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CN1297612C - Method for dispersion of inorganic pigment with high-temperature stability in oily medium - Google Patents

Method for dispersion of inorganic pigment with high-temperature stability in oily medium Download PDF

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CN1297612C
CN1297612C CNB2005100265910A CN200510026591A CN1297612C CN 1297612 C CN1297612 C CN 1297612C CN B2005100265910 A CNB2005100265910 A CN B2005100265910A CN 200510026591 A CN200510026591 A CN 200510026591A CN 1297612 C CN1297612 C CN 1297612C
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surface treatment
treatment agent
temperature stability
water
slurry materials
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CN1699480A (en
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陈爱英
顾剑锋
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Shanghai Jiao Tong University
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Abstract

The present invention relates to a method for dispersing inorganic pigment with high-temperature stability in an oiliness medium, which belongs to the technical field of surface treatment. Slurry materials are washed by water for 1 to 3 times so as to remove saline matters, and the slurry materials are dispersed in water for 5 to 20 minutes, wherein the temperature is raised by 40 to 90 DEG C, and the pH value is adjusted from 5 to 9; subsequently, a surface treating agent is added, and the pH is adjusted to 6 to 7 after the slurry materials are emulsified for 10 to 30 minutes at high speed; finally, the slurry materials are cooled, placed statically, filtered, washed, dried and crushed to obtain a finished product. Alternatively, the slurry materials are washed by the water for 1 to 3 times, excess electrolyte is removed, the slurry materials are dispersed in water for 5 to 20 minutes, wherein the temperature is raised by 40 to 90 DEG C, and the pH value is adjusted from 6 to 7; subsequently, the surface treating agent is added, and the slurry materials are placed statically, cooled and filtered after being emulsified for 10 to 30 minutes at high speed; finally, 0.2 to 8% of fog drops of the surface treating agent is added to the slurry materials in the processes of drying and crushing, and then the finished product is obtained by drying and crushing the slurry materials. The method improves the performance of sulfuration resistance, UV resistance and high-temperature resistance of the pigment, and particularly improves the performance of oil solubility and uniform stability of the pigment in the usage process. Thus, the method is applicable to the application fields of high-grade coatings, plastics, etc.

Description

具有高温稳定性的无机颜料在油性介质中的分散方法Dispersion method of inorganic pigment with high temperature stability in oily medium

技术领域technical field

本发明涉及一种颜料在油性介质中的分散方法,具体是一种具有高温稳定性的无机颜料在油性介质中的分散方法。属于表面处理技术领域。The invention relates to a method for dispersing a pigment in an oily medium, in particular to a method for dispersing an inorganic pigment with high temperature stability in an oily medium. It belongs to the technical field of surface treatment.

背景技术Background technique

无机颜料具有色泽鲜艳、遮盖力强等特点,被广泛应用于油漆、油墨、塑料等行业中。颜料在介质中的有效用量及均匀、一致性直接影响其色彩、透明、亮度、热稳定等性能。随着油漆,油墨、塑料等行业的生产工艺的优化和应用品质的高要求,对颜料的性能要求标准尤其是分散性和互溶稳定性越来越高。由于无机颜料表面的亲水性强,使其在油漆,油墨、塑料、涂料等油性介质中的互溶性下降,由此在使用过程中获得良好的分散性是困难的,并且稳定性不好,大大限制了其使用期限和使用范围,尤其限制了颜料在户外的使用。Inorganic pigments have the characteristics of bright color and strong hiding power, and are widely used in paint, ink, plastic and other industries. The effective dosage, uniformity and consistency of the pigment in the medium directly affect its color, transparency, brightness, thermal stability and other properties. With the optimization of the production process of paint, ink, plastics and other industries and the high requirements of application quality, the performance requirements of pigments, especially the dispersion and mutual solubility stability, are getting higher and higher. Due to the strong hydrophilicity of the surface of inorganic pigments, the miscibility in oily media such as paints, inks, plastics, and coatings decreases, so it is difficult to obtain good dispersion during use, and the stability is not good. It greatly limits its service life and scope of use, especially limits the use of pigments outdoors.

经对现有技术的文献检索发现,中国专利公开号为CN1171419A的专利,该专利公开了为提高铬系颜料耐酸碱、耐热、耐硫化等性能而进行的无机氧化物包膜处理方法,其工艺为:在颜料浆料中加入铝、硼、锰、钛、锑化合物作为表面处理剂,约占总量的3-12%,以硅化合物及水合金属氧化物及强酸作为包膜助剂,用量为12-28%,温度在85℃以上,压力在20-80Mpa,pH在9-13的条件下,在高能、高压装置内进行包膜处理1-10h。但采用此工艺处理的颜料吸油量较大,互溶性较差。After searching the literature of the prior art, it is found that the Chinese patent publication number is CN1171419A, which discloses an inorganic oxide coating treatment method for improving the properties of chromium pigments such as acid and alkali resistance, heat resistance, and vulcanization resistance. The process is: add aluminum, boron, manganese, titanium, antimony compounds to the pigment slurry as surface treatment agents, accounting for about 3-12% of the total, and use silicon compounds, hydrated metal oxides and strong acids as coating aids , the dosage is 12-28%, the temperature is above 85°C, the pressure is 20-80Mpa, and the pH is 9-13, and the coating treatment is carried out in a high-energy, high-pressure device for 1-10h. However, the pigments treated with this process have a large oil absorption capacity and poor mutual solubility.

发明内容Contents of the invention

本发明针对现有技术的不足和缺陷,提供一种具有高温稳定性的无机颜料在油性介质中的分散方法,使其提高了颜料的耐硫化、耐UV、耐高热性能,尤其提高了颜料在使用过程的油溶性和均匀稳定性,适用于中高档涂料、塑料等应用领域。Aiming at the deficiencies and defects of the prior art, the present invention provides a method for dispersing an inorganic pigment with high temperature stability in an oily medium, which improves the vulcanization resistance, UV resistance, and high heat resistance of the pigment, especially improves the pigment's Oil solubility and uniform stability during use, suitable for medium and high-grade coatings, plastics and other application fields.

本发明是通过以下技术方案实现的,包括两种方法,具体如下:The present invention is achieved through the following technical solutions, including two methods, specifically as follows:

湿法:浆料物料水洗1-3次,去除盐分,物料与水配比为1∶1-10,水中分散5-20min,升温40-90℃,pH值5-9,加入表面处理剂,表面处理剂用量为0.2-10%,高速乳化10-30min后,调节pH至6-7,降温静置、过滤、洗涤、干燥、粉碎即得成品。Wet method: the slurry material is washed 1-3 times with water to remove salt, the ratio of material to water is 1:1-10, dispersed in water for 5-20min, the temperature is raised to 40-90°C, the pH value is 5-9, and the surface treatment agent is added. The dosage of the surface treatment agent is 0.2-10%. After high-speed emulsification for 10-30 minutes, adjust the pH to 6-7, cool down and let stand, filter, wash, dry and pulverize to obtain the finished product.

混合法:浆料物料水洗1-3次,去除过量电解质,物料与水配比为1∶1-10,水中分散5-20min,升温40-90℃,pH值约6-7,加入表面处理剂,表面处理剂用量为0.2-8%,高速乳化10-30min后,降温静置、过滤,在烘干粉碎过程中吹入表面处理剂雾滴0.2-8%,或在研磨粉碎工序中加入表面处理剂0.2-8%,研磨20-120min,干燥、粉碎得成品。Mixing method: the slurry material is washed 1-3 times with water to remove excess electrolyte, the ratio of material to water is 1:1-10, dispersed in water for 5-20min, the temperature is raised to 40-90°C, the pH value is about 6-7, and surface treatment is added The amount of surface treatment agent is 0.2-8%. After high-speed emulsification for 10-30 minutes, cool down and stand still, filter, and blow in 0.2-8% of surface treatment agent droplets during the drying and crushing process, or add in the grinding and crushing process Surface treatment agent 0.2-8%, grind for 20-120min, dry and pulverize to get the finished product.

所述的表面处理剂,包括多种非离子表面活性剂和阴离子表面活性剂,如聚醚、酯醚、磷酸酯醚,硫酸酯醚、多元醇酯、改性硅油等,分子量为200-20000。表面处理剂的使用可依据不同产品的需要,选择其中一种或多种组合,比例不限。The surface treatment agent includes a variety of nonionic surfactants and anionic surfactants, such as polyethers, ester ethers, phosphate ethers, sulfate ethers, polyol esters, modified silicone oils, etc., with a molecular weight of 200-20000 . The use of surface treatment agents can be selected according to the needs of different products, and one or more combinations can be selected, and the ratio is not limited.

本发明的生产过程包括配料、乳化包膜、过滤、洗涤、烘干、粉碎、包装等常规工艺,创新点在于颜料表面高能乳化包膜工艺是颜料浆体在温度40-90℃范围内,pH值5-9,加入表面处理剂,高速乳化10-30min后,在颜料表面形成致密的有机包覆膜,以改变颜料表面的亲水疏油平衡状况。The production process of the present invention includes conventional processes such as batching, emulsification coating, filtration, washing, drying, crushing, and packaging. If the value is 5-9, add a surface treatment agent and emulsify at a high speed for 10-30 minutes to form a dense organic coating film on the surface of the pigment to change the balance of hydrophilic and oleophobic on the surface of the pigment.

本发明方法直接以无机颜料如铅铬黄为原料,采用多种混合表面处理剂,工艺简单经济,处理后的铅铬黄颜料的各项指标都达到较高的数值,铅铬黄颜料处理前后主要技术指标对比如下表:   样品  颜色(与标准样比)   吸油量(g/100g)   热稳定性(180℃烘30min)   互溶性(清漆介质)   分散性(清漆介质)   处理前  近似   22-34   变色   两天分层   差,不均匀   处理后  标准   12-18   稍变色或基本不变色   三个月未见分层   良好 The method of the present invention directly uses inorganic pigments such as lead chrome yellow as raw materials, adopts multiple mixed surface treatment agents, the process is simple and economical, and the indicators of the processed lead chrome yellow pigment all reach higher numerical values. The main technical indicators are compared in the following table: sample Color (compared with standard sample) Oil absorption (g/100g) Thermal stability (baking at 180°C for 30min) Miscibility (varnish medium) Dispersion (varnish medium) before processing approximate 22-34 discoloration two day stratification poor, uneven after treatment standard 12-18 Little or no color change Three months without delamination good

本发明依据颜料表面和使用介质的极性大小选择不同亲水亲油平衡值(HLB)的表面处理剂种类和分子量,经高能乳化包膜处理后,形成致密的表面包覆膜,制得色泽鲜艳,遮盖力好,着色力强,热稳定性高的颜料,大大提高了颜料在油性介质中的互溶性和稳定性。工艺简单,操作方便,不需新添加设备,经济环保,拓宽了应用领域,尤其适用于汽车用等中高档涂料的使用,有良好的市场需求和应用前景。According to the polarity of the pigment surface and the medium used, the present invention selects the types and molecular weights of surface treatment agents with different hydrophilic-lipophilic balance values (HLB), and forms a dense surface coating film after high-energy emulsification coating treatment to obtain color and luster. Vibrant, good hiding power, strong tinting power and high thermal stability pigments, which greatly improves the mutual solubility and stability of pigments in oily medium. The process is simple, the operation is convenient, no new equipment is needed, it is economical and environmentally friendly, and it broadens the application field. It is especially suitable for the use of medium and high-grade coatings for automobiles, and has good market demand and application prospects.

具体实施方式Detailed ways

结合本发明的内容提供以下实施例:Provide following embodiment in conjunction with content of the present invention:

实施例1Example 1

在搅拌条件下,将1000Kg铬红颜料(铬红或半成品浆料1000Kg)投于反应釜中,水洗3次,高速搅拌20nin,配料比1∶10,升温85±5℃,pH值约9,加入聚醚(分子量约16000-20000)表面活性剂100Kg,高速乳化30min后,降温静置、过滤、洗涤、干燥、粉碎即得成品。制得的铬红颜料色泽鲜艳、在油墨中分散效果良好。Under the condition of stirring, put 1000Kg of chrome red pigment (1000Kg of chrome red or semi-finished slurry) into the reaction kettle, wash 3 times with water, stir at high speed for 20nin, the proportioning ratio is 1:10, the temperature rises to 85±5°C, and the pH value is about 9. Add 100Kg of polyether (molecular weight about 16000-20000) surfactant, emulsify at high speed for 30 minutes, cool down and let stand, filter, wash, dry and pulverize to get the finished product. The prepared chrome red pigment has bright color and good dispersion effect in ink.

实施例2Example 2

在搅拌条件下,将1000Kg铬红颜料(铬红或半成品浆料1000Kg)投于反应釜中,水洗1次,高速搅拌5min,配料比1∶1,升温45±5℃,pH值约5,加入聚醚/酯醚/硫酸酯醚表面活性剂(分子量200-800间)2Kg,高速乳化10min后,降温静置、过滤、洗涤、干燥、粉碎即得成品。制得的铬红颜料在涂料中的耐光性、分散性好。Under the condition of stirring, put 1000Kg of chrome red pigment (1000Kg of chrome red or semi-finished slurry) into the reaction kettle, wash once with water, stir at high speed for 5min, the ratio of ingredients is 1:1, the temperature rises to 45±5°C, and the pH value is about 5. Add 2Kg of polyether/ester ether/sulfate ether surfactant (molecular weight between 200-800), high-speed emulsification for 10 minutes, cool down and let stand, filter, wash, dry, and pulverize to obtain the finished product. The prepared chrome red pigment has good light fastness and dispersibility in paint.

实施例3Example 3

在搅拌条件下,将1000Kg铬红颜料(铬红或半成品浆料1000Kg)投于反应釜中,水洗2次,高速搅拌10min,配料比1∶5,升温65±5℃,pH值约7,加入聚醚/硫酸酯醚表面活性剂(分子量约8000-12000)50Kg,高速乳化20min后,降温静置、过滤、洗涤、干燥、粉碎即得成品。制得的铬红颜料色泽鲜艳、颗粒疏松,在油墨中分散效果良好。Under the condition of stirring, put 1000Kg of chrome red pigment (1000Kg of chrome red or semi-finished slurry) into the reaction kettle, wash it twice with water, stir at high speed for 10min, the proportion of ingredients is 1:5, the temperature rises to 65±5°C, and the pH value is about 7. Add 50Kg of polyether/sulfate ether surfactant (molecular weight about 8000-12000), emulsify at high speed for 20 minutes, cool down and let stand, filter, wash, dry and pulverize to get the finished product. The prepared chrome red pigment has bright color, loose particles and good dispersion effect in ink.

实施例4Example 4

在搅拌条件下,将1000Kg铅铬黄包膜颜料(或铅铬黄包膜半成品浆料1000Kg)投于反应釜中,水洗1次,高速搅拌5min,配料比1∶1,升温45±5℃,pH值约5,加入改性硅油表面活性剂(分子量约200-400)2Kg,高速乳化10min后,降温静置、过滤、洗涤、干燥、吹入聚醚/改性硅油非离子表面活性剂(分子量约200-400)雾滴2Kg,继续干燥,粉碎后得成品。制得的铬红颜料色泽鲜艳、热稳定性良好,在塑料中分散效果良好。Under the condition of stirring, put 1000Kg of lead chrome yellow coating pigment (or 1000Kg of lead chrome yellow coating semi-finished product slurry) into the reaction kettle, wash once with water, stir at high speed for 5min, the proportion of ingredients is 1:1, and the temperature rises to 45±5℃ , the pH value is about 5, add 2Kg of modified silicone oil surfactant (molecular weight about 200-400), emulsify at high speed for 10 minutes, let it cool down, filter, wash, dry, and blow in polyether/modified silicone oil nonionic surfactant (Molecular weight about 200-400) mist drop 2Kg, continue to dry, and get the finished product after crushing. The prepared chrome red pigment has bright color, good thermal stability and good dispersion effect in plastics.

实施例5Example 5

在搅拌条件下,将1000Kg铅铬黄包膜颜料(或铅铬黄包膜半成品浆料1000Kg)投于反应釜中,水洗3次,高速搅拌20min,配料比1∶10,升温85±5℃,pH值约9,加入聚醚/酯醚/硫酸酯醚表面活性剂(分子量约16000-20000)80Kg,高速乳化30min后,降温静置、过滤、洗涤、预干燥,粉碎研磨过程中加入多元醇酯/改性硅油非离子表面活性剂(分子量约16000-20000)80Kg,研磨120min,干燥、粉碎得成品。制得的铅铬黄颜料色泽鲜艳、热稳定性良好,在涂料中分散效果良好。Under the condition of stirring, put 1000Kg of lead chrome yellow coated pigment (or 1000Kg of lead chrome yellow coated semi-finished product slurry) into the reaction kettle, wash 3 times with water, stir at high speed for 20min, the ratio of ingredients is 1:10, and the temperature rises to 85±5℃ , pH value is about 9, add polyether/ester ether/sulfate ether surfactant (molecular weight about 16000-20000) 80Kg, after high-speed emulsification for 30min, cool down and stand, filter, wash, pre-dry, add multi-component Alcohol ester/modified silicone oil nonionic surfactant (molecular weight about 16000-20000) 80Kg, grind for 120min, dry and pulverize to get the finished product. The prepared lead chrome yellow pigment has bright color, good thermal stability and good dispersion effect in paint.

实施例6Example 6

在搅拌条件下,将1000Kg铅铬黄包膜颜料(或铅铬黄包膜半成品浆料1000Kg)投于反应釜中,水洗2次,高速搅拌10min,配料比1∶5,升温65±5℃,pH值约7,加入聚醚/酯醚/硫酸酯醚表面活性剂(分子量约8000-12000)40Kg,高速乳化30min后,降温静置、过滤、洗涤、预干燥,粉碎研磨过程中加入多元醇酯/改性硅油非离子表面活性剂(分子量约8000-12000)40Kg,研磨70min,干燥、粉碎得成品。制得的铅铬黄颜料色泽鲜艳、热稳定性良好,在涂料中分散效果良好。Under the condition of stirring, put 1000Kg of lead chrome yellow coated pigment (or 1000Kg of lead chrome yellow coated semi-finished product slurry) into the reaction kettle, wash twice with water, stir at high speed for 10min, the proportion of ingredients is 1:5, and the temperature rises to 65±5℃ , the pH value is about 7, add polyether/ester ether/sulfate ether surfactant (molecular weight about 8000-12000) 40Kg, emulsify at high speed for 30min, cool down and stand, filter, wash, pre-dry, add multi-component Alcohol ester/modified silicone oil nonionic surfactant (molecular weight about 8000-12000) 40Kg, grind for 70min, dry and pulverize to obtain the finished product. The prepared lead chrome yellow pigment has bright color, good thermal stability and good dispersion effect in paint.

Claims (8)

1, a kind of dispersing method of mineral dye in oil medium with high-temperature stability, it is characterized in that salinity is removed in slurry material washing 1-3 time, disperse 5-20min in the water, intensification 40-90 ℃, pH value 5-9 adds surface treatment agent, the surface treatment agent consumption is 0.2-10%, behind the emulsify at a high speed 10-30min, regulate pH to 6-7, cooling leaves standstill, filters, washs, dry, pulverize and get product.
2, the dispersing method of mineral dye in oil medium with high-temperature stability according to claim 1 is characterized in that, described slurry material washing, and material and water proportioning are 1: 1-10.
3, the dispersing method of mineral dye in oil medium with high-temperature stability according to claim 1, it is characterized in that, described surface treatment agent, for: polyethers, ester ether, phosphoric acid ester ether, one or more combinations in sulfuric ester ether, polyol ester, the modified silicon oil.
4, according to claim 1 or the 3 described dispersing method of mineral dye in oil medium, it is characterized in that described surface treatment agent, molecular weight are 200-20000 with high-temperature stability.
5, a kind of dispersing method of mineral dye in oil medium with high-temperature stability, it is characterized in that, slurry material washing 1-3 time, remove excessive ionogen, disperse 5-20min in the water, intensification 40-90 ℃, pH value 6-7 adds surface treatment agent, and the surface treatment agent consumption is 0.2-8%, behind the emulsify at a high speed 10-30min, cooling is left standstill, is filtered, and is blown into surface treatment agent droplet 0.2-8% in the oven dry crushing process, or adds surface treatment agent 0.2-8% in grinding operation, grind 20-120min, dry, pulverize finished product.
6, the dispersing method of mineral dye in oil medium with high-temperature stability according to claim 5 is characterized in that, described slurry material washing, and material and water proportioning are 1: 1-10.
7, the dispersing method of mineral dye in oil medium with high-temperature stability according to claim 5, it is characterized in that, described surface treatment agent, for: polyethers, ester ether, phosphoric acid ester ether, one or more combinations in sulfuric ester ether, polyol ester, the modified silicon oil.
8, according to claim 5 or the 7 described dispersing method of mineral dye in oil medium, it is characterized in that described surface treatment agent, molecular weight are 200-20000 with high-temperature stability.
CNB2005100265910A 2005-06-09 2005-06-09 Method for dispersion of inorganic pigment with high-temperature stability in oily medium Expired - Fee Related CN1297612C (en)

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US5451254A (en) * 1991-09-18 1995-09-19 L'oreal Fine dispersion of melanin pigments, its preparation and its use in cosmetics
CN1359987A (en) * 2001-12-28 2002-07-24 中山大学 Composite gaolinite/rare-earth/iron oxide-base nano pigment and its microwave process for synthesizing it
CN1597791A (en) * 2003-09-17 2005-03-23 宗世栋 Predispersion pigment and its preparation process

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5158606A (en) * 1991-03-06 1992-10-27 Sun Chemical Corporation Low rub printing ink
US5451254A (en) * 1991-09-18 1995-09-19 L'oreal Fine dispersion of melanin pigments, its preparation and its use in cosmetics
CN1359987A (en) * 2001-12-28 2002-07-24 中山大学 Composite gaolinite/rare-earth/iron oxide-base nano pigment and its microwave process for synthesizing it
CN1597791A (en) * 2003-09-17 2005-03-23 宗世栋 Predispersion pigment and its preparation process

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