CN107073759A - 可光固化组合物 - Google Patents
可光固化组合物 Download PDFInfo
- Publication number
- CN107073759A CN107073759A CN201580059762.1A CN201580059762A CN107073759A CN 107073759 A CN107073759 A CN 107073759A CN 201580059762 A CN201580059762 A CN 201580059762A CN 107073759 A CN107073759 A CN 107073759A
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- CN
- China
- Prior art keywords
- methyl
- compounds
- photocurable composition
- ethylenic
- ethylenically unsaturated
- 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.)
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Classifications
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- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C35/00—Heating, cooling or curing, e.g. crosslinking or vulcanising; Apparatus therefor
- B29C35/02—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould
- B29C35/08—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould by wave energy or particle radiation
- B29C35/0805—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould by wave energy or particle radiation using electromagnetic radiation
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- B28B7/00—Moulds; Cores; Mandrels
- B28B7/0064—Moulds characterised by special surfaces for producing a desired surface of a moulded article, e.g. profiled or polished moulding surfaces
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- B28B7/00—Moulds; Cores; Mandrels
- B28B7/34—Moulds, cores, or mandrels of special material, e.g. destructible materials
- B28B7/346—Manufacture of moulds
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B28B—SHAPING CLAY OR OTHER CERAMIC COMPOSITIONS; SHAPING SLAG; SHAPING MIXTURES CONTAINING CEMENTITIOUS MATERIAL, e.g. PLASTER
- B28B7/00—Moulds; Cores; Mandrels
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- B28B7/364—Linings or coatings, e.g. removable, absorbent linings, permanent anti-stick coatings; Linings becoming a non-permanent layer of the moulded article of plastic material or rubber
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- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C33/00—Moulds or cores; Details thereof or accessories therefor
- B29C33/38—Moulds or cores; Details thereof or accessories therefor characterised by the material or the manufacturing process
- B29C33/3842—Manufacturing moulds, e.g. shaping the mould surface by machining
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C33/00—Moulds or cores; Details thereof or accessories therefor
- B29C33/42—Moulds or cores; Details thereof or accessories therefor characterised by the shape of the moulding surface, e.g. ribs or grooves
- B29C33/424—Moulding surfaces provided with means for marking or patterning
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C33/00—Moulds or cores; Details thereof or accessories therefor
- B29C33/56—Coatings, e.g. enameled or galvanised; Releasing, lubricating or separating agents
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C39/00—Shaping by casting, i.e. introducing the moulding material into a mould or between confining surfaces without significant moulding pressure; Apparatus therefor
- B29C39/003—Shaping by casting, i.e. introducing the moulding material into a mould or between confining surfaces without significant moulding pressure; Apparatus therefor characterised by the choice of material
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C39/00—Shaping by casting, i.e. introducing the moulding material into a mould or between confining surfaces without significant moulding pressure; Apparatus therefor
- B29C39/02—Shaping by casting, i.e. introducing the moulding material into a mould or between confining surfaces without significant moulding pressure; Apparatus therefor for making articles of definite length, i.e. discrete articles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B33—ADDITIVE MANUFACTURING TECHNOLOGY
- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y70/00—Materials specially adapted for additive manufacturing
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- 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
- C08F2/00—Processes of polymerisation
- C08F2/46—Polymerisation initiated by wave energy or particle radiation
- C08F2/48—Polymerisation initiated by wave energy or particle radiation by ultraviolet or visible light
-
- 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
- C09D11/00—Inks
- C09D11/02—Printing inks
- C09D11/10—Printing inks based on artificial resins
- C09D11/101—Inks specially adapted for printing processes involving curing by wave energy or particle radiation, e.g. with UV-curing following the printing
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C35/00—Heating, cooling or curing, e.g. crosslinking or vulcanising; Apparatus therefor
- B29C35/02—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould
- B29C35/08—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould by wave energy or particle radiation
- B29C35/0805—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould by wave energy or particle radiation using electromagnetic radiation
- B29C2035/0827—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould by wave energy or particle radiation using electromagnetic radiation using UV radiation
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C35/00—Heating, cooling or curing, e.g. crosslinking or vulcanising; Apparatus therefor
- B29C35/02—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould
- B29C35/08—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould by wave energy or particle radiation
- B29C35/0805—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould by wave energy or particle radiation using electromagnetic radiation
- B29C2035/0833—Heating or curing, e.g. crosslinking or vulcanizing during moulding, e.g. in a mould by wave energy or particle radiation using electromagnetic radiation using actinic light
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C64/00—Additive manufacturing, i.e. manufacturing of three-dimensional [3D] objects by additive deposition, additive agglomeration or additive layering, e.g. by 3D printing, stereolithography or selective laser sintering
- B29C64/10—Processes of additive manufacturing
- B29C64/106—Processes of additive manufacturing using only liquids or viscous materials, e.g. depositing a continuous bead of viscous material
- B29C64/124—Processes of additive manufacturing using only liquids or viscous materials, e.g. depositing a continuous bead of viscous material using layers of liquid which are selectively solidified
- B29C64/129—Processes of additive manufacturing using only liquids or viscous materials, e.g. depositing a continuous bead of viscous material using layers of liquid which are selectively solidified characterised by the energy source therefor, e.g. by global irradiation combined with a mask
- B29C64/135—Processes of additive manufacturing using only liquids or viscous materials, e.g. depositing a continuous bead of viscous material using layers of liquid which are selectively solidified characterised by the energy source therefor, e.g. by global irradiation combined with a mask the energy source being concentrated, e.g. scanning lasers or focused light sources
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Abstract
本发明涉及一种用于制造模具用模头的方法,所述模具用于生产具有三维纹理的砖。
Description
技术领域
本发明涉及一种用于制造模具用模头的方法,所述模具用于生产具有三维纹理的砖。
现有技术
随着持续增长的产品选择和款式选项的数量,陶瓷砖的世界是广阔且壮观的。
在众多建筑设计中的一个流行选项是使用各种各样在暴露表面具有三维(3D)纹理的砖,从而创造“浅浮雕”的外观和感觉。这些特定砖兼顾用于地面装饰和墙面装饰以及其它用途,具有不同的图案和尺寸,提供了广泛范围的纹理。
例如,陶器和瓷器制造商创造了具有以下特点的砖,所述砖提供类似天然外观和主题(例如天然石头或木头)的纹理和色彩。其它则显示出复杂且独特的三维几何图案。
用于生产陶瓷砖的常规过程是形成具有约6/12wt%水的研磨矿物材料的粉末加料量。将仍是粉末状的混合物在模具中压制(成型),其组合为粘合砖体,所述粘合砖体坚固到足以抵抗温和处理。然后,“生”砖进行修整、干燥、并用釉料涂布。在置于耐火定位器(refractory setter)上之后,将砖输送通过炉进行最终烧制。
用于在砖上获得3D纹理的一个方法是考虑用装有模头的模具成型,所述模头具有(负向)3D纹理表面。例如,通过在合适基质上施加具有3D纹理表面的弹性体材料、或者通过用酸(化学蚀刻)雕刻或者通过激光烧蚀雕刻金属模头,获得这些模头。
施加弹性体材料的传统技术需要非常复杂的制造过程,并且不能以连续工艺制造用于砖成型的模头。
还实施了金属表面的化学蚀刻,但是其不能实现高精度的蚀刻深度,并且需要使用大量危险且存在环境问题的无机酸。
激光烧蚀是一种慢速技术,并且实践中并不能制造用于大尺寸砖的模头。
最终,对于变得越来越常见的具有非常精细细节的复杂且多变图案印象,这些模头的造价实际上变得异常高。
现在我们发现,通过将特定可光固化组合物适当涂敷于基础模头(base-die)上,并对该特定可光固化组合物进行光固化,产生具有三维图案的膜,可以在用于砖成型的模具用模头上获得三维纹理。使用这些特定组合物,可以以低成本容易地制造具有种类繁多的3D纹理、同时具有复杂且精细图案的模头,特别是当用数字设备涂敷组合物时。用这些组合物获得的具有三维纹理的膜呈现出高耐磨性、对基质的高粘附性、对粉末混合物的低粘性、以及良好的砖纹理化性能。此外,易于从3D模头上去除膜,并且基础模头可以重复使用。
发明内容
因此,本发明的一个目的在于提供一种用于制造具有3D纹理的砖的方法,所述方法包括用装备有模头的模具对所述砖进行成型的步骤,所述模头由包括以下步骤的工艺制造:
I)提供含有如下组分a)和b)的可光固化组合物:
a)70-99重量%(wt%)、优选75~95wt%的至少一种烯键式不饱和化合物;
b)1-12wt%、优选3~10wt%的至少一种光引发剂;
II)将所述可光固化组合物涂敷到基础模头表面上,以形成具有三维图案的膜;
III)通过将基础模头表面曝露于波长200~600nm的光,对所述可光固化组合物进行光固化;
前提是,当膜通过在钢板上对200g/m2的所述可光固化组合物进行光固化而获得的情况下,其根据标准方法ISO1522:2006确定的弹性硬度为50~300秒、优选80~250秒、更优选100~220秒。
发明详述
本领域中的专家可以很容易地发现,在涂料工业中使用的烯键式不饱和化合物中,合适的化合物及其混合物为膜提供了实现本发明所需的弹性硬度。用于制造硬涂层的那些化合物是特别优选的。
可以在每分子具有一个或多个不饱和基团的化合物中选择烯键式不饱和化合物,并且这些化合物可以单独使用、或者作为混合物组合使用。它们可以具有低分子量(单体的)、或高分子量(低聚的)。
优选,组分a)是具有不同数量烯键式不饱和基团的化合物的混合物。
在本发明的一个实施方式中,基于组分a)的总重量,组分a)由如下组成:0~40wt%的具有一个烯键式不饱和基团的烯键式不饱和化合物、0~60wt%的具有两个烯键式不饱和基团的烯键式不饱和化合物、0~70wt%的具有三个烯键式不饱和基团的烯键式不饱和化合物、以及0~70wt%的具有四个或更多个烯键式不饱和基团的烯键式不饱和化合物。
优选,基于组分a)的总重量,组分a)由如下组成:0~20wt%的具有一个烯键式不饱和基团的烯键式不饱和化合物、0~55wt%的具有两个烯键式不饱和基团的烯键式不饱和化合物、0~60wt%的具有三个烯键式不饱和基团的烯键式不饱和化合物、以及0~60wt%的具有四个或更多个烯键式不饱和基团的烯键式不饱和化合物。
更优选,分别以10~50wt%、10~60wt%、10~60wt%的量包含所述具有两个烯键式不饱和基团的化合物、具有三个烯键式不饱和基团的化合物、以及具有四个或更多个烯键式不饱和基团的化合物,前提是它们构成100wt%的组分a)。
优选,组分a)的烯键式不饱和化合物选自在每分子具有一个或多个烯键式不饱和基团的(甲基)丙烯酸酯化合物。
在表达(甲基)丙烯酸酯化合物时,我们同时包括甲基丙烯酸酯化合物和丙烯酸酯化合物,其选自:(甲基)丙烯酸酯化合物、氨基甲酸酯(甲基)丙烯酸酯化合物、环氧(甲基)丙烯酸酯化合物、聚酯(甲基)丙烯酸酯化合物、聚醚(甲基)丙烯酸酯化合物、硅酮(甲基)丙烯酸酯化合物、(甲基)丙烯酸类(甲基)丙烯酸酯化合物、及其混合物。
具有一个烯键式不饱和基团的(甲基)丙烯酸酯化合物的具体例子包括:(甲基)丙烯酸2-羟乙基酯、(甲基)丙烯酸2-羟丙基酯、(甲基)丙烯酸异丁基酯、(甲基)丙烯酸叔丁基酯、(甲基)丙烯酸2-乙基己基酯、(甲基)丙烯酸2-乙基己基卡必醇酯、(甲基)丙烯酸丁氧基乙酯、(甲基)丙烯酸二乙氧基乙酯、(甲基)丙烯酸甲氧基三乙二醇酯、(甲基)丙烯酸甲氧基聚乙二醇酯、(甲基)丙烯酸硬脂酯、(甲基)丙烯酸环己基酯、(甲基)丙烯酸四氢糠酯、(甲基)丙烯酸异冰片酯、(甲基)丙烯酸二环戊烯酯、(甲基)丙烯酸二环戊酯、(甲基)丙烯酸二环苄酯、N-羟甲基丙烯酰胺、N-甲氧基甲基丙烯酰胺、N-乙氧基甲基丙烯酰胺、N-正丁氧基甲基丙烯酰胺、N-甲基丙烯酰胺、N,N-二甲基丙烯酰胺、(甲基)丙烯酸N,N-二甲基氨乙酯、N,N-二甲基氨丙基丙烯酰胺、丙烯酰基吗啉、(甲基)丙烯酸二缩水甘油酯、(甲基)丙烯酸正丁酯、(甲基)丙烯酸乙酯、及它们的混合物。
具有两个烯键式不饱和基团的(甲基)丙烯酸酯的例子包括以下化合物:二(甲基)丙烯酸乙二醇酯、二(甲基)丙烯酸二乙二醇酯、二(甲基)丙烯酸三乙二醇酯、二(甲基)丙烯酸丙二醇酯、二(甲基)丙烯酸二丙二醇酯、二(甲基)丙烯酸三丙二醇酯、二(甲基)丙烯酸1,3-丁二醇酯、二(甲基)丙烯酸1,4-丁二醇酯、二(甲基)丙烯酸1,5-戊二醇酯、二(甲基)丙烯酸异戊二醇酯、二(甲基)丙烯酸1,6-己二醇酯、二(甲基)丙烯酸新戊二醇酯、二(甲基)丙烯酸辛二醇酯、二(甲基)丙烯酸1,2-环己二醇酯、二(甲基)丙烯酸1,4-环己二醇酯、氢化双酚A二(甲基)丙烯酸酯、二(甲基)丙烯酸甘油酯、三羟甲基乙烷二(甲基)丙烯酸酯、三羟甲基丙烷二(甲基)丙烯酸酯、具有平均4~25个重复亚乙氧基的二(甲基)丙烯酸聚乙二醇酯、具有平均4~25个重复亚丙氧基的二(甲基)丙烯酸聚丙二醇酯、乙氧基化双酚A二(甲基)丙烯酸酯和丙氧基化双酚二(甲基)丙烯酸酯、以及它们的混合物。
具有三个烯键式不饱和基团的(甲基)丙烯酸酯化合物的例子是:三(甲基)丙烯酸甘油酯、乙氧基化或丙氧基化的三(甲基)丙烯酸甘油酯、三羟甲基乙烷三(甲基)丙烯酸酯、三羟甲基丙烷三(甲基)丙烯酸酯、乙氧基化或丙氧基化的三羟甲基丙烷三(甲基)丙烯酸酯、三(甲基)丙烯酸双甘油酯、三(甲基)丙烯酸赤藓糖醇酯、三(甲基)丙烯酸季戊四醇酯、二-三羟甲基丙烷三(甲基)丙烯酸酯和三[(甲基)丙烯酰氧基乙基]异氰尿酸酯、以及它们的混合物。
具有超过三个烯键式不饱和基团的(甲基)丙烯酸酯化合物的例子是:四(甲基)丙烯酸赤藓糖醇酯、四(甲基)丙烯酸季戊四醇酯、四(甲基)丙烯酸双甘油酯、和二-三羟甲基丙烷四(甲基)丙烯酸酯;五价醇的(甲基)丙烯酸酯化合物,诸如四(甲基)丙烯酸三甘油酯和五(甲基)丙烯酸三甘油酯;以及六价醇的(甲基)丙烯酸酯化合物,诸如五(甲基)丙烯酸二季戊四醇酯和六(甲基)丙烯酸二季戊四醇酯、或者它们的混合物。
具有两个或更多个烯键式不饱和基团的氨基甲酸酯(甲基)丙烯酸酯包括:氨基甲酸酯(甲基)丙烯酸酯,其是通过可具有氧化烯链的(甲基)丙烯酸2-羟乙酯与六亚甲基二异氰酸酯、异佛尔酮二异氰酸酯、2,4,4-三甲基六亚甲基二异氰酸酯、二环己基甲烷二异氰酸酯、降冰片烯二异氰酸酯、或甲基环己烷二异氰酸酯反应获得的反应混合物,或者,是通过可具有氧化烯链的(甲基)丙烯酸2-羟乙酯与氨基甲酸酯预聚物反应获得的反应混合物,所述氨基甲酸酯预聚物通过如下制造:将上述异氰酸酯与低分子量多官能多元醇例如具有重复单元(诸如环氧乙烷或环氧丙烷或环氧己烷)的聚亚烷基二醇、聚酯二醇、聚碳酸酯二醇和聚丁二烯二醇,或者低分子量多元醇(诸如乙二醇、丙二醇、1,3-丙二醇、1,4-丁二醇、1,5-戊二醇、1,6-己二醇、新戊二醇、二乙二醇、二丙二醇、1,4-环己二醇、1,4-环己烷二甲醇、甘油、三羟甲基丙烷或季戊四醇)反应。
而且,可以使用高支化(甲基)丙烯酸酯树脂,其通常是氨基甲酸酯(甲基)丙烯酸酯或聚酯(甲基)丙烯酸酯,并且可以具有至多18个不饱和基团。
包含酸基团、在氮上具有供电子取代基的叔胺(例如,购自Allnex工业公司的Ebecryl P104、Ebecryl P105、Ebecryl 7100)的(甲基)丙烯酸酯也可适用于实现本发明,所述酸基团通常是羧酸基团(诸如丙烯酸,例如购自Sartomer Europe公司的CD9051、CD9051;购自Allnex工业公司的Ebecryl 168和Ebecryl 170)。
硅酮(甲基)丙烯酸酯化合物提供具有不粘的表面的平滑膜,并且也适合用实现本发明。这些烯键式不饱和化合物的例子是购自Allnex公司的Ebecryl 350和Ebecryl 1360。
可用作组分b)的光引发剂的例子包括:酰基氧化膦(单酰基氧化膦和二酰基氧化膦皆是)、3-酰基香豆素衍生物、芳香族鎓盐化合物、有机过氧化物、噻吨酮类、六芳基双咪唑、O-酰基肟酯、硼酸盐/酯化合物、嗪鎓化合物、茂金属化合物、二苯甲酮类、α-二酮、酮砜、α-氨基酮、苯偶姻和苯偶姻醚、苯偶酰缩酮、α-羟基酮、双功能光引发剂、以及它们的混合物。噻吨酮类的例子为:噻吨酮、二乙基噻吨酮、2-异丙基噻吨酮、2-氯噻吨酮、2,4-二乙基噻吨酮、2-十二烷基噻吨酮、2,4-二甲基噻吨酮、1-甲氧基羰基噻吨酮、2-乙氧基羰基噻吨酮、3-(2-甲氧基乙氧基羰基)噻吨酮、4-丁氧基羰基噻吨酮、3-丁氧基羰基-7-甲基噻吨酮、或者如专利申请WO/2012/062692中描述的那些噻吨酮类诸如正十二烷基-7-甲基-噻吨酮-3-羧酸盐/酯、N,N-二异丁基-7-甲基-噻吨酮-3-脲、以及它们的混合物。
α-羟基酮和α-氨基酮的例子为:1-羟基环己基苯基酮、2-羟基-2甲基-1-苯基丙烷-1-酮、1-[4-(2-羟基乙氧基)苯基]-2-羟基-2-甲基-1-丙烷-1-酮、2-羟基-1-{4-[4-(2-羟基-2-甲基-丙酰基)-苄基]苯基}-2-甲基-丙烷-1-酮、2-羟基-1[4-(4-(2-羟基-2-甲基丙酰基)苯氧基)苯基]-2-甲基丙-1-酮、2-甲基-1-(4-甲基噻吩基)-2-吗啉代丙烷-1-酮)、2-苄基-2-二甲基氨基-1-(4-吗啉代苯基)-丁-1-酮、(2-(二甲基氨基)-2-[(4-甲基苯基)甲基]-1-[4-(4-吗啉基)苯基]-1-丁酮)、以及它们的混合物。
合适的酮砜的例子为1-[4-[(4-苯甲酰基-苯基)-硫]-苯基]-2-甲基-2-[(4-甲基-苯基)-磺酰基]-丙-1-酮。
O-酰基肟酯光引发剂的例子为1,2-辛二酮、1-[4-(苯硫基)苯基]-,2-(O-苯甲酰基肟)、乙酮、1-[9-乙基-6-(2-甲基苯甲酰基)-9H-咔唑-3-基],1-(O-乙酰基肟)、及它们的混合物。
酰基氧化膦光引发剂的例子包括但不限于:双(2,4,6-三甲基苯甲酰基)苯基氧化膦、2,4,6-三甲基苯甲酰基-二苯基氧化膦和双(2,6-二甲氧基苯甲酰基)-2,4,4-三甲基戊基氧化膦。
二苯甲酮类的例子是:二苯甲酮、4-苯基二苯甲酮、4-甲氧基二苯甲酮、4-氯二苯甲酮、4,4'-二甲氧基二苯甲酮、4,4'-二甲基二苯甲酮、4,4'-二氯二苯甲酮、4,4'-二甲基氨基二苯甲酮、4,4'-二乙基氨基二苯甲酮、4-甲基二苯甲酮、4,4'-二氨基二苯甲酮、2,4,6-三甲基二苯甲酮、4-(4-甲基噻吩基)二苯甲酮、和它们的混合物。
3-酰基香豆素衍生物的例子是:3-苯甲酰基香豆素、3-苯甲酰基-7-甲氧基香豆素、3-苯甲酰基-5,7-二(丙氧基)香豆素、3-苯甲酰基-6,8-二氯香豆素、3-苯甲酰基-6-氯香豆素、及其混合物。
光引发剂的其它具体例子包括:苯乙酮、苯乙酮苯偶酰缩酮、2,2-二甲氧基-2-苯基苯乙酮、呫吨酮、茐酮、蒽醌、3-甲基苯乙酮、米氏酮、苯偶姻丙醚、苯偶姻乙醚、苯偶酰二甲基缩酮、以及它们的混合物。
优选的光引发剂是:酰基氧化膦、α-羟基酮、α-氨基酮、酮砜、二苯甲酮、双功能光引发剂、及它们的混合物,例如,意大利的Lamberti股份公司出售的Esacure 1001M、Esacure ONE、Esacure KIP 160和Esacure TZT。
本发明的可光固化组合物还可以包含0.05~12wt%、优选0.1~10wt%的至少一种光敏剂,作为其它添加剂。
在本文中,对于光敏剂,我们是指是在光引发剂自身无反应活性的波长下,通过能量转移过程使光引发剂活化的一种化合物。也可以单独使用这些化合物中的一部分作为光引发剂。
光敏剂的例子是本领域中常规使用的那些光敏剂:芳族羰基化合物、例如噻吨酮、蒽醌、香豆素和3-酰基香豆素衍生物、三联苯、苯乙烯酮、以及樟脑醌,并且还有曙红染料、若丹明染料和赤藓红染料。
香豆素衍生物的例子可包括:4-甲基-7-二甲基氨基香豆素、4-甲基-7-乙基氨基香豆素、4-甲基哌啶基[3.2-g]香豆素、4-甲基-7-环己基氨基香豆素、4-三氟甲基-7-二乙基氨基香豆素、3-苯基-4-甲基-7-二乙基氨基香豆素、3-(2'-N-甲基苯并咪唑基)-7-二乙基氨基香豆素、4-三氟甲基-6-甲基-7-乙基氨基香豆素、3-苯基-7-氨基香豆素、以及它们的混合物。
适合用作光敏剂的3-酰基香豆素衍生物和噻吨酮的例子是上述提及的那些。
在本发明的可光固化组合物也可方便地包括共引发剂,其是用作氢供体以增加聚合速率的分子。所述共引发剂是本领域已知的,并且通常是醇、硫醇、胺或醚,它们具有与杂原子相邻的碳成键的可用氢。在可光固化组合物中,基于可光固化组合物总重量,该共引发剂存在的量通常为0.2至12wt%,优选为0.2至8wt%。合适的共引发剂包括但不限于:脂族胺、脂环族胺、芳族胺、芳-脂胺、杂环胺、低聚胺或者聚合胺。它们可以是伯胺、仲胺或者叔胺,例如,丁基胺、二丁基胺、三丁基胺、环己胺、苄基二甲基胺、二环己胺、N-苯基甘氨酸、三乙胺、苯基-二乙醇胺、三乙醇胺、哌啶、哌嗪、吗啉、吡啶、喹啉、二甲基氨基苯甲酸的酯、米氏酮(4,4'-双-二甲基氨基二苯甲酮)、以及对应的衍生物。
作为胺共引发剂,可以使用胺改性丙烯酸酯化合物,该胺改性丙烯酸酯的例子包括:通过用US 3,844,916、EP 280222、US 5,482,649或US 5,734,002所述伯胺或仲胺的反应改性的丙烯酸酯。
优选的共引发剂是Lamberti股份公司出售的Esacure A198(双-N,N-[4-二甲基氨基苯甲酰基)氧基乙烯基-1-基]-甲基胺)和Esacure EDB(乙基-4-二甲基氨基苯甲酸酯)、2-乙基己基-4-二甲基氨基苯甲酸酯、以及N-苯基甘氨酸。
除了如上所述的化合物以外,可以向本发明的可光固化组合物加入本领域常用且本领域技术人员已知的其它组分。例如,通常使用的热稳定剂、光氧化稳定剂、抗氧化剂、溶剂、分散剂、粘合促进剂、以及其它添加剂。本发明的可光固化组合物的其它组分可以是粉末状无机填料,其能够增加3D膜的硬度。该组分、例如氧化铝、二氧化硅或氧化钛是硬涂层行业中众所周知的。
本发明的可光固化组合物可以通过在室温下、或者如果存在需要溶解的固态化合物则在光加热下,简单混合如上所述各种组分。
本发明的可光固化组合物在50rpm和40℃下测定的 RVT粘度为20~2000mPa*s,优选30-500mPa*s,更优选40~200mPa*s。
本发明的可光固化组合物可以涂敷在任何类型的基础模头上。其可以适用于插入模具的任何形状和尺寸,并且可以用通常用于砖成型使用的任何材料制成,诸如金属、例如钢,或具有玻璃纤维、碳纤维和Kevlar的复合材料。优选基础模头材料是金属,更优选钢。
使用能够在模头表面上获得三维纹理的技术,诸如光刻、喷雾印刷、喷墨印刷、以及立体光刻(stereo-litography),将本发明的可光固化组合物涂敷到基础模头上。可光固化组合物的涂敷可以在不同步骤中进行,各自随后对所涂敷组合物进行光固化。优选,本发明的可光固化组合物通过喷墨印刷涂敷。
在涂敷前,基础模头可以经受一些处理,例如,其可以磨光、或者将一层底漆涂敷在其表面上。这些预处理可以增加3D膜的粘性和性能。
根据本发明的光固化工艺通过将带有所述可光固化组合物的基础模头表面曝露于波长200~600nm的光进行。因此,可以使用大量各种光源。点光源和平面辐射源(灯带)都是合适的。例子是:炭弧光灯、氙弧光灯、中压汞弧光辐射源、高压汞弧光辐射源和低压汞弧光辐射源、(在适当情况下掺杂金属卤化物)的灯(金属卤化物灯)、微波激发金属蒸气灯、准分子灯、超光化荧光灯管、荧光灯、氩气白炽灯、闪光灯、摄影泛光灯、发光二极管(LED)、电子束、X-射线和激光。取决于可光固化组合物层的厚度和/或光引发剂的类型和用量,酌情选择活化能射线的辐射能量。优选光源包括任意种类的汞弧光辐射源和LED灯。
本发明的组合物可用于制造在任何种类成型工艺中使用的模具用模头,用于生产具有3D纹理的砖,所述工艺例如非连续工艺或连续工艺、干或半干工艺等。此处所公开的可光固化组合物特别适用于制造用于连续成型工艺的模具用模头。
仅出于说明的目的而非限制性的,根据本发明制造可光固化组合物的例子在以下段落中进行描述。
实施例
实施例1~8
用于制造可光固化组合物的烯键式不饱和化合物(单体或低聚物)、光引发剂和共引发剂如表1中所述。
表1
将光引发剂和共引发剂溶解于烯键式不饱和化合物的混合物中,制造实施例1~8的可光固化组合物。各成分以wt%计的量如表2中所示。
使用电刮棒涂布机,以200g/m2的量将各可光固化组合物涂敷到钢板上。使用装备有中压汞灯的Fusion UV系统,在空气中以10m/min的速度对膜进行固化。灯功率设为160W/cm。
表2
表2还显示了根据标准方法ISO1522:2006(摆),在40℃和50rpm测定的实施例1~8的组合物的RVT粘度(mPa*s)和弹性硬度(秒)。
3D模头的制造
使用实施例1~8的组合物,评估本发明可光固化组合物用于制造具有3D纹理的模头的适用性。由使用将200W/cm的Hg灯连接到印刷机头进行改装的数字印刷机(ChromojetLM15-HSV400),将所述组合物涂敷到钢板上。这能够立刻固化所涂敷的组合物。
软件设定为具有类似天然石头的多层涂敷。各层具有20微米的厚度,并且在涂敷结束时,具有3D纹理的膜的最厚区域为约600微米深。
最终的膜显示出对于基质非常良好的粘附性、以及不存在污迹的良好精细度、良好的硬度和低粘性。这些特性使得它们特别适用于砖的成型。
Claims (10)
1.一种用于制造具有3D纹理的砖的方法,所述方法包括用装备有模头的模具对所述砖进行成型的步骤,所述模头由包括以下步骤的方法制造:
a)提供含有如下的可光固化组合物:
a)70-99wt%的至少一种烯键式不饱和化合物;
b)1-12wt%的至少一种光引发剂;
II)将所述可光固化组合物涂敷到基础模头表面上,以形成具有三维图案的膜;
III)通过将基础模头表面曝露于波长200~600nm的光,对所述可光固化组合物进行光固化;
前提是,当所述膜是通过在钢板上对200g/m2的所述可光固化组合物进行光固化而获得的情况下,其根据标准方法ISO1522:2006确定的弹性硬度为50~300秒。
2.如权利要求1所述的方法,其特征在于,所述可光固化组合物生产弹性硬度为80~250秒的膜。
3.如权利要求1所述的方法,其特征在于,所述可光固化组合物包含:
a)75-95wt%的至少一种烯键式不饱和化合物;
b)3-10wt%的至少一种光引发剂。
4.如权利要求1所述的方法,其特征在于,基于组分a)的总重量,组分a)由如下组成:0~40wt%的具有一个烯键式不饱和基团的烯键式不饱和化合物、0~60wt%的具有两个烯键式不饱和基团的烯键式不饱和化合物、0~70wt%的具有三个烯键式不饱和基团的烯键式不饱和化合物、以及0~70wt%的具有四个或更多个烯键式不饱和基团的烯键式不饱和化合物。
5.如权利要求4所述的方法,其特征在于,基于组分a)的总重量,组分a)由如下组成:0~20wt%的具有一个烯键式不饱和基团的烯键式不饱和化合物、0~55wt%的具有两个烯键式不饱和基团的烯键式不饱和化合物、0~60wt%的具有三个烯键式不饱和基团的烯键式不饱和化合物、以及0~60wt%的具有四个或更多个烯键式不饱和基团的烯键式不饱和化合物。
6.如权利要求5所述的方法,其特征在于,基于组分a)的总重量,组分a)由如下组成:10~50wt%的具有两个烯键式不饱和基团的烯键式不饱和化合物、10~60wt%的具有三个烯键式不饱和基团的烯键式不饱和化合物、以及0~60wt%的具有四个或更多个烯键式不饱和基团的烯键式不饱和化合物。
7.如权利要求1所述的方法,其特征在于,所述至少一种烯键式不饱和化合物选自每分子具有一个或更多个烯键式不饱和基团的(甲基)丙烯酸酯化合物。
8.如权利要求1所述的方法,其特征在于,至少一种光引发剂选自如下:酰基氧化膦、3-酰基香豆素衍生物、芳香族鎓盐化合物、有机过氧化物、噻吨酮类、六芳基双咪唑、O-酰基肟酯、硼酸盐/酯化合物、嗪鎓化合物、茂金属化合物、二苯甲酮类、α-二酮、酮砜、α-氨基酮、苯偶姻和苯偶姻醚、苯偶酰缩酮、α-羟基酮、双功能光引发剂、以及它们的混合物。
9.如权利要求8所述的方法,其特征在于,所述至少一种光引发剂选自酰基氧化膦、α-羟基酮、α-氨基酮、酮砜、二苯甲酮类、双功能光引发剂、以及它们的混合物。
10.如权利要求1所述的方法,其特征在于,所述可光固化组合物进一步包含0.2~12wt%的至少一种共引发剂。
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CN101770163A (zh) * | 2008-12-27 | 2010-07-07 | 鸿富锦精密工业(深圳)有限公司 | 模仁的制造方法 |
CN202344654U (zh) * | 2011-10-29 | 2012-07-25 | 佛山市新鹏陶瓷机械有限公司 | 一种数码喷绘的陶瓷砖成型模芯压胶母模 |
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US10471633B2 (en) | 2019-11-12 |
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EP3215339A1 (en) | 2017-09-13 |
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US20170334098A1 (en) | 2017-11-23 |
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