CN114958030A - 一种用于聚酯着色的超细颜料制备物的制备方法 - Google Patents
一种用于聚酯着色的超细颜料制备物的制备方法 Download PDFInfo
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- CN114958030A CN114958030A CN202210756780.7A CN202210756780A CN114958030A CN 114958030 A CN114958030 A CN 114958030A CN 202210756780 A CN202210756780 A CN 202210756780A CN 114958030 A CN114958030 A CN 114958030A
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- Prior art keywords
- pigment
- preparation
- polyester
- resin
- ball mill
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 28
- 229920005989 resin Polymers 0.000 claims abstract description 25
- 239000011347 resin Substances 0.000 claims abstract description 25
- 239000002245 particle Substances 0.000 claims abstract description 24
- 238000000227 grinding Methods 0.000 claims abstract description 18
- 229920001225 polyester resin Polymers 0.000 claims abstract description 18
- 239000004645 polyester resin Substances 0.000 claims abstract description 18
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- JRZJOMJEPLMPRA-UHFFFAOYSA-N olefin Natural products CCCCCCCC=C JRZJOMJEPLMPRA-UHFFFAOYSA-N 0.000 claims description 4
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- MYONAGGJKCJOBT-UHFFFAOYSA-N benzimidazol-2-one Chemical compound C1=CC=CC2=NC(=O)N=C21 MYONAGGJKCJOBT-UHFFFAOYSA-N 0.000 claims description 3
- 229910052797 bismuth Inorganic materials 0.000 claims description 3
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- 229910052759 nickel Inorganic materials 0.000 claims description 3
- DGBWPZSGHAXYGK-UHFFFAOYSA-N perinone Chemical compound C12=NC3=CC=CC=C3N2C(=O)C2=CC=C3C4=C2C1=CC=C4C(=O)N1C2=CC=CC=C2N=C13 DGBWPZSGHAXYGK-UHFFFAOYSA-N 0.000 claims description 3
- 125000002080 perylenyl group Chemical group C1(=CC=C2C=CC=C3C4=CC=CC5=CC=CC(C1=C23)=C45)* 0.000 claims description 3
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- 125000003367 polycyclic group Chemical group 0.000 claims description 3
- FYNROBRQIVCIQF-UHFFFAOYSA-N pyrrolo[3,2-b]pyrrole-5,6-dione Chemical compound C1=CN=C2C(=O)C(=O)N=C21 FYNROBRQIVCIQF-UHFFFAOYSA-N 0.000 claims description 3
- IZMJMCDDWKSTTK-UHFFFAOYSA-N quinoline yellow Chemical compound C1=CC=CC2=NC(C3C(C4=CC=CC=C4C3=O)=O)=CC=C21 IZMJMCDDWKSTTK-UHFFFAOYSA-N 0.000 claims description 3
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- LSGOVYNHVSXFFJ-UHFFFAOYSA-N vanadate(3-) Chemical compound [O-][V]([O-])([O-])=O LSGOVYNHVSXFFJ-UHFFFAOYSA-N 0.000 claims description 3
- 229910052984 zinc sulfide Inorganic materials 0.000 claims description 3
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09B—ORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
- C09B67/00—Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
- C09B67/0097—Dye preparations of special physical nature; Tablets, films, extrusion, microcapsules, sheets, pads, bags with dyes
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/006—Combinations of treatments provided for in groups C09C3/04 - C09C3/12
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/04—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/04—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
- C09C3/041—Grinding
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/10—Treatment with macromolecular organic compounds
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
- D01F1/02—Addition of substances to the spinning solution or to the melt
- D01F1/04—Pigments
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Abstract
本发明提供一种用于聚酯着色的超细颜料制备物的制作方法,在有夹套的搅拌球磨机中加入研磨介质,开启30r/min搅拌,将20‑70份颜料、80‑30份聚酯树脂、80‑100份水、0.3‑1份分散剂预混料加入到高能量球磨设备,加热到60‑68℃软化树脂,利用300r/min‑800r/min快速的撞击1小时研磨将颜料颗粒粉碎、包覆入软化的树脂,并在树脂中有分散3‑4小时,进一步降温到20‑25℃经过滤、50℃干燥得到用于聚酯着色的颜料制备物。本发明的聚酯超细颜料制备物特别适用于聚酯纤维或聚酯长丝的纺丝着色,用于在各种挤出、模塑、注塑、吹塑、压延和吹膜设备中加工着色。
Description
技术领域
本发明属于颜料制备物合成的技术领域,特别涉及一种用于聚酯着色的超细颜料制备物的制备。
背景技术
聚酯是由多元醇和多元酸缩聚而得的聚合物总称,具有较高的强度与弹性恢复能力,是一类性能优异、用途广泛的工程塑料。最常见的聚酯树脂是聚对苯二甲酸乙二醇 酯(PET),它是对苯二甲酸与乙二醇聚合脱水的反应产物。
聚酯经纺丝所得的合成纤维简称聚酯纤维,俗称″涤纶″,是当前合成纤维的第一大品种。聚脂纤维材料的分子结构决定了其染色困难,人们研究出了很多方法来改进其染色性能,除了常用的织物染色外,还可在纤维纺丝前对其着色,然后直接制成有色纤维。纺前着色聚酯纤维,因其具有较好的色牢度、较少的环境污染、适当的成本、优异的性能价格比等诸多良好的特性而受重视,成为重点发展的纤维品种之一。
用于聚酯纤维原液着色的有机颜料要耐高温,在聚酯树脂中呈分散状态,粒径在0.5μm左右,在聚酯树脂中有一定的浸润性,颜料分子有足够的亲酯性基团。
当今常用于聚酯的着色剂,不外乎颜料干粉,液体色母料,以及颜料制备物。颜料干粉由于其粉尘以及颗粒絮凝性,逐渐被液体色母料或颜料制备物所取代。液体色母料由颜料或染料与流动的高分子聚合物构成,藉着流动的高分子聚合物确保颜料与塑料的兼容性,促进液体色母料的均匀分散。然而液体色母料需要经过多道工序的研磨,成本较高,而且这些产品不适合用于透明塑料着色,消费者发现液体色母料有产品稳定性问题、加工问题、以及需要对计量设备进行资本投资。
色母粒着色是目前应用较多的聚酯着色生产方式。生产工艺简单、灵活,适合有色聚酯纤维的生产过程。目前,国内外有多项专利揭示了不同聚酯纤维原液纺丝用色母粒的制备和应用方法,如申请号为CN201210534384.6的中国专利揭示了一种低熔点聚酯色母粒的制备方法,该方法通过将低熔点聚酯、聚酰胺蜡、颜料等原料经双螺杆挤出机熔融共混、造粒得到一种低熔点聚酯色母粒。但使用色母粒对聚酯纤维进行着色,存在三个缺点:1)色母粒生产过程中,颜料在载体中的分散完全靠螺杆之间的机械剪切分散,因此,一方面,涤纶色母粒的生产对颜料的加工精度低,另一方面,对颜料本身的分散性存在极大的要求,限制了颜料的选择范围;2)涤纶等聚酯纤维用色母粒易吸水受潮,为避免水解,在使用时必须烘干。这样增加了设备投资、设备污染和能耗;3)色母粒制造过程中,载体树脂已经熔融了一次,色母粒和聚酯本体切片混合纺丝时又熔融了一次,经过两次熔融,不仅增加了能耗,也加剧了载体树脂的热降解和热氧化降解程度,其特性粘度会降低,势必影响其可纺性以及物理性能。
最适合的着色剂当属颜料制备物。颜料制备物制作常用的方法为挤水换相法,其中将经压滤的颜料滤饼与有机物质(油或树脂)在混合机内捏合,将颜料颗粒从水相转换到有机介质中。然后除去被置换出来的水。为了除去残留的水,尚需对制备物进一步处理,在真空下加热干燥。美国专利4036652描述了一种使用捏合机将高固含的颜料滤饼与碱溶树脂混合,在不停的剪切作用下将水分离而成,完成树脂对颜料颗粒的包覆。美国专利4,474,473则描述了一种使用同向旋转双螺杆挤出机,连续将颜料滤饼挤水换相的方法。该方法需要颜料含量为35%重量或更高固含的滤饼。美国专利4,309,223则公开了一种使用单螺杆挤出机将颜料滤饼挤水换相的方法。该方法使用极为稀释的滤饼浆液,约0.5%重量至10%重量颜料的浆料。美国专利6273599提供了使用双螺杆挤出机,将滤饼先均质化为流化物质,再连续挤水换相生产颜料制备物的方法。欧洲专利申请号 8,373A1公开了一种线性聚酯的颜料制备物,通过添加双丙酮醇溶剂与氯化钠盐捏合的方法,将20至80份颜料和80至20份在60℃和160℃之间熔化的聚酯捏合,然后与可纺线型聚酯熔融在一起,并加工制成颗粒的预浓缩物。
颜料制备物最重要的优势就是能提供最大的着色强度,颜料在制备物制作过程中已得到充分的分散,呈现分布狭窄的细小颗粒,这是颜色着色强度优越的主要原因。然而,挤水转相所得颜料制备物,由于捏合机剪切力相对较小,颜料不能在制备物载体树脂中充分分散,颜色强度得不到最优展现。随着客户对产品的着色强度,光泽度和透明度需求的不断增加,在不损害产品其它性能的需求下,市场对生产超细颜料制备物的呼声更多。
发明内容
本发明聚酯类超细颜料制备物的制备实凭借特殊设备的强度剪切与打击,将颜料颗粒包覆进入聚酯树脂,并在树脂内快速被细化,确保颜料分散的均匀性,提升颜色的透明度和着色力,主要包含以下操作:
一种用于聚酯着色的超细颜料制备物的制作方法,在有夹套的搅拌球磨机中加入研磨介质,开启30r/min搅拌,将20-70份颜料、80-30份聚酯树脂、80-100份水、0.3-1 份分散剂预混料加入到高能量球磨设备,加热到60-68℃软化树脂,利用 300r/min-800r/min快速的撞击1小时研磨将颜料颗粒粉碎、包覆入软化的树脂,并在树脂中有分散3-4小时,进一步降温到20-25℃经过滤、50℃干燥得到用于聚酯着色的颜料制备物。
所述的聚酯树脂是由芳香族和/或脂肪族二羧酸与脂肪族二醇的共聚酯或烯烃、丙烯酸酯和甲基丙烯酸酯的共聚物中的一种。
球磨设备包括但不限于卧式球磨机、超微磨碎机、高速球磨机、搅拌球磨机、振动球磨机、立式或卧式的小型介质研磨机。
研磨珠介质的密度为5~15g/cm3,介质包括以下材料:不锈钢、碳钢、铈锆氧化物、镁锆氧化物、钇锆氧化物、锆硅石以及它们的混合物。
使用的颜料是任何常规的有机或无机颜料,颜料以滤饼或粉末方式加入,颜料的添加量在整个制备物中占5%-80%。
颜料的添加量优选在整个制备物中占20%-70%;其中无机颜料优选为20-50%重量,有机颜料为40-70%重量。
使用的颜料有:偶氮类,色淀偶氮,苯并咪唑酮,二偶氮缩合,偶氮金属络合物颜料和多环颜料例如酞菁,喹吖啶酮,苝,紫环酮,蒽醌,二恶嗪,喹酞酮,异吲哚酮,异吲哚啉和二酮吡咯并吡咯颜料或炭黑。合适的无机颜料是二氧化钛、硫化锌、氧化铁、氧化铬、群青、镍或铬锑钛氧化物、钴氧化物、钴和铝的混合氧化物、钒酸铋和体质颜料。
本发明制作方法制作的超细颜料制备物适用于对聚酯短纤维和聚酯长丝进行着色。
本发明制作方法制作的制作的超细颜料制备,用于在各种挤出、模塑、注塑、吹塑、压延和吹膜设备中加工着色。
本发明的有益效果为:本发明的聚酯超细颜料制备物特别适用于聚酯纤维或聚酯长丝的纺丝着色,特别是可用于借助侧流挤出机加入聚酯纺丝熔体中,或通过将此聚酯制备物与聚酯纺丝料预先混合,然后在纺丝机中共同熔融而着色。也适用于在各种挤出、模塑、流延和吹膜物料的着色加工。
具体实施方式
下面结合具体实施例,对本发明的技术方案作进一步详细说明。
(1)将20-70份颜料、80-30份聚酯树脂及0.3-1份分散剂等在预混釜中加80-100份水30r/min预混10min,将预混液加入到高剪切、高撞击的设备中,如球磨机,高搅拌球磨机,均质机等,同时将温度加热提升到树脂的软化点60-68℃,藉由 300r/min-800r/min钢珠或锆珠的撞击研磨1小时,颜料被撞击进入微小的树脂中,通过取样检测,滤纸上无颜料颗粒渗出,表明正实现完全的包覆。
(2)将颜料粒径进一步细化,即在60-68℃的温度下,加快研磨介质的撞击,颜料在树脂环境的持续研辗下3-4小时,将颗粒分散粉碎制成超细制备物。
(3)将制作的颜料制备物过滤,然后在50℃的温度下干燥。
优选地,步骤(1)所使用的聚酯树脂,是由芳香族和/或脂肪族二羧酸与脂肪族二醇的共聚酯或烯烃、丙烯酸酯和甲基丙烯酸酯的共聚物中的一种。
聚酯树脂的选择在聚酯颜料制备物的制备中很重要。它必须能够润湿颜料或染料,同时必须能够容易分散在整个产品,在加工过程中不被加工的温度分解,且不能包含大量的水或较低的分子量酯类。其分子量约10000~30000,玻璃化转变温度在50-80℃,软化点高于60℃,熔化范围在130到150℃之间。由芳香族和/或脂肪族二羧酸与脂肪族二醇的共聚酯所使用的二元羧酸选自对苯二甲酸、间苯二甲酸、壬二酸、癸二酸和己二酸中的一种或两种;脂肪族二醇选自乙二醇、1,4-丁二醇、1,4-二(羟甲基)-环己烷和新戊二醇中的一种。由烯烃、丙烯酸酯和甲基丙烯酸酯的共聚物,选自乙烯-丙烯酸甲酯共聚物、乙烯-甲基丙烯酸甲酯共聚物、乙烯-丙烯酸乙酯共聚物、乙烯-甲基丙烯酸乙酯共聚物、乙烯-丙烯酸丁酯共聚物,乙烯-甲基丙烯酸丁酯共聚物中的一种。这些共聚物能与多种其它聚合物高度相容,可以增强工程聚合物的物理性能,例如对基材的附着力、高填料接受度、改进的加工性以及增加的冲击和韧性。
优选地,步骤(1)所使用的分散剂是褐煤酯蜡、蓖麻蜡粉末和亚乙基双硬脂酰胺(EBS)粉末中的一种。
进一步优选地,分散剂用量占总制备物的0.3-1%。
优选地,步骤(1)颜料必须有适当的耐热性与分散性,常用于聚酯用超细制备物的有机颜料包含偶氮类,色淀偶氮,苯并咪唑酮,二偶氮缩合,偶氮金属络合物颜料和多环颜料例如酞菁,喹吖啶酮,苝,紫环酮,蒽醌,二恶嗪,喹酞酮,异吲哚酮,异吲哚啉和二酮吡咯并吡咯颜料或炭黑;无机颜料包含二氧化钛、硫化锌、氧化铁、氧化铬、群青、镍或铬锑钛氧化物、钴氧化物、钴和铝的混合氧化物、钒酸铋和体质颜料。
进一步优选地,颜料的添加量在整个制备物中占20%-70%。其中,无机颜料的添加量为20-50%,有机颜料为40-70%。
优选地,步骤(3)干燥的方法包括烘箱干燥,喷雾干燥,以及流化床干燥中的一种。
实施例1
在一台装备有夹套的6L立式高速搅拌球磨机中加入16kg球形不锈钢钢球,钢球的直径为18-20mm。开启30r/min转速低速搅拌,加入1000g的水,540g的乙烯 -甲基丙烯酸乙酯共聚物(丙烯酸乙酯含量5%~20%,密度0.93g/cm3,软化点64℃), 5g的亚乙基双硬脂酰胺(EBS)分散剂,1260g的有机颜料红122。混合10分钟,加入 800g的水,加热到64℃,调整转速为500r/min,高速研磨1h。通过取样检测,滤纸上无颜料颗粒渗出。确定颜料完全进入软化的树脂,继续高速研磨3小时,降低温度到20℃。过滤,滤饼用冷水洗涤,放入烘箱50℃干燥,得到1789g含聚酯树脂的超细颜料红122制备物。
使用本发明生产的制备物很容易掺入到PET纺丝材料中,而过滤值检测压力0.83par/g,低于常规制备物2par/g的质量标准。长丝染色的匀染性同样得到改善,测色仪检测色相DE=0.11,小于0.2,可判定为无色差。
实施例2
在一台装备有夹套的6L立式高速搅拌球磨机中加入16kg球形不锈钢钢球,钢球的直径为18-20mm。开启30r/min转速低速搅拌,加入1000g的水,1080g的对苯二甲酸/间苯二甲酸和乙二醇的共聚酯,其中含有25%的间苯二甲酸的共聚物(软化点60℃),18g的褐煤酯蜡分散剂,加入720g的有机颜料红179。混合10分钟,加入600g的水,加热到60℃,调整转速为300r/min,高速研磨1h。通过取样检测,滤纸上无颜料颗粒渗出。确定颜料完全进入软化的树脂,继续高速研磨3.5小时,降低温度到20℃。过滤,滤饼用冷水洗涤,放入烘箱50℃干燥,得到1791g含聚酯树脂的超细颜料红179制备物。
使用本发明生产的制备物很容易掺入到PET纺丝材料中,而过滤值检测压力0.77par/g,低于常规制备物2par/g的质量标准。长丝染色的匀染性同样得到改善,测色仪检测色相DE=0.16,小于0.2,可判定为无色差。
实施例3
在一台装备有夹套的6L立式高速搅拌球磨机中加入16kg球形不锈钢钢球,钢球的直径为18-20mm。开启30r/min转速低速搅拌,加入1000g的水,900gEBAC SP2810(EBACSP2810是乙烯与丙烯酸丁酯共聚物,EASTMAN化学公司,软化点为67℃),5g的亚乙基双硬脂酰胺(EBS)分散剂,加入900g的有机颜料黄180。混合 10分钟,加入600g的水,加热到67℃,调整转速为800r/min,高速研磨1h。通过取样检测,滤纸上无颜料颗粒渗出。确定颜料完全进入软化的树脂,继续高速研磨3小时,降低温度到25℃。过滤,滤饼用冷水洗涤,放入烘箱50℃干燥,得到1783g含聚酯树脂的超细颜料黄180制备物。
使用本发明制备的制备物所着色的瓶子呈透明状,且无可见漩纹,过滤值检测压力 0.74par/g,低于常规制备物2par/g的质量标准。测色仪检测色相DE=0.09,小于0.2,可判定为无色差。
实施例4
在一台装备有夹套的6L立式高速搅拌球磨机中加入16kg球形不锈钢钢球,钢球的直径为18-20mm。开启30r/min转速低速搅拌,加入1000g的水,1440gEMAC SP1330(EMACSP1330是乙烯与丙烯酸甲酯共聚物,EASTMAN化学公司,软化点为68℃),10g的蓖麻蜡分散剂,加入360g的无机颜料群青。混合10分钟,加入400g 的水,加热到68℃,调整转速为800r/min,高速研磨1h。通过取样检测,滤纸上无颜料颗粒渗出。确定颜料完全进入软化的树脂,继续高速研磨4小时,降低温度到25℃。过滤,滤饼用冷水洗涤,放入烘箱50℃干燥,得到1783g含聚酯树脂的超细颜料黄180 制备物。
使用本发明制备物所着色的瓶子呈透明状,且无可见漩纹,过滤值检测压力0.69par/g,低于常规制备物2par/g的质量标准。测色仪检测色相DE=0.12,小于0.2,可判定为无色差。
实施例5
在一台装备有夹套的6L立式高速搅拌球磨机中加入16kg球形不锈钢钢球,钢球的直径为18-20mm。开启30r/min转速低速搅拌,加入1000g的水,900g的对苯二甲酸/间苯二甲酸和乙二醇的共聚酯,其中含有25%的间苯二甲酸的共聚物(软化点 60℃),18g的褐煤酯蜡分散剂,加入900g的无机颜料黑7。混合10分钟,加入600g 的水,加热到60℃,调整转速为500r/min,高速研磨1.5h。通过取样检测,滤纸上无颜料颗粒渗出。确定颜料完全进入软化的树脂,继续高速研磨3小时,降低温度23℃。过滤,滤饼用冷水洗涤,放入烘箱50℃干燥,得到1779g含聚酯树脂的超细颜料黑7 制备物。
使用本发明制备的制备物所着色的瓶子呈透明状,且无可见漩纹,过滤值检测压力 0.85par/g,低于常规制备物2par/g的质量标准。测色仪检测色相DE=0.16,小于0.2,可判定为无色差。
实施例6
在一台装备有夹套的6L立式高速搅拌球磨机中加入16kg球形不锈钢钢球,钢球的直径为18-20mm。开启30r/min转速低速搅拌,加入1000g的水,1080g的EBAC SP2810(EBACSP2810是乙烯与丙烯酸丁酯共聚物,EASTMAN化学公司,软化点为67℃),10g的蓖麻蜡分散剂,加入720g的有机颜料黑酞青蓝15-3。混合10分钟,加入800g的水,加热到67℃,调整转速为500r/min,高速研磨1h。通过取样检测,滤纸上无颜料颗粒渗出。确定颜料完全进入软化的树脂,继续高速研磨3小时,降低温度到22℃。过滤,滤饼用冷水洗涤,放入烘箱50℃干燥,得到1779g含聚酯树脂的超细颜料黑7制备物。
使用本发明制备的制备物所着色的瓶子呈透明状,且无可见漩纹,过滤值检测压力 0.85par/g,低于常规制备物2par/g的质量标准。测色仪检测色相DE=0.16,小于0.2,可判定为无色差。
以上的实施例是为了说明本发明公开的实施方案,并不能理解为对本发明的限制。此外,本文所列出的各种修改以及发明中方法、组合物的变化,在不脱离本发明的范围和精神的前提下对本领域内的技术人员来说是显而易见的。虽然已结合本发明的多种具体优选实施例对本发明进行了具体的描述,但应当理解,本发明不应仅限于这些具体实施例。事实上,各种如上所述的对本领域内的技术人员来说显而易见的修改来获取发明都应包括在本发明的范围内。
Claims (9)
1.一种用于聚酯着色的超细颜料制备物的制作方法,其特征在于,在有夹套的搅拌球磨机中加入研磨介质,开启30r/min搅拌,将20-70份颜料、80-30份聚酯树脂、80-100份水、0.3-1份分散剂预混料加入到高能量球磨设备,加热到60-68℃软化树脂,利用300r/min-800r/min快速的撞击1小时研磨将颜料颗粒粉碎、包覆入软化的树脂,并在树脂中有分散3-4小时,进一步降温到20-25℃经过滤、50℃干燥得到用于聚酯着色的颜料制备物。
2.根据权利要求1所述的制作方法,其特征在于,聚酯树脂是由芳香族和/或脂肪族二羧酸与脂肪族二醇的共聚酯或烯烃、丙烯酸酯和甲基丙烯酸酯的共聚物中的一种。
3.根据权利要求1的制作方法,其特征在于,球磨设备包括但不限于卧式球磨机、超微磨碎机、高速球磨机、搅拌球磨机、振动球磨机、立式或卧式的小型介质研磨机。
4.根据权利要求1的制作方法,其特征在于,研磨珠介质的密度为5~15g/cm3,介质包括以下材料:不锈钢、碳钢、铈锆氧化物、镁锆氧化物、钇锆氧化物、锆硅石以及它们的混合物。
5.根据权利要求1的制作方法,其特征在于,使用的颜料是任何常规的有机或无机颜料,颜料以滤饼或粉末方式加入,颜料的添加量在整个制备物中占5%-80%。
6.根据权利要求1的制作方法,其特征在于,颜料的添加量在整个制备物中占20%-70%;其中无机颜料优选为20-50%重量,有机颜料为40-70%重量。
7.根据权利要求5的制作方法,其特征在于,使用的颜料有:偶氮类,色淀偶氮,苯并咪唑酮,二偶氮缩合,偶氮金属络合物颜料和多环颜料例如酞菁,喹吖啶酮,苝,紫环酮,蒽醌,二恶嗪,喹酞酮,异吲哚酮,异吲哚啉和二酮吡咯并吡咯颜料或炭黑。合适的无机颜料是二氧化钛、硫化锌、氧化铁、氧化铬、群青、镍或铬锑钛氧化物、钴氧化物、钴和铝的混合氧化物、钒酸铋和体质颜料。
8.根据权利要求1的制作方法制作的超细颜料制备物适用于对聚酯短纤维和聚酯长丝进行着色。
9.根据权利要求1制作方法制作的制作的超细颜料制备,用于在各种挤出、模塑、注塑、吹塑、压延和吹膜设备中加工着色。
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