor coating, comprising the following steps:
(1)原料准备(1) Raw material preparation
①所述耐热型植物油基聚氨酯地坪涂料包含A、B、C三个组份。① The heat-resistant vegetable oil-based polyurethane floor coating includes three components A, B and C.
所述A组份中各原料的重量份组成为:The parts by weight of each raw material in the described A component consist of:
大豆油:100重量份,采用吉安市红苹果天然香料油有限公司生产的大豆油;Soybean oil: 100 parts by weight, adopt the soybean oil produced by Ji'an Red Apple Natural Perfume Oil Co., Ltd.;
乙二醇:5重量份,采用上海石化公司生产的乙二醇;Ethylene glycol: 5 parts by weight, adopt the ethylene glycol produced by Shanghai Petrochemical Company;
苯酐:10重量份,采用金陵石化公司生产的苯酐;Phthalic anhydride: 10 parts by weight, adopt the phthalic anhydride produced by Jinling Petrochemical Company;
氢氧化锂0.3重量份,采用上海中锂公司生产的氢氧化锂;Lithium hydroxide 0.3 weight part, adopts the lithium hydroxide that Shanghai Zhongli Company produces;
聚乙二醇双油酸酯:3重量份,采用江苏省海安石化公司生产的、型号为PEG-400的产品;Polyethylene glycol dioleate: 3 parts by weight, adopting the product produced by Jiangsu Hai'an Petrochemical Company, the model is PEG-400;
去离子水:60重量份。Deionized water: 60 parts by weight.
所述B组分为甲苯二异氰酸酯三聚体,采用德国拜耳公司生产的、型号为Desmodur-L75的产品。The B component is a trimer of toluene diisocyanate, which is produced by German Bayer Company and whose model is Desmodur-L75.
所述C组分填料中各原料的重量份组成为:The parts by weight of each raw material in the C component filler consist of:
绿色颜料:5重量份,采用德国巴斯夫公司生产的、型号为K8740的产品;Green pigment: 5 parts by weight, the product that adopts Germany BASF company to produce, the model is K8740;
沸石粉:10重量份,采用宁波嘉和新材料科技有限公司生产的沸石粉;Zeolite powder: 10 parts by weight, adopts the zeolite powder produced by Ningbo Jiahe New Material Technology Co., Ltd.;
石英粉:30重量份,采用广州艺峰矿业有限公司生产的1250目的产品;Quartz powder: 30 parts by weight, adopting the 1250 mesh product produced by Guangzhou Yifeng Mining Co., Ltd.;
去离子水:30重量份。Deionized water: 30 parts by weight.
② 按原料的重量份准备原料。② Prepare the raw materials according to the weight of the raw materials.
(2)各组份的制备(2) Preparation of each component
① A组份的制备① Preparation of component A
Ⅰ、将大豆油、乙二醇、苯酐、氢氧化锂按照重量份的比例加入反应釜,抽真空,通入惰性气体保护。Ⅰ. Add soybean oil, ethylene glycol, phthalic anhydride, and lithium hydroxide into the reactor according to the proportion of parts by weight, vacuumize, and pass in an inert gas for protection.
Ⅱ、升温至200℃反应2小时,而后冷却至室温,得到植物油基多元醇,出料待用。II. Raise the temperature to 200° C. to react for 2 hours, and then cool to room temperature to obtain vegetable oil-based polyol, which is discharged for use.
Ⅲ、将3重量份聚乙二醇双油酸酯、60重量份去离子水加入上述反应釜中,在室温下快速搅拌,在搅拌中缓慢滴加步骤Ⅱ得到的植物油基多元醇,控制在1小时滴加完所述的植物油基多元醇。Ⅲ. Add 3 parts by weight of polyethylene glycol dioleate and 60 parts by weight of deionized water into the above reaction kettle, stir rapidly at room temperature, and slowly add the vegetable oil-based polyol obtained in step Ⅱ during the stirring, and control it at The vegetable oil-based polyol was added dropwise in 1 hour.
Ⅳ、继续搅拌0.5小时,获得植物油基多元醇乳液。IV. Continue stirring for 0.5 hour to obtain vegetable oil-based polyol emulsion.
② B组分直接采用德国拜耳公司生产的型号为Desmodur-L75的产品。② Component B directly adopts the product of model Desmodur-L75 produced by German Bayer company.
③ C组份的制备③ Preparation of component C
将5重量份颜料、10重量份沸石粉、30重量份石英粉、40重量份去离子水投入拉缸中,启动分散机,按400转/分钟的转速搅拌15分钟进行分散,获得分散均匀的C组份混合料;Put 5 parts by weight of pigments, 10 parts by weight of zeolite powder, 30 parts by weight of quartz powder, and 40 parts by weight of deionized water into the tank, start the disperser, stir for 15 minutes at a speed of 400 rpm to disperse, and obtain a uniformly dispersed C component mixture;
④ 将所述A组份与C组分分开配料和分散。④ Separately mix and disperse the components A and C.
(3)包装(3) Packaging
将步骤(2)制备的A组份和C组分通过罐装、分装设备分开包装。The components A and C prepared in step (2) are packaged separately through canning and dispensing equipment.
涂覆前,将所述A组份、B组份与C组份按重量比A:B:C=2:1:0.5配合使用:在搅拌状态下,先将C组分加入A组份;再将B组分缓慢加入A组份与C组份的混合组分中,搅拌5分钟,用馒刀刮涂,后用消泡滚筒消泡处理,在室温下固化14天成膜。Before coating, use the A component, B component and C component in a weight ratio of A:B:C=2:1:0.5: first add C component to A component in the stirring state; Then slowly add component B into the mixed component of component A and component C, stir for 5 minutes, scrape it with a steamed knife, and then use a defoaming roller for defoaming treatment, and cure at room temperature for 14 days to form a film.
实施例2制备的耐热型植物油基聚氨酯地坪涂料成膜后的耐热性能和力学性能的测试结果见表1。Table 1 shows the test results of heat resistance and mechanical properties of the heat-resistant vegetable oil-based polyurethane floor coating prepared in Example 2 after film formation.
实施例3 一种耐热型植物油基聚氨酯地坪涂料的制备方法,包含以下步骤:Embodiment 3 A preparation method of heat-resistant vegetable oil-based polyurethane floor coating, comprising the following steps:
(1)原料准备(1) Raw material preparation
①所述耐热型植物油基聚氨酯地坪涂料包含A、B、C三个组份。① The heat-resistant vegetable oil-based polyurethane floor coating includes three components A, B and C.
所述A组份中各原料的重量份组成为:The parts by weight of each raw material in the described A component consist of:
亚麻油:100重量份,采用吉安市红苹果天然香料油有限公司生产的亚麻籽油;Linseed oil: 100 parts by weight, adopt the linseed oil produced by Ji'an Red Apple Natural Perfume Oil Co., Ltd.;
一缩二乙二醇:20重量份,采用上海石化公司生产的一缩二乙二醇;Diethylene glycol: 20 parts by weight, adopting the diethylene glycol produced by Shanghai Petrochemical Company;
甲阶酚醛树脂:20重量份,采用济宁百川化工有限公司生产的、型号为PF-6815的产品;Resole phenolic resin: 20 parts by weight, the product that adopts Jining Baichuan Chemical Co., Ltd. to produce, model is PF-6815;
钛酸酯:1重量份,采用上海德榜化工有限公司生产的钛酸丁酯;Titanate: 1 part by weight, using butyl titanate produced by Shanghai Debang Chemical Co., Ltd.;
蓖麻油聚氧乙烯醚:5重量份,采用江苏省海安石化公司生产的、型号为EL-90的产品;Castor oil polyoxyethylene ether: 5 parts by weight, adopting the product produced by Jiangsu Hai'an Petrochemical Company, the model is EL-90;
去离子水:160重量份。Deionized water: 160 parts by weight.
所述B组分为异氟尔酮二异氰酸酯,采用德国拜耳公司生产的、型号为IPDI产品。The B component is isophorone diisocyanate, which is produced by Bayer Company of Germany and whose model is IPDI.
所述C组分填料中各原料的重量份组成为:The parts by weight of each raw material in the C component filler consist of:
绿色颜料:1重量份,采用德国巴斯夫公司生产的、型号为K8740的产品;Green pigment: 1 part by weight, the product that adopts German BASF company to produce, the model is K8740;
沸石粉:5重量份,采用宁波嘉和新材料科技有限公司生产的沸石粉;Zeolite powder: 5 parts by weight, adopts the zeolite powder produced by Ningbo Jiahe New Material Technology Co., Ltd.;
石英粉:20重量份,采用广州艺峰矿业有限公司生产的1250目产品;Quartz powder: 20 parts by weight, adopting the 1250 mesh product produced by Guangzhou Yifeng Mining Co., Ltd.;
去离子水:30重量份。Deionized water: 30 parts by weight.
② 按原料的重量份准备原料。② Prepare the raw materials according to the weight of the raw materials.
(2)各组份的制备(2) Preparation of each component
① A组份的制备① Preparation of component A
Ⅰ、将亚麻油、一缩二乙二醇、甲阶酚醛树脂、钛酸丁酯按照重量份的比例加入反应釜,抽真空,通入惰性气体保护。Ⅰ. Add linseed oil, diethylene glycol, resole phenolic resin, and butyl titanate to the reaction kettle in proportions by weight, vacuumize, and pass in an inert gas for protection.
Ⅱ、升温至220℃反应2小时,而后冷却至室温,得到植物油基多元醇,出料待用。II. Raise the temperature to 220° C. to react for 2 hours, and then cool to room temperature to obtain vegetable oil-based polyol, which is discharged for use.
Ⅲ、将5重量份蓖麻油聚氧化乙烯醚、120重量份去离子水加入上述反应釜中,在室温下快速搅拌,在搅拌中缓慢滴加步骤Ⅱ得到的植物油基多元醇,控制在0.5小时滴加完所述的植物油基多元醇。Ⅲ. Add 5 parts by weight of castor oil polyoxyethylene ether and 120 parts by weight of deionized water into the above-mentioned reaction kettle, stir rapidly at room temperature, and slowly add the vegetable oil-based polyol obtained in step Ⅱ during the stirring, and control it within 0.5 hours Add the vegetable oil-based polyol dropwise.
Ⅳ、继续搅拌2小时,获得植物油基多元醇乳液。Ⅳ. Stirring was continued for 2 hours to obtain vegetable oil-based polyol emulsion.
② B组分直接采用德国拜耳公司生产的型号为IPDI产品。② Component B directly adopts the model produced by German Bayer Company as IPDI product.
③ C组份的制备③ Preparation of component C
将1重量份颜料、5重量份沸石粉、20重量份石英粉、30质量份去离子水投入拉缸中,启动分散机,按800转/分钟的转速搅拌30分钟进行分散,获得分散均匀的C组份混合料;Put 1 part by weight of pigment, 5 parts by weight of zeolite powder, 20 parts by weight of quartz powder, and 30 parts by mass of deionized water into the tank, start the disperser, stir at a speed of 800 rpm for 30 minutes to disperse, and obtain a uniformly dispersed C component mixture;
④ 将所述A组份与C组分分开配料和分散。④ Separately mix and disperse the components A and C.
(3)包装(3) Packaging
将步骤(2)制备的A组份和C组分通过罐装、分装设备分开包装。The components A and C prepared in step (2) are packaged separately through canning and dispensing equipment.
涂覆前,将所述A组份、B组份与C组份按重量比A:B:C=2:3:1配合使用:在搅拌状态下,先将C组分加入A组份;再将B组分缓慢加入A组份与C组份的混合组分中,搅拌5分钟,用馒刀刮涂,后用消泡滚筒消泡处理,在室温下固化14天成膜。Before coating, use the components A, B and C in a weight ratio of A:B:C=2:3:1: first add component C to component A under stirring; Then slowly add component B into the mixed component of component A and component C, stir for 5 minutes, scrape it with a steamed knife, and then use a defoaming roller for defoaming treatment, and cure at room temperature for 14 days to form a film.
实施例3制备的耐热型植物油基聚氨酯地坪涂料成膜后的耐热性能和力学性能的测试结果见表1。Table 1 shows the test results of heat resistance and mechanical properties of the heat-resistant vegetable oil-based polyurethane floor coating prepared in Example 3 after film formation.
实施例4 一种耐热型植物油基聚氨酯地坪涂料的制备方法,包含以下步骤:Embodiment 4 A preparation method of heat-resistant vegetable oil-based polyurethane floor coating, comprising the following steps:
(1)原料准备(1) Raw material preparation
①所述耐热型植物油基聚氨酯地坪涂料包含A、B、C三个组份。① The heat-resistant vegetable oil-based polyurethane floor coating includes three components A, B and C.
所述A组份中各原料的重量份组成为:The parts by weight of each raw material in the described A component consist of:
棕榈油:100重量份;采用吉安市红苹果天然香料油有限公司生产的棕榈油;Palm oil: 100 parts by weight; adopt the palm oil produced by Ji'an Red Apple Natural Perfume Oil Co., Ltd.;
三羟甲基丙烷:8重量份,采用上海石化公司生产的三羟甲基丙烷;Trimethylolpropane: 8 parts by weight, adopt the trimethylolpropane produced by Shanghai Petrochemical Company;
松香:30重量份,采用武汉市黑飞马化工原料有限责任公司生产的一级松香;Rosin: 30 parts by weight, adopt the first-grade rosin produced by Wuhan Black Pegasus Chemical Raw Materials Co., Ltd.;
氢氧化锂:0.7重量份,采用上海中锂公司生产的氢氧化锂;Lithium hydroxide: 0.7 parts by weight, adopts the lithium hydroxide produced by Shanghai Zhongli Company;
聚氧化乙烯壬基酚醚:5重量份,采用江苏省海安石化公司生产的、型号为TX-10的产品;Polyoxyethylene nonylphenol ether: 5 parts by weight, adopting the product produced by Jiangsu Haian Petrochemical Company, the model is TX-10;
去离子水:80重量份。Deionized water: 80 parts by weight.
所述B组分为聚甲撑聚苯基异氰酸酯,采用美国陶氏公司生产的、型号为PAPI135C的产品。The B component is polymethylene polyphenylisocyanate, which is produced by American Dow Company and whose model is PAPI135C.
所述C组分填料中各原料的重量份组成为:The parts by weight of each raw material in the C component filler consist of:
绿色颜料:4重量份,采用德国巴斯夫公司生产的、型号为K8740的产品;Green pigment: 4 parts by weight, the product that adopts Germany BASF company to produce, the model is K8740;
沸石粉:6重量份,采用宁波嘉和新材料科技有限公司生产的沸石粉;Zeolite powder: 6 parts by weight, adopts the zeolite powder produced by Ningbo Jiahe New Material Technology Co., Ltd.;
高岭土:27重量份,采用淮安市汇江钛白粉有限公司生产的1250目产品;Kaolin: 27 parts by weight, using the 1250 mesh product produced by Huaian Huijiang Titanium Dioxide Co., Ltd.;
去离子水:60重量份。Deionized water: 60 parts by weight.
② 按原料的重量份准备原料。② Prepare the raw materials according to the weight of the raw materials.
(2)各组份的制备(2) Preparation of each component
① A组份的制备① Preparation of component A
Ⅰ、将棕榈油、三羟甲基丙烷、松香、氢氧化锂按照重量份的比例加入反应釜,抽真空,通入惰性气体保护。1. Add palm oil, trimethylolpropane, rosin, and lithium hydroxide to the reaction kettle in proportions by weight, vacuumize, and pass in an inert gas for protection.
Ⅱ、升温至230℃反应2小时,而后冷却至室温,得到植物油基多元醇,出料待用。II. Raise the temperature to 230° C. to react for 2 hours, and then cool to room temperature to obtain vegetable oil-based polyol, which is discharged for use.
Ⅲ、将5重量份聚氧化乙烯壬基酚醚、80重量份去离子水加入上述反应釜中,在室温下快速搅拌,在搅拌中缓慢滴加步骤Ⅱ得到的植物油基多元醇,控制在1小时滴加完所述的植物油基多元醇。Ⅲ. Add 5 parts by weight of polyoxyethylene nonylphenol ether and 80 parts by weight of deionized water into the above reaction kettle, stir rapidly at room temperature, and slowly add the vegetable oil-based polyol obtained in step Ⅱ during the stirring, and control it at 1 Add the vegetable oil-based polyol dropwise in hours.
Ⅳ、继续搅拌2小时,获得植物油基多元醇乳液。Ⅳ. Stirring was continued for 2 hours to obtain vegetable oil-based polyol emulsion.
② B组分直接采用美国陶氏公司生产的型号为PAPI135C的产品。② Component B directly adopts the product of model PAPI135C produced by American Dow Company.
③ C组份的制备③ Preparation of component C
将4重量份颜料、6重量份沸石粉、27重量份高岭土、60质量份去离子水投入拉缸中,启动分散机,按700转/分钟的转速搅拌30分钟进行分散,获得分散均匀的C组份混合料;Put 4 parts by weight of pigments, 6 parts by weight of zeolite powder, 27 parts by weight of kaolin, and 60 parts by weight of deionized water into the tank, start the disperser, stir for 30 minutes at a speed of 700 rpm to disperse, and obtain evenly dispersed C component mixture;
④ 将所述A组份与C组分分开配料和分散。④ Separately mix and disperse the components A and C.
(3)包装(3) Packaging
将步骤(2)制备的A组份和C组分通过罐装、分装设备分开包装。The components A and C prepared in step (2) are packaged separately through canning and dispensing equipment.
涂覆前,将所述A组份、B组份与C组份按重量比A:B:C=2:2.5:1配合使用:在搅拌状态下,先将C组分加入A组份;再将B组分缓慢加入A组份与C组份的混合组分中,搅拌5分钟,用馒刀刮涂,后用消泡滚筒消泡处理,在室温下固化14天成膜。Before coating, use the components A, B and C in a weight ratio of A:B:C=2:2.5:1: add component C to component A under stirring; Then slowly add component B into the mixed component of component A and component C, stir for 5 minutes, scrape it with a steamed knife, and then use a defoaming roller for defoaming treatment, and cure at room temperature for 14 days to form a film.
实施例4制备的耐热型植物油基聚氨酯地坪涂料成膜后的耐热性能和力学性能的测试结果见表1。Table 1 shows the test results of heat resistance and mechanical properties of the heat-resistant vegetable oil-based polyurethane floor coating prepared in Example 4 after film formation.
比较例1——为了证明实施例1~4制备的耐热型植物油基聚氨酯地坪涂料成膜后的耐热性能和力学性能,我们设计了此比较例。Comparative Example 1—In order to prove the heat resistance and mechanical properties of the heat-resistant vegetable oil-based polyurethane floor coatings prepared in Examples 1-4 after film formation, we designed this comparative example.
一种植物油基聚氨酯地坪涂料的制备方法,包含以下步骤:A preparation method of vegetable oil-based polyurethane floor paint, comprising the following steps:
(1)原料准备(1) Raw material preparation
①所述耐热型植物油基聚氨酯地坪涂料包含A、B、C三个组份。① The heat-resistant vegetable oil-based polyurethane floor coating includes three components A, B and C.
所述A组份中各原料的重量份组成为:The parts by weight of each raw material in the described A component consist of:
蓖麻油:100重量份,采用吉安市红苹果天然香料油有限公司生产的精制蓖麻油;Castor oil: 100 parts by weight, adopt the refining castor oil produced by Ji'an Red Apple Natural Perfume Oil Co., Ltd;
丙三醇:16重量份,采用上海石化公司生产的甘油(丙三醇);Glycerol: 16 parts by weight, adopt the glycerol (glycerol) produced by Shanghai Petrochemical Company;
钛酸酯:0.5重量份,采用上海德榜化工有限公司生产的钛酸丁酯;Titanate: 0.5 parts by weight, using butyl titanate produced by Shanghai Debang Chemical Co., Ltd.;
聚氧化乙烯壬基酚醚:4重量份,采用江苏省海安石化公司生产的、型号为TX-10的产品;Polyoxyethylene nonylphenol ether: 4 parts by weight, adopting the product produced by Jiangsu Haian Petrochemical Company, the model is TX-10;
去离子水:120重量份。Deionized water: 120 parts by weight.
所述B组分为二苯基甲烷二异氰酸酯:采用烟台万华公司生产的、型号为MDI-100的产品。The B component is diphenylmethane diisocyanate: a product of the model MDI-100 produced by Yantai Wanhua Company.
所述C组分填料中各原料的重量份组成为:The parts by weight of each raw material in the C component filler consist of:
绿色颜料:3重量份,采用德国巴斯夫公司生产的型号为K8740的产品;Green pigment: 3 parts by weight, the model that adopts Germany BASF company to produce is the product of K8740;
沸石粉:8重量份,采用宁波嘉和新材料科技有限公司生产的沸石粉;Zeolite powder: 8 parts by weight, adopts the zeolite powder produced by Ningbo Jiahe New Material Technology Co., Ltd.;
高岭土:25重量份,采用淮安市汇江钛白粉有限公司生产的1250目产品;Kaolin: 25 parts by weight, using the 1250 mesh product produced by Huaian Huijiang Titanium Dioxide Co., Ltd.;
去离子水:40重量份。Deionized water: 40 parts by weight.
② 按原料的重量份准备原料。② Prepare the raw materials according to the weight of the raw materials.
(2)各组份的制备(2) Preparation of each component
① A组份的制备① Preparation of component A
Ⅰ、将蓖麻油、丙三醇、钛酸丁酯按照重量份的比例加入反应釜,抽真空,通入惰性气体保护。Ⅰ. Add castor oil, glycerin, and butyl titanate to the reaction kettle in proportions by weight, vacuumize, and pass in an inert gas for protection.
Ⅱ、升温至220℃反应3小时,而后冷却至室温,得到植物油基多元醇,出料待用。II. Raise the temperature to 220° C. for 3 hours and then cool to room temperature to obtain vegetable oil-based polyol, which is discharged for use.
Ⅲ、将4重量份聚氧化乙烯壬基酚醚、100重量份去离子水加入上述反应釜中,在室温下快速搅拌,在搅拌中缓慢滴加步骤Ⅱ得到的植物油基多元醇,控制在0.5小时滴加完所述的植物油基多元醇。Ⅲ. Add 4 parts by weight of polyoxyethylene nonylphenol ether and 100 parts by weight of deionized water into the above-mentioned reaction kettle, stir rapidly at room temperature, and slowly add the vegetable oil-based polyol obtained in step Ⅱ during the stirring, and control it at 0.5 Add the vegetable oil-based polyol dropwise in hours.
Ⅳ、继续搅拌2小时,获得植物油基多元醇乳液。Ⅳ. Stirring was continued for 2 hours to obtain vegetable oil-based polyol emulsion.
② B组分直接采用烟台万华公司生产的型号为MDI-100的产品。② Component B directly adopts the product of model MDI-100 produced by Yantai Wanhua Company.
③ C组份的制备③ Preparation of component C
将3重量份颜料、8重量份沸石粉、25重量份高岭土、40重量份去离子水投入拉缸中,启动分散机,按500转/分钟的转速搅拌20分钟进行分散,获得分散均匀的C组份混合料;Put 3 parts by weight of pigments, 8 parts by weight of zeolite powder, 25 parts by weight of kaolin, and 40 parts by weight of deionized water into the tank, start the disperser, stir at a speed of 500 rpm for 20 minutes to disperse, and obtain evenly dispersed C component mixture;
④ 将所述A组份与C组分分开配料和分散。④ Separately mix and disperse the components A and C.
(3)包装(3) Packaging
将步骤(2)制备的A组份和C组分通过罐装、分装设备分开包装。The components A and C prepared in step (2) are packaged separately through canning and dispensing equipment.
涂覆前,将所述A组份、B组份与C组份按重量比A:B:C=2:2:0.7配合使用:在搅拌状态下,先将C组分加入A组份;再将B组分缓慢加入A组份与C组份的混合组分中,搅拌5分钟,用馒刀刮涂,后用消泡滚筒消泡处理,在室温下固化14天成膜。Before coating, use the A component, B component and C component in a weight ratio of A:B:C=2:2:0.7: under stirring, first add C component to A component; Then slowly add component B into the mixed component of component A and component C, stir for 5 minutes, scrape it with a steamed knife, and then use a defoaming roller for defoaming treatment, and cure it at room temperature for 14 days to form a film.
比较例1制备的耐热型植物油基聚氨酯地坪涂料成膜后的耐热性能和力学性能的测试结果见表1。Table 1 shows the test results of heat resistance and mechanical properties of the heat-resistant vegetable oil-based polyurethane floor coating prepared in Comparative Example 1 after film formation.
表1. 实施例1~4制备的耐热型植物油基聚氨酯地坪涂料以及比较例1制备的植物油基聚氨酯地坪涂料成膜后的耐热性能和力学性能测试结果Table 1. Heat-resistant vegetable oil-based polyurethane floor coatings prepared in Examples 1 to 4 and the heat resistance and mechanical performance test results of the vegetable oil-based polyurethane floor coatings prepared in Comparative Example 1 after film formation
。 .
从表1的测试结果能明显看出:实施例1~4制备的耐热型植物油基聚氨酯地坪涂料成膜后在“热变形温度”、“抗压强度”和“抗折强度”上均明显好于比较例1。From the test results in Table 1, it can be clearly seen that the heat-resistant vegetable oil-based polyurethane floor coatings prepared in Examples 1 to 4 have the same performance in "heat distortion temperature", "compressive strength" and "flexural strength" after film formation. significantly better than Comparative Example 1.
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