WO2015127794A1 - 一种光固化涂料及其制备方法 - Google Patents

一种光固化涂料及其制备方法 Download PDF

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WO2015127794A1
WO2015127794A1 PCT/CN2014/090054 CN2014090054W WO2015127794A1 WO 2015127794 A1 WO2015127794 A1 WO 2015127794A1 CN 2014090054 W CN2014090054 W CN 2014090054W WO 2015127794 A1 WO2015127794 A1 WO 2015127794A1
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parts
weight parts
photoinitiator
deionized water
photocurable coating
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PCT/CN2014/090054
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李穆生
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李穆生
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    • C—CHEMISTRY; METALLURGY
    • C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
    • C09D4/00—Coating compositions, e.g. paints, varnishes or lacquers, based on organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond ; Coating compositions, based on monomers of macromolecular compounds of groups C09D183/00 - C09D183/16
    • C09D4/06—Organic non-macromolecular compounds having at least one polymerisable carbon-to-carbon unsaturated bond in combination with a macromolecular compound other than an unsaturated polymer of groups C09D159/00 - C09D187/00

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  • the invention relates to a photocurable coating and a preparation method thereof, and belongs to the technical field of chemical materials.
  • Photocurable coatings also known as photosensitive coatings, are mainly composed of photosensitive resins, photosensitizers (photoinitiators) and diluents, and some additives such as heat stabilizers are added to add pigments and fillers when preparing paints.
  • UV curing refers to the process of completely converting a reactive liquid material into a solid by ultraviolet light.
  • Conventional coating curing usually removes the solvent in the polymer solution by heating or physical drying to obtain a hardened paint film.
  • the mechanism of ultraviolet curing is that a network polymer can be formed by the interconnection of polymer chains and by the reaction of monomers or oligomers having at least two active sites per molecule. When ultraviolet radiation causes initiation, it is followed by a chain reaction with an extremely fast reaction rate. Since most monomer molecules usually do not produce active species under ultraviolet light, a photoinitiator must be added. Therefore, a typical UV-curing formulation must contain two basic components: it can effectively absorb ultraviolet light and efficiently produce activity. A photoinitiator and a monomer or oligomer having at least two unsaturated groups capable of forming a polymer network.
  • UV curing Compared with the general curing method, UV curing has the following advantages: 1 Short curing time, fast speed, curing in a few seconds, can be applied to occasions requiring fast curing; 2 No heating, this is for finishing wood, paper, plastic Materials that are not suitable for heating, materials with large heat capacity such as concrete and thick metal plates are very useful; 3 can be formulated into solvent-free products to reduce air pollution and contribute to environmental protection; 4 save energy, the efficiency of ultraviolet light source is higher than that of oven; Processes can be automated to increase automation in production, thereby increasing productivity and economics.
  • UV-curable oil-based coatings are currently the most widely used UV-curable coatings, but there are some disadvantages. Commonly used acrylates can cause skin irritation and have irritating odors. The curing mechanism is caused by free radicals and is generally affected by oxygen. The suppression is easy to cause poor surface curing; UV-curable powder coating is a new technology that combines traditional powder coating and UV curing technology, but the cost is high. UV-curable water-based coating combines the characteristics of traditional UV-curable coatings and water-based coatings. Compared with traditional photo-curing oil-based coatings, it has the advantages of wide source of raw materials, low price, strong applicability and good product quality.
  • the object of the present invention is to provide a photocurable coating which is an aqueous coating, which replaces the organic diluent with deionized water, reduces toxicity and irritation, is easier to manufacture and control viscosity, and obtains a cured film. It has strong adhesion to the substrate, high abrasion resistance, low shrinkage of the cured film, short curing time and good coating stability.
  • the technical solution adopted by the invention is: a photocurable coating consisting of the following parts by weight: 10-30 parts of polyester acrylate, 20-40 parts of epoxy acrylate, 20-30 parts of styrene, 1-10 parts of zinc oxide, 1-10 parts of talc, 50-200 parts of deionized water, dodecane 1 to 5 parts of sodium sulfonate, 1 to 8 parts of ammonium persulfate, 3 to 10 parts of potassium persulfate, and 1 to 5 parts of a photoinitiator.
  • each constituent raw material is: 10-25 parts of polyester acrylate, 20-30 parts of epoxy acrylate, 20-28 parts of styrene, 1-8 parts of zinc oxide, and 1-8 parts of talc. 70 to 180 parts of deionized water, 1 to 4 parts of sodium dodecyl sulfate, 1 to 5 parts of ammonium persulfate, 3 to 8 parts of potassium persulfate, and 1 to 4 parts of photoinitiator.
  • each constituent raw material is: 20 parts of polyester acrylate, 25 parts of epoxy acrylate, 25 parts of styrene, 5 parts of zinc oxide, 5 parts of talc, 120 parts of deionized water, and twelve. 3 parts of sodium alkyl sulfonate, 2.5 parts of ammonium persulfate, 5 parts of potassium persulfate, and 3 parts of photoinitiator.
  • the photoinitiator is a free radical polymerization photoinitiator.
  • the photoinitiator is preferably one of 2-hydroxy-2-methyl-1-phenylacetone, 1-hydroxycyclohexyl phenyl ketone, and methyl benzoylformate.
  • the method for preparing a photocurable coating according to the present invention comprises the following steps: mixing the raw materials in a ratio of 60 to 80 ° C for 0.5 to 1 h, and then reacting at 80 to 85 ° C under the protection of nitrogen in the reaction vessel 3 ⁇ 4h, after the reaction, it is naturally cooled to room temperature, and the pH is adjusted to 7.2-7.5 with ammonia water to obtain the product.
  • an aqueous UV-curable coating which replaces the organic diluent with deionized water, reduces toxicity and irritation, is easier to manufacture and control viscosity, and obtains curing.
  • the film has strong adhesion to the substrate, the shrinkage rate of the cured film is low, the curing time is short, and the stability of the coating is good.
  • Example 1 The composition of the present invention was made up of the following parts by weight: 20 parts of polyester acrylate, 25 parts of epoxy acrylate, 25 parts of styrene, 5 parts of zinc oxide, 5 parts of talc, and 120 parts of deionized water. 3 parts of sodium dodecyl sulfate, 2.5 parts of ammonium persulfate, 5 parts of potassium persulfate, 3 parts of 2-hydroxy-2-methyl-1-phenylacetone; prepared by the following steps: mixing raw materials in proportion The mixture was stirred at 60 ° C for 0.5 h, and then reacted at 82 ° C for 4 h under the protection of nitrogen in the reaction vessel. After the reaction, it was naturally cooled to room temperature, and the pH was adjusted to 7.4 with aqueous ammonia to obtain a product.
  • Example 2 The composition of the present invention was made up of the following parts by weight: 10 parts of polyester acrylate, 33 parts of epoxy acrylate, 20 parts of styrene, 5 parts of zinc oxide, 6 parts of talc, and 200 parts of deionized water. 2 parts of sodium dodecyl sulfonate, 8 parts of ammonium persulfate, 10 parts of potassium persulfate, and 3 parts of photoinitiator (1-hydroxycyclohexyl phenyl ketone); prepared by the following steps: mixing raw materials in proportion The mixture was stirred at 70 ° C for 0.5 h, and then reacted at 80 ° C for 4 h under the protection of nitrogen in the reaction vessel. After the reaction, it was naturally cooled to room temperature, and the pH was adjusted to 7.3 with ammonia water. That is the product.
  • Example 3 The composition of the present invention was made up of the following parts by weight: 25 parts of polyester acrylate, 20 parts of epoxy acrylate, 25 parts of styrene, 1 part of zinc oxide, 8 parts of talc, and 180 parts of deionized water. 3 parts of sodium dodecyl sulfate, 5 parts of ammonium persulfate, 3 parts of potassium persulfate, 1 part of 2-hydroxy-2-methyl-1-phenylacetone photoinitiator; prepared by the following steps: The mixture was mixed at 80 ° C for 1 h, and then reacted at 85 ° C for 3.5 h under the protection of nitrogen. After the reaction, it was naturally cooled to room temperature, and the pH was adjusted to 7.2 with aqueous ammonia to obtain a product.
  • Example 4 The composition of the present invention was made up of the following parts by weight: 22 parts of polyester acrylate, 20 parts of epoxy acrylate, 28 parts of styrene, 8 parts of zinc oxide, 1 part of talc, 70 parts of deionized water. 4 parts of sodium dodecyl sulfonate, 1 part of ammonium persulfate, 8 parts of potassium persulfate, 4 parts of photoinitiator (methyl benzoylformate); prepared by the following steps: mixing the raw materials in proportion at 80 ° C The mixture was stirred for 0.5 h, and then reacted at 85 ° C for 3 h under the protection of nitrogen in the reaction vessel. After the reaction, the mixture was naturally cooled to room temperature, and the pH was adjusted to 7.5 with aqueous ammonia to obtain a product.
  • photoinitiator methyl benzoylformate
  • Example 5 The composition of the present invention was made up of the following parts by weight: 30 parts of polyester acrylate, 24 parts of epoxy acrylate, 30 parts of styrene, 10 parts of zinc oxide, 6 parts of talc, 50 parts of deionized water. 1 part of sodium dodecyl sulfate, 2 parts of ammonium persulfate, 31 parts of potassium persulfate, 5 parts of photoinitiator (methyl benzoylformate); prepared by the following steps: mixing the raw materials in proportion at 70 ° C The mixture was stirred for 1 hour, and then reacted at 80 ° C for 4 hours under the protection of nitrogen in the reaction vessel. After the reaction, it was naturally cooled to room temperature, and the pH was adjusted to 7.2 with aqueous ammonia to obtain a product.
  • photoinitiator methyl benzoylformate

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Wood Science & Technology (AREA)
  • Organic Chemistry (AREA)
  • Paints Or Removers (AREA)
  • Macromonomer-Based Addition Polymer (AREA)

Abstract

一种光固化涂料，由以下重量份数的原料组成：聚酯丙烯酸酯10～30份、环氧丙烯酸酯20～40份、苯乙烯20～30份、氧化锌1～10份、滑石粉1～10份、去离子水50～200份、十二烷基磺酸钠1～5份、过硫酸铵1～8份、过硫酸钾3～10份、光引发剂1～5份。该涂料以去离子水替代有机稀释剂，固化时间短，稳定性佳，所得的固化膜对底材粘附力强，耐磨度高，固化膜收缩率低。

Description

一种光固化涂料及其制备方法 技术领域
本发明涉及一种光固化涂料及其制备方法，属于化工材料技术领域。
背景技术
光固化涂料又称光敏涂料，主要由光敏树脂、光敏剂(光引发剂)和稀释剂组成，同时加入一些添加剂，如热稳定剂，制备色漆时加入颜料和填料。
紫外光固化是指以紫外线为能源引发反应性的液体物料完全快速转变成固体的过程。传统的涂料固化通常是通过加热即物理干燥的方法除去高分子溶液中的溶剂，得到硬化的漆膜。紫外光固化机理为：一个网状聚合物既能由高分子链相互连接形成，又能通过那些每个分子上至少含有2个活性点的单体或低聚物的反应而形成。当紫外光辐射导致引发时，随即是一种反应速度极快的链反应。由于大部分单体分子通常在紫外光辐射下不产生活性种，必须加入光引发剂，因此典型的紫外光固化配方必须包含2个最基本组分：能有效地吸收紫外光并能高效产生活性种的光引发剂和至少带有2个能形成聚合物网络的不饱和基团的单体或低聚物。
与一般固化方法比较，紫外光固化有下列优点：①固化时间短，速度快，可在几秒内固化，可以应用于要求快速固化的场合；②不需要加热，这对于涂饰木材、纸张、塑料等不宜加热的材料及混凝土、厚金属板等热容量大的材料十分有用；③可配制成无溶剂产品，减少大气污染，有利于环保；④节省能量，紫外光源的效率要高于烘箱；⑤固化过程可以自动化操作，提高生产中的自动化程度，从而提高生产效率和经济效益。
紫外光固化油性涂料是目前应用最广泛的一类紫外固化涂料，但是存在着一些缺点，常用的丙烯酸酯会引起皮肤过敏，并具有刺激性气味，且固化机理属于自由基引发，一般要受氧气的阻抑，易造成表面固化不良等；紫外光固化粉末涂料是一项将传统粉末涂料和紫外固化技术相结合的新技术，但成本较高。紫外光固化水性涂料结合了传统紫外光固化涂料和水性涂料的各自特点，相对于传统光固化油性涂料，具有原料来源广、价格低廉、适用性强、产品质量好等优点。
发明内容
本发明的目的是提供一种光固化涂料，该种光固化涂料为水性涂料，以去离子水替代有机稀释剂，降低了毒性和刺激性，更易于生产制造及控制粘度，所获得的固化膜对底材的粘附力强、耐磨度高，固化膜收缩率低，固化时间短，涂料稳定性佳。
本发明所采用的技术方案是：一种光固化涂料，由以下重量份数的原料组成： 聚酯丙烯酸酯10-30份、环氧丙烯酸酯20～40份、苯乙烯20～30份、氧化锌1～10份、滑石粉1～10份、去离子水50～200份、十二烷基磺酸钠1～5份、过硫酸铵1～8份、过硫酸钾3～10份、光引发剂1～5份。
各组成原料优选的重量份数配比为：聚酯丙烯酸酯10-25份、环氧丙烯酸酯20～30份、苯乙烯20～28份、氧化锌1～8份、滑石粉1～8份、去离子水70～180份、十二烷基磺酸钠1～4份、过硫酸铵1～5份、过硫酸钾3～8份、光引发剂1～4份。
各组成原料进一步优选的重量份数配比为：聚酯丙烯酸酯20份、环氧丙烯酸酯25份、苯乙烯25份、氧化锌5份、滑石粉5份、去离子水120份、十二烷基磺酸钠3份、过硫酸铵2.5份、过硫酸钾5份、光引发剂3份。
所述光引发剂为自由基聚合光引发剂。所述光引发剂优选2-羟基-2-甲基-1-苯基丙酮、1-羟基环己基苯基甲酮、苯甲酰甲酸甲酯中的一种。
本发明所述光固化涂料的制备方法，其特征在于：包括以下步骤：把原料按比例混合于60～80℃保温搅拌0.5～1h，然后在反应釜于氮气的保护下80～85℃反应3～4h，反应后自然冷却至室温，用氨水调制pH为7.2～7.5，即得产品。
本发明相对于现有技术的有益效果是：是一种水性的紫外光固化涂料，以去离子水替代有机稀释剂，降低了毒性和刺激性，更易于生产制造及控制粘度，所获得的固化膜对底材的粘附力强，固化膜收缩率低，固化时间短，涂料的稳定性佳。
具体实施方式
下面通过实施例对本发明做进一步详细说明，这些实施例仅用来说明本发明，并不限制本发明的范围。
实施例1本实施例的采用以下重量份数的原料组成：聚酯丙烯酸酯20份、环氧丙烯酸酯25份、苯乙烯25份、氧化锌5份、滑石粉5份、去离子水120份、十二烷基磺酸钠3份、过硫酸铵2.5份、过硫酸钾5份、2-羟基-2-甲基-1-苯基丙酮3份；采用以下步骤制备：把原料按比例混合于60℃保温搅拌0.5h，然后在反应釜于氮气的保护下82℃反应4h，反应后自然冷却至室温，用氨水调制pH为7.4，即得产品。
实施例2本实施例的采用以下重量份数的原料组成：聚酯丙烯酸酯10份、环氧丙烯酸酯33份、苯乙烯20份、氧化锌5份、滑石粉6份、去离子水200份、十二烷基磺酸钠2份、过硫酸铵8份、过硫酸钾10份、光引发剂(1-羟基环己基苯基甲酮)3份；采用以下步骤制备：把原料按比例混合于70℃保温搅拌0.5h，然后在反应釜于氮气的保护下80℃反应4h，反应后自然冷却至室温，用氨水调制pH为7.3， 即得产品。
实施例3本实施例的采用以下重量份数的原料组成：聚酯丙烯酸酯25份、环氧丙烯酸酯20份、苯乙烯25份、氧化锌1份、滑石粉8份、去离子水180份、十二烷基磺酸钠3份、过硫酸铵5份、过硫酸钾3份、2-羟基-2-甲基-1-苯基丙酮光引发剂1份；采用以下步骤制备：把原料按比例混合于80℃保温搅拌1h，然后在反应釜于氮气的保护下85℃反应3.5h，反应后自然冷却至室温，用氨水调制pH为7.2，即得产品。
实施例4本实施例的采用以下重量份数的原料组成：聚酯丙烯酸酯22份、环氧丙烯酸酯20份、苯乙烯28份、氧化锌8份、滑石粉1份、去离子水70份、十二烷基磺酸钠4份、过硫酸铵1份、过硫酸钾8份、光引发剂(苯甲酰甲酸甲酯)4份；采用以下步骤制备：把原料按比例混合于80℃保温搅拌0.5h，然后在反应釜于氮气的保护下85℃反应3h，反应后自然冷却至室温，用氨水调制pH为7.5，即得产品。
实施例5本实施例的采用以下重量份数的原料组成：聚酯丙烯酸酯30份、环氧丙烯酸酯24份、苯乙烯30份、氧化锌10份、滑石粉6份、去离子水50份、十二烷基磺酸钠1份、过硫酸铵2份、过硫酸钾31份、光引发剂(苯甲酰甲酸甲酯)5份；采用以下步骤制备：把原料按比例混合于70℃保温搅拌1h，然后在反应釜于氮气的保护下80℃反应4h，反应后自然冷却至室温，用氨水调制pH为7.2，即得产品。

Claims (6)

  1. 一种光固化涂料，其特征在于：由以下重量份数的原料组成：聚酯丙烯酸酯10-30份、环氧丙烯酸酯20～40份、苯乙烯20～30份、氧化锌1～10份、滑石粉1～10份、去离子水50～200份、十二烷基磺酸钠1～5份、过硫酸铵1～8份、过硫酸钾3～10份、光引发剂1～5份。
  2. 根据权利要求1所述的光固化涂料，其特征在于：各组成原料的重量份数为：聚酯丙烯酸酯10-25份、环氧丙烯酸酯20～30份、苯乙烯20～28份、氧化锌1～8份、滑石粉1～8份、去离子水70～180份、十二烷基磺酸钠1～4份、过硫酸铵1～5份、过硫酸钾3～8份、光引发剂1～4份。
  3. 根据权利要求1所述的光固化涂料，其特征在于：各组成原料的重量份数为：聚酯丙烯酸酯20份、环氧丙烯酸酯25份、苯乙烯25份、氧化锌5份、滑石粉5份、去离子水120份、十二烷基磺酸钠3份、过硫酸铵2.5份、过硫酸钾5份、光引发剂3份。
  4. 根据权利要求1所述的光固化涂料，其特征在于：所述光引发剂为自由基聚合光引发剂。
  5. 根据权利要求4所述的光固化涂料，其特征在于：所述光引发剂为2-羟基-2-甲基-1-苯基丙酮、1-羟基环己基苯基甲酮、苯甲酰甲酸甲酯中的一种。
  6. 一种权利要求1所述光固化涂料的制备方法，其特征在于：包括以下步骤：把原料按比例混合于60～80℃保温搅拌0.5～1h，然后在反应釜于氮气的保护下80～85℃反应3～4h，反应后自然冷却至室温，用氨水调制pH为7.2～7.5，即得产品。
PCT/CN2014/090054 2014-02-25 2014-10-31 一种光固化涂料及其制备方法 WO2015127794A1 (zh)

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