CN106893479A - 一种粉末涂料的制备方法 - Google Patents

一种粉末涂料的制备方法 Download PDF

Info

Publication number
CN106893479A
CN106893479A CN201510954326.2A CN201510954326A CN106893479A CN 106893479 A CN106893479 A CN 106893479A CN 201510954326 A CN201510954326 A CN 201510954326A CN 106893479 A CN106893479 A CN 106893479A
Authority
CN
China
Prior art keywords
added
parts
mixing
reactor
coating
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201510954326.2A
Other languages
English (en)
Inventor
宋容
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Individual
Original Assignee
Individual
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Individual filed Critical Individual
Priority to CN201510954326.2A priority Critical patent/CN106893479A/zh
Publication of CN106893479A publication Critical patent/CN106893479A/zh
Pending legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D175/00Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
    • C09D175/04Polyurethanes
    • C09D175/08Polyurethanes from polyethers
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00Polymeric products of isocyanates or isothiocyanates
    • C08G18/06Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/08Processes
    • C08G18/0804Manufacture of polymers containing ionic or ionogenic groups
    • C08G18/0819Manufacture of polymers containing ionic or ionogenic groups containing anionic or anionogenic groups
    • C08G18/0823Manufacture of polymers containing ionic or ionogenic groups containing anionic or anionogenic groups containing carboxylate salt groups or groups forming them
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00Polymeric products of isocyanates or isothiocyanates
    • C08G18/06Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/08Processes
    • C08G18/10Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step
    • C08G18/12Prepolymer processes involving reaction of isocyanates or isothiocyanates with compounds having active hydrogen in a first reaction step using two or more compounds having active hydrogen in the first polymerisation step
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00Polymeric products of isocyanates or isothiocyanates
    • C08G18/06Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/40High-molecular-weight compounds
    • C08G18/48Polyethers
    • C08G18/4804Two or more polyethers of different physical or chemical nature
    • C08G18/4808Mixtures of two or more polyetherdiols
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00Polymeric products of isocyanates or isothiocyanates
    • C08G18/06Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/65Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
    • C08G18/66Compounds of groups C08G18/42, C08G18/48, or C08G18/52
    • C08G18/6666Compounds of group C08G18/48 or C08G18/52
    • C08G18/667Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38
    • C08G18/6681Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/32 or C08G18/3271 and/or polyamines of C08G18/38
    • C08G18/6685Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/32 or polyamines of C08G18/38 with compounds of group C08G18/32 or C08G18/3271 and/or polyamines of C08G18/38 with compounds of group C08G18/3225 or polyamines of C08G18/38
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00Polymeric products of isocyanates or isothiocyanates
    • C08G18/06Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/28Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the compounds used containing active hydrogen
    • C08G18/65Low-molecular-weight compounds having active hydrogen with high-molecular-weight compounds having active hydrogen
    • C08G18/66Compounds of groups C08G18/42, C08G18/48, or C08G18/52
    • C08G18/6666Compounds of group C08G18/48 or C08G18/52
    • C08G18/6692Compounds of group C08G18/48 or C08G18/52 with compounds of group C08G18/34
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08GMACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
    • C08G18/00Polymeric products of isocyanates or isothiocyanates
    • C08G18/06Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
    • C08G18/70Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
    • C08G18/72Polyisocyanates or polyisothiocyanates
    • C08G18/74Polyisocyanates or polyisothiocyanates cyclic
    • C08G18/75Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic
    • C08G18/751Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring
    • C08G18/752Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group
    • C08G18/753Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group
    • C08G18/755Polyisocyanates or polyisothiocyanates cyclic cycloaliphatic containing only one cycloaliphatic ring containing at least one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group containing one isocyanate or isothiocyanate group linked to the cycloaliphatic ring by means of an aliphatic group having a primary carbon atom next to the isocyanate or isothiocyanate group and at least one isocyanate or isothiocyanate group linked to a secondary carbon atom of the cycloaliphatic ring, e.g. isophorone diisocyanate
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/03Powdery paints
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/03Powdery paints
    • C09D5/033Powdery paints characterised by the additives
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D5/00Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
    • C09D5/08Anti-corrosive paints
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40Additives
    • C09D7/47Levelling agents
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40Additives
    • C09D7/60Additives non-macromolecular
    • C09D7/61Additives non-macromolecular inorganic
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40Additives
    • C09D7/60Additives non-macromolecular
    • C09D7/61Additives non-macromolecular inorganic
    • C09D7/62Additives non-macromolecular inorganic modified by treatment with other compounds
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40Additives
    • C09D7/60Additives non-macromolecular
    • C09D7/63Additives non-macromolecular organic
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/40Additives
    • C09D7/65Additives macromolecular
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D7/00Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
    • C09D7/80Processes for incorporating ingredients
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/011Nanostructured additives
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/03Polymer mixtures characterised by other features containing three or more polymers in a blend
    • C08L2205/035Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Engineering & Computer Science (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacturing & Machinery (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Paints Or Removers (AREA)

Abstract

本发明公开了粉末涂料的制备方法,包括如下工序:1)在室温下向第一反应釜中加入异佛尔酮二异氰酸酯等,得到初级制品;2)向初级制品内加入二羟甲基丙酸,再加入三乙胺,制得脂肪族粉末乳液;3)制得改性硅溶胶;4)在室温下向第三反应釜中加入脂肪族粉末乳液和改性硅溶胶,得到混合乳液;5)向盛有蒸馏水的第四反应釜中加入适量的丙烯酸共聚物钾盐等,得到混合底液;6)向混合底液内加入混合乳液,得到粉末涂料。采用本发明制得的涂料能对被保护物进行有效的封闭防护,防止被保护物受到污染、腐蚀和损伤。同时,该涂料还具有可剥性好、涂膜强度高、内聚力强及稳定性高的优点。

Description

一种粉末涂料的制备方法
技术领域
本发明涉及包装装潢领域,尤其是涉及粉末涂料的制备方法。
背景技术
为防止暴露在大气环境下的材料或半产品受到污染、腐蚀和损伤,并延长使用寿命,通常会在它们的表面涂抹具有良好防护性和可剥性的涂料以对其进行有效的且临时的封存保护。如此,既可隔离外界的空气、盐雾、微生物的入侵,达到防腐效果;又可通过吸附污染物以达到清洁去污的效果。较溶剂型防护涂料而言,防护涂料更具安全性及环保性,因而被广泛应用于产品的包装装潢领域中。但是,现有防护涂料仍然具有涂膜强度低、可剥性较差及防护性能单一的缺点。
发明内容
本发明的目的是克服上述现有技术的缺陷,提供粉末涂料的制备方法,采用本发明制得的涂料能对被保护物进行有效的封闭防护,具有可剥性好、涂膜强度高、内聚力强及稳定性高的优点。
本发明的目的主要通过以下技术方案实现:
粉末涂料的制备方法,包括如下工序:
1)在室温下向第一反应釜中加入异佛尔酮二异氰酸酯、聚丙二醇、聚乙二醇、二月桂酸二丁基锡及丁酮,再将温度升至58~80℃,使它们在第一反应釜内混合反应至体系中-NCO%值不再变化,得到初级制品,备用;
2)将温度控制在80℃,向工序1)所得的初级制品内加入二羟甲基丙酸并反应220~260min,再将温度降至38~43℃,加入三乙胺,得到次级制品;向盛有蒸馏水的第二反应釜中加入次级制品并使次级制品分散于蒸馏水中,再加入二乙烯三胺水溶液,制得脂肪族粉末乳液;
3)向盛有乙醇的烧瓶内加入丙基三甲氧基硅烷,按100~200r/min的转速搅拌混合5~10min,得到硅烷溶液;控制转速为200~300r/min,向盛有碱性硅溶胶的第三反应釜中滴加硅烷溶液;滴加完毕后,在50~65℃的温度下,按250r/min的转速搅拌混合450~500min,得到改性硅溶胶,备用;
4)在室温下向第四反应釜中加入工序2)所得的脂肪族粉末乳液和工序3)所得的改性硅溶胶,按200~300r/min的转速搅拌混合50~70min,得到混合乳液,备用;
5)向盛有蒸馏水的第五反应釜中加入适量的丙烯酸共聚物钾盐、碱溶胀丙烯酸增稠剂和聚醚改性有机硅,按200~300r/min的转速搅拌混合4~10min,再加入适量的二氧化钛、云母,按1500~1800r/min的转速搅拌混合35~42min,得到混合底液;
6)向工序5)所得的混合底液内加入工序4)所得的混合乳液,按350~500r/min的转速搅拌混合12~22min;再加入适量的十二烷基苯磺酸钠、聚醚改性二甲基硅氧烷、碱溶胀丙烯酸增稠剂、硅油、聚醚改性有机硅,按200~300r/min的转速搅拌混合15~20min,得到粉末涂料;
所述改性硅溶胶由以下质量配比的原料制得:碱性硅溶胶40~60份,乙醇30~50份,丙基三甲氧基硅烷1~6份;所述脂肪族粉末乳液由以下质量配比的原料制得:异佛尔酮二异氰酸酯40~80份,聚丙二醇25~40份,聚乙二醇25~80份,二羟甲基丙酸3~10份,丁酮50~80份,二乙烯三胺5~12份,三乙胺3~9份,二月桂酸二丁基锡1~3份,蒸馏水40~80份;所述粉末涂料由以下质量分数的原料制得:脂肪族粉末乳液60~80%,改性硅溶胶5~10%,二氧化钛2~5%,云母3~5%,硅油1~3%,十二烷基苯磺酸钠0.1~0.5%,碱溶胀丙烯酸增稠剂0.5~1%,聚醚改性二甲基硅氧烷0.3~0.6%,丙烯酸共聚物钾盐0.1~0.5%,聚醚改性有机硅0.1~0.5%,余量为蒸馏水。
本发明在制备粉末涂料过程中,先将各助剂在蒸馏水中混合,再向其内加入颜填料形成分散均匀的混合底液,最后再将混合乳液与混合底液混合均匀。此种生产工艺能降低各种助剂的运动阻力,尤其是润湿剂和分散剂,使得它们能更好地吸附到颜填料表面,进而能大大提高颜填料的分散度,避免颗粒团聚的问题。防护涂料主要由成膜物质、颜填料、助剂和溶剂组成。其中,成膜物质是防护涂料的核心成分,本发明选用脂肪族粉末乳液和改性硅溶胶复配作为成膜物质,能提高涂料的机械强度、可剥性以及对酸碱盐溶液的耐受性。在脂肪族粉末乳液的制备中选用如下原料:选用异佛尔酮二异氰酸酯和聚丙二醇与聚乙二醇进行异氰酸酯基团和羟基的反应,可提高成膜的力学性能和耐能。在该反应时,加入丁酮可降低初级制品的黏度。由于当该反应的温度高于80℃时,-NCO的含量虽能迅速达到理论值,但此时副反应较多,这样易使产品质量不稳定;而当反应低于58℃时,又会因反应速度较慢而影响生产效率。因此,将该反应温度控制在58~80℃。选用二乙烯三胺作为扩链剂,它可对次级制品进行扩链,这样可提高涂料涂膜的拉伸强度。
为提高碱性硅溶胶与脂肪族粉末乳液复配时的稳定性,本发明对碱性硅溶胶进行了表面改性处理。其中,选用丙基三甲氧基硅烷作为硅烷偶联剂,可使粉末涂料能在室温环境下稳定贮存6~12个月而不出现凝胶现象。改性硅溶胶的加入可使纳米二氧化硅填充到涂料涂膜中,而二氧化硅的链段可与涂料中的有机高分子聚合物以及云母构成相互贯穿的网络状结构,这样,可提高有机聚合物的柔韧性,同时,涂料涂膜整体强度和硬度也会得到提高。由于改性硅溶胶的渗透性极好,它能够渗透到被保护的基材内部,使得涂料涂膜牢固地附着在基材上。改性硅溶胶还可提高涂料涂膜的致密度,这样可阻止水分和其他介质入侵,进而提高涂膜的耐腐蚀性。
颜填料是涂料配方中不可缺少的部分,在涂料中起着色和填充作用。二氧化钛是遮盖力十分好的白色颜料,且具有良好的紫外线吸收屏蔽功能。选用云母作为填料,可改善涂料涂膜的硬度、强度、耐磨性及基材附着力等性能。碱溶胀丙烯酸增稠剂能够提高分散体系的黏度,有利于云母在体系中的分散,防止云母下沉结块;同时还可增加涂料的稠度,提高涂料的稳定性。硅油的使用能够调节涂料涂膜的基材附着力,使涂膜有较好的剥离效果。十二烷基苯磺酸钠作为润湿剂,它可降低涂料涂膜的表面张力,使涂料能跟好地润湿基材,减少出现涂膜缩边现象,防止由于被保护物不清洁而使涂装不均匀。由于颜填料都具有疏,因而它们在水中的稳定性较差,容易团聚和下沉。而通过加入丙烯酸共聚物钾盐,则可保持颜填料在水中的分散性。聚醚改性二甲基硅氧烷作为流平剂,可降低涂料与底材之间的界面张力,提高涂料对被底材的润湿性,减少因底材而引起的缩孔、附着力不良等现象。涂料在生产、贮存和施工过程中都需要各种人工和机械操作,这样极易导致泡沫产生,而泡沫会阻碍云母的分散,并造成涂膜表面形成针孔和缩孔,从而影响涂料涂膜的外观、防腐性和耐候性。而加入聚醚改性有机硅则可有效改善上述问题。
为保证异氰酸基-NCO与所述羟基-OH反应的顺利进行,进一步地,所述脂肪族粉末乳液的原料中异氰酸基-NCO与所述羟基-OH的摩尔比为2.6~4:1。当-NCO/-OH<2.6时,会增大反应产物的黏度,而不易分散;而当-NCO/-OH>4时,脂肪族粉末乳液易凝胶,降低贮存期。
为达到良好的中和效果,进一步地,所述三乙胺的加入量与所述二羟甲基丙酸等摩尔量。
为在附着力与剥离强度之间达到平衡,进一步地,所述改性硅溶胶与所述脂肪族粉末乳液的质量比为1:4。改性硅溶胶的用量直接影响涂料的综合性能及生产成本。具体地,当改性硅溶胶的加入量过多时,不仅会导致涂膜变脆,涂膜附着力过大,不利于剥离;还会影响涂料体系的稳定性,增加涂料的生产成本。而改性硅溶胶用量过少时,纳米粒子在涂料中的作用力较弱,这样导致涂料的性能改善效果并不明显。因此改性硅溶胶在涂料中的用量必须合理适当。本发明选用该比值时,可使得涂料涂膜的拉伸强度和断裂伸长率得到增强,同时还保持有适中的剥离强度,良好的耐酸碱盐性能。
为提高颜填料于体系中的稳定性,进一步地,所述丙烯酸共聚物钾盐的加入量为所述二氧化钛和云母总量的2~4%。
进一步地,所述乙醇的固含量与所述碱性硅溶胶的固含量的质量比为1:1。加入乙醇能够减缓丙基三甲氧基硅烷中硅醇的自缩合,使大部分硅醇参与对碱性硅溶胶的改性反应,但是乙醇量过多并不利于改性反应,因而将乙醇与碱性硅溶胶中二氧化硅的质量比控制在1:1。
进一步地,所述丙基三甲氧基硅烷的加入量占所述碱性硅溶胶固含量的4~6%。丙基三甲氧基硅烷的用量必须足够才能有良好的改性效果。若用量不足,会使得碱性硅溶胶粒子表面的硅羟基改性不完全;若用量过多,多余的丙基三甲氧基硅烷可能会发生一些副反应而使粒子团聚或交联。
进一步地,所述工序1)中混合反应的温度控制在78~80℃,且混合反应时间为100~150min。由于异佛尔酮二异氰酸酯的反应活性较低,因而需工序1)的反应温度应高于75℃,再加上丁酮的沸点为79.6℃,因而可将温度控制在78~80℃。
为有效控制工序1)反应中-NCO基团的反应速率,进一步地,所述工序1)中还包括如下步骤:在混合反应期间,每隔5~8min测量一次所述第一反应釜内-NCO基团占体系的质量百分含量。
本发明具有以下有益效果:采用本发明制得的粉末涂料能对被保护物进行有效的封闭防护,防止被保护物受到污染、腐蚀和损伤。同时,该涂料还具有较强的内聚力、良好的可剥性、较高的涂膜强度及较高的稳定性。具体地,选用脂肪族粉末乳液和改性硅溶胶复配作为成膜物质,能提高涂料的机械强度、可剥性以及对酸碱盐溶液的耐受性。选用云母作为填料,可改善涂料涂膜的硬度、强度、耐磨性及基材附着力等性能。选用碱溶胀丙烯酸增稠剂能够提高分散体系的黏度,增加涂料的稠度,提高涂料的稳定性。选用硅油作为剥离剂,能调节涂料涂膜的基材附着力,提高涂膜的可剥离性。选用十二烷基苯磺酸钠作为润湿剂,可使涂料能跟好地润湿基材,减少出现涂膜缩边现象。选用丙烯酸共聚物钾盐作为分散剂,可保持颜填料在水中的分散性。选用聚醚改性二甲基硅氧烷作为流平剂,可降低涂料与底材之间的界面张力,提高涂料对被底材的润湿性。选用聚醚改性有机硅作为消泡剂,能减少泡沫的产生,从而改善涂料涂膜的外观、防腐性和耐候性。
具体实施方式
下面结合实施例对本发明做进一步的详细说明,但本发明的实施方式不限于此。
实施例1
粉末涂料的制备方法,包括如下工序:
1)在室温下向第一反应釜中加入异佛尔酮二异氰酸酯、聚丙二醇、聚乙二醇、二月桂酸二丁基锡及丁酮,再将温度升至58~80℃,使它们在第一反应釜内混合反应至体系中-NCO%值不再变化,得到初级制品,备用;
2)将温度控制在80℃,向工序1)所得的初级制品内加入二羟甲基丙酸并反应220~260min,再将温度降至38~43℃,加入三乙胺,得到次级制品;向盛有蒸馏水的第二反应釜中加入次级制品并使次级制品分散于蒸馏水中,再加入二乙烯三胺水溶液,制得脂肪族粉末乳液;
3)向盛有乙醇的烧瓶内加入丙基三甲氧基硅烷,按100~200r/min的转速搅拌混合5~10min,得到硅烷溶液;控制转速为200~300r/min,向盛有碱性硅溶胶的第三反应釜中滴加硅烷溶液;滴加完毕后,在50~65℃的温度下,按250r/min的转速搅拌混合450~500min,得到改性硅溶胶,备用;
4)在室温下向第四反应釜中加入工序2)所得的脂肪族粉末乳液和工序3)所得的改性硅溶胶,按200~300r/min的转速搅拌混合50~70min,得到混合乳液,备用;
5)向盛有蒸馏水的第五反应釜中加入适量的丙烯酸共聚物钾盐、碱溶胀丙烯酸增稠剂和聚醚改性有机硅,按200~300r/min的转速搅拌混合4~10min,再加入适量的二氧化钛、云母,按1500~1800r/min的转速搅拌混合35~42min,得到混合底液;
6)向工序5)所得的混合底液内加入工序4)所得的混合乳液,按350~500r/min的转速搅拌混合12~22min;再加入适量的十二烷基苯磺酸钠、聚醚改性二甲基硅氧烷、碱溶胀丙烯酸增稠剂、硅油、聚醚改性有机硅,按200~300r/min的转速搅拌混合15~20min,得到粉末涂料;
所述改性硅溶胶由以下质量配比的原料制得:碱性硅溶胶40~60份,乙醇30~50份,丙基三甲氧基硅烷1~6份;所述脂肪族粉末乳液由以下质量配比的原料制得:异佛尔酮二异氰酸酯40~80份,聚丙二醇25~40份,聚乙二醇25~80份,二羟甲基丙酸3~10份,丁酮50~80份,二乙烯三胺5~12份,三乙胺3~9份,二月桂酸二丁基锡1~3份,蒸馏水40~80份;所述粉末涂料由以下质量分数的原料制得:脂肪族粉末乳液60~80%,改性硅溶胶5~10%,二氧化钛2~5%,云母3~5%,硅油1~3%,十二烷基苯磺酸钠0.1~0.5%,碱溶胀丙烯酸增稠剂0.5~1%,聚醚改性二甲基硅氧烷0.3~0.6%,丙烯酸共聚物钾盐0.1~0.5%,聚醚改性有机硅0.1~0.5%,余量为蒸馏水。
本发明在制备粉末涂料过程中,先将各助剂在蒸馏水中混合,再向其内加入颜填料形成分散均匀的混合底液,最后再将混合乳液与混合底液混合均匀。此种生产工艺能降低各种助剂的运动阻力,尤其是润湿剂和分散剂,使得它们能更好地吸附到颜填料表面,进而能大大提高颜填料的分散度,避免颗粒团聚的问题。防护涂料主要由成膜物质、颜填料、助剂和溶剂组成。其中,成膜物质是防护涂料的核心成分,本发明选用脂肪族粉末乳液和改性硅溶胶复配作为成膜物质,能提高涂料的机械强度、可剥性以及对酸碱盐溶液的耐受性。在脂肪族粉末乳液的制备中选用如下原料:选用异佛尔酮二异氰酸酯和聚丙二醇与聚乙二醇进行异氰酸酯基团和羟基的反应,可提高成膜的力学性能和耐能。在该反应时,加入丁酮可降低初级制品的黏度。由于当该反应的温度高于80℃时,-NCO的含量虽能迅速达到理论值,但此时副反应较多,这样易使产品质量不稳定;而当反应低于58℃时,又会因反应速度较慢而影响生产效率。因此,将该反应温度控制在58~80℃。选用二乙烯三胺作为扩链剂,它可对次级制品进行扩链,这样可提高涂料涂膜的拉伸强度。
为提高碱性硅溶胶与脂肪族粉末乳液复配时的稳定性,本发明对碱性硅溶胶进行了表面改性处理。其中,选用丙基三甲氧基硅烷作为硅烷偶联剂,可使粉末涂料能在室温环境下稳定贮存6~12个月而不出现凝胶现象。改性硅溶胶的加入可使纳米二氧化硅填充到涂料涂膜中,而二氧化硅的链段可与涂料中的有机高分子聚合物以及云母构成相互贯穿的网络状结构,这样,可提高有机聚合物的柔韧性,同时,涂料涂膜整体强度和硬度也会得到提高。由于改性硅溶胶的渗透性极好,它能够渗透到被保护的基材内部,使得涂料涂膜牢固地附着在基材上。改性硅溶胶还可提高涂料涂膜的致密度,这样可阻止水分和其他介质入侵,进而提高涂膜的耐腐蚀性。
颜填料是涂料配方中不可缺少的部分,在涂料中起着色和填充作用。二氧化钛是遮盖力十分好的白色颜料,且具有良好的紫外线吸收屏蔽功能。选用云母作为填料,可改善涂料涂膜的硬度、强度、耐磨性及基材附着力等性能。碱溶胀丙烯酸增稠剂能够提高分散体系的黏度,有利于云母在体系中的分散,防止云母下沉结块;同时还可增加涂料的稠度,提高涂料的稳定性。硅油的使用能够调节涂料涂膜的基材附着力,使涂膜有较好的剥离效果。十二烷基苯磺酸钠作为润湿剂,它可降低涂料涂膜的表面张力,使涂料能跟好地润湿基材,减少出现涂膜缩边现象,防止由于被保护物不清洁而使涂装不均匀。由于颜填料都具有疏,因而它们在水中的稳定性较差,容易团聚和下沉。而通过加入丙烯酸共聚物钾盐,则可保持颜填料在水中的分散性。聚醚改性二甲基硅氧烷作为流平剂,可降低涂料与底材之间的界面张力,提高涂料对被底材的润湿性,减少因底材而引起的缩孔、附着力不良等现象。涂料在生产、贮存和施工过程中都需要各种人工和机械操作,这样极易导致泡沫产生,而泡沫会阻碍云母的分散,并造成涂膜表面形成针孔和缩孔,从而影响涂料涂膜的外观、防腐性和耐候性。而加入聚醚改性有机硅则可有效改善上述问题。
为保证异氰酸基-NCO与所述羟基-OH反应的顺利进行,优选地,所述脂肪族粉末乳液的原料中异氰酸基-NCO与所述羟基-OH的摩尔比为2.6~4:1。当-NCO/-OH<2.6时,会增大反应产物的黏度,而不易分散;而当-NCO/-OH>4时,脂肪族粉末乳液易凝胶,降低贮存期。
为达到良好的中和效果,优选地,所述三乙胺的加入量与所述二羟甲基丙酸等摩尔量。
为在附着力与剥离强度之间达到平衡,优选地,所述改性硅溶胶与所述脂肪族粉末乳液的质量比为1:4。改性硅溶胶的用量直接影响涂料的综合性能及生产成本。具体地,当改性硅溶胶的加入量过多时,不仅会导致涂膜变脆,涂膜附着力过大,不利于剥离;还会影响涂料体系的稳定性,增加涂料的生产成本。而改性硅溶胶用量过少时,纳米粒子在涂料中的作用力较弱,这样导致涂料的性能改善效果并不明显。因此改性硅溶胶在涂料中的用量必须合理适当。本发明选用该比值时,可使得涂料涂膜的拉伸强度和断裂伸长率得到增强,同时还保持有适中的剥离强度,良好的耐酸碱盐性能。
为提高颜填料于体系中的稳定性,优选地,所述丙烯酸共聚物钾盐的加入量为所述二氧化钛和云母总量的2~4%。
优选地,所述乙醇的固含量与所述碱性硅溶胶的固含量的质量比为1:1。加入乙醇能够减缓丙基三甲氧基硅烷中硅醇的自缩合,使大部分硅醇参与对碱性硅溶胶的改性反应,但是乙醇量过多并不利于改性反应,因而将乙醇与碱性硅溶胶中二氧化硅的质量比控制在1:1。
优选地,所述丙基三甲氧基硅烷的加入量占所述碱性硅溶胶固含量的4~6%。丙基三甲氧基硅烷的用量必须足够才能有良好的改性效果。若用量不足,会使得碱性硅溶胶粒子表面的硅羟基改性不完全;若用量过多,多余的丙基三甲氧基硅烷可能会发生一些副反应而使粒子团聚或交联。
优选地,所述工序1)中混合反应的温度控制在78~80℃,且混合反应时间为100~150min。由于异佛尔酮二异氰酸酯的反应活性较低,因而需工序1)的反应温度应高于75℃,再加上丁酮的沸点为79.6℃,因而可将温度控制在78~80℃。
为有效控制工序1)反应中-NCO基团的反应速率,优选地,所述工序1)中还包括如下步骤:在混合反应期间,每隔5~8min测量一次所述第一反应釜内-NCO基团占体系的质量百分含量。
以上内容是结合具体的优选实施方式对本发明作的进一步详细说明,不能认定本发明的具体实施方式只局限于这些说明。对于本发明所属技术领域的普通技术人员来说,在不脱离本发明的技术方案下得出的其他实施方式,均应包含在本发明的保护范围内。

Claims (1)

1.粉末涂料的制备方法,其特征在于:
包括如下工序:
1)在室温下向第一反应釜中加入异佛尔酮二异氰酸酯、聚丙二醇、聚乙二醇、二月桂酸二丁基锡及丁酮,再将温度升至58~80℃,使它们在第一反应釜内混合反应至体系中-NCO%值不再变化,得到初级制品,备用;
2)将温度控制在80℃,向工序1)所得的初级制品内加入二羟甲基丙酸并反应220~260min,再将温度降至38~43℃,加入三乙胺,得到次级制品;向盛有蒸馏水的第二反应釜中加入次级制品并使次级制品分散于蒸馏水中,再加入二乙烯三胺水溶液,制得脂肪族粉末乳液;
3)向盛有乙醇的烧瓶内加入丙基三甲氧基硅烷,按100~200r/min的转速搅拌混合5~10min,得到硅烷溶液;控制转速为200~300r/min,向盛有碱性硅溶胶的第三反应釜中滴加硅烷溶液;滴加完毕后,在50~65℃的温度下,按250r/min的转速搅拌混合450~500min,得到改性硅溶胶,备用;
4)在室温下向第四反应釜中加入工序2)所得的脂肪族粉末乳液和工序3)所得的改性硅溶胶,按200~300r/min的转速搅拌混合50~70min,得到混合乳液,备用;
5)向盛有蒸馏水的第五反应釜中加入适量的丙烯酸共聚物钾盐、碱溶胀丙烯酸增稠剂和聚醚改性有机硅,按200~300r/min的转速搅拌混合4~10min,再加入适量的二氧化钛、云母,按1500~1800r/min的转速搅拌混合35~42min,得到混合底液;
6)向工序5)所得的混合底液内加入工序4)所得的混合乳液,按350~500r/min的转速搅拌混合12~22min;再加入适量的十二烷基苯磺酸钠、聚醚改性二甲基硅氧烷、碱溶胀丙烯酸增稠剂、硅油、聚醚改性有机硅,按200~300r/min的转速搅拌混合15~20min,得到粉末涂料;
所述改性硅溶胶由以下质量配比的原料制得:碱性硅溶胶40~60份,乙醇30~50份,丙基三甲氧基硅烷1~6份;所述脂肪族粉末乳液由以下质量配比的原料制得:异佛尔酮二异氰酸酯40~80份,聚丙二醇25~40份,聚乙二醇25~80份,二羟甲基丙酸3~10份,丁酮50~80份,二乙烯三胺5~12份,三乙胺3~9份,二月桂酸二丁基锡1~3份,蒸馏水40~80份;所述粉末涂料由以下质量分数的原料制得:脂肪族粉末乳液60~80%,改性硅溶胶5~10%,二氧化钛2~5%,云母3~5%,硅油1~3%,十二烷基苯磺酸钠0.1~0.5%,碱溶胀丙烯酸增稠剂0.5~1%,聚醚改性二甲基硅氧烷0.3~0.6%,丙烯酸共聚物钾盐0.1~0.5%,聚醚改性有机硅0.1~0.5%,余量为蒸馏水。
CN201510954326.2A 2015-12-20 2015-12-20 一种粉末涂料的制备方法 Pending CN106893479A (zh)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201510954326.2A CN106893479A (zh) 2015-12-20 2015-12-20 一种粉末涂料的制备方法

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201510954326.2A CN106893479A (zh) 2015-12-20 2015-12-20 一种粉末涂料的制备方法

Publications (1)

Publication Number Publication Date
CN106893479A true CN106893479A (zh) 2017-06-27

Family

ID=59189070

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201510954326.2A Pending CN106893479A (zh) 2015-12-20 2015-12-20 一种粉末涂料的制备方法

Country Status (1)

Country Link
CN (1) CN106893479A (zh)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111876069A (zh) * 2020-07-01 2020-11-03 江苏瑞腾涂装科技有限公司 新型修复涂塑钢管

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111876069A (zh) * 2020-07-01 2020-11-03 江苏瑞腾涂装科技有限公司 新型修复涂塑钢管

Similar Documents

Publication Publication Date Title
CN106811072A (zh) 防腐蚀水性保护膜组合物的制备方法
CN106893471A (zh) 一种耐水性包装膜组合物的制备方法
CN106811081A (zh) 水性可剥离涂料的制备方法
CN106810658A (zh) 高稳定性防护用涂料的制备方法
CN106893474A (zh) 一种耐冷冻包装膜组合物的制备方法
CN106810986A (zh) 脂肪族水性聚氨酯乳液型可剥离涂料的制备方法
CN106810708A (zh) 高强度保护膜组合物涂膜的制备方法
CN106893479A (zh) 一种粉末涂料的制备方法
CN106811094A (zh) 含有改性硅溶胶的涂料涂膜的制备方法
CN106893470A (zh) 一种防火涂料的制备方法
CN106811066A (zh) 水性聚氨酯涂料的制备方法
CN106811062A (zh) 环氧改性聚氨酯包装涂料的制备方法
CN106811061A (zh) 保护用可剥离涂料的制备方法
CN106811078A (zh) 基于改性硅溶胶乳液的防护膜组合物
CN106811070A (zh) 耐水型包装膜组合物的制备方法
CN106811048A (zh) 改性硅溶胶与聚氨酯乳液复配的可剥离保护涂料
CN106811075A (zh) 改性硅溶胶与聚氨酯乳液复配式可剥离保护涂料的制备方法
CN106893478A (zh) 溶剂性涂料的制备方法
CN106893475A (zh) 一种防腐涂料的制备方法
CN106893476A (zh) 导电涂料的制备方法
CN106893472A (zh) 防水材料的制备方法
CN106811071A (zh) 基于改性硅溶胶乳液的包装体组合物的制备方法
CN106811093A (zh) 防护用涂料涂膜的制备方法
CN106811084A (zh) 可剥离保护膜组合物的制备方法
CN106893071A (zh) 一种耐高温包装膜组合物的制备方法

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
WD01 Invention patent application deemed withdrawn after publication
WD01 Invention patent application deemed withdrawn after publication

Application publication date: 20170627