CN103788469A - Method for preparing pre-dispersing pigment by using ethylene-vinyl acetate copolymer wax as dehydrating agent - Google Patents

Method for preparing pre-dispersing pigment by using ethylene-vinyl acetate copolymer wax as dehydrating agent Download PDF

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Publication number
CN103788469A
CN103788469A CN201410041876.0A CN201410041876A CN103788469A CN 103788469 A CN103788469 A CN 103788469A CN 201410041876 A CN201410041876 A CN 201410041876A CN 103788469 A CN103788469 A CN 103788469A
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China
Prior art keywords
pigment
wax
eva3
kneader
filter cake
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CN201410041876.0A
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Chinese (zh)
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庞国栋
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Individual
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Individual
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Priority to CN201410041876.0A priority Critical patent/CN103788469A/en
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    • 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
    • C08K5/00Use of organic ingredients
    • C08K5/16Nitrogen-containing compounds
    • C08K5/20Carboxylic acid amides
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09BORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
    • C09B67/00Influencing 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
    • C09B67/0001Post-treatment of organic pigments or dyes
    • C09B67/0003Drying, e.g. sprax drying; Sublimation of the solvent
    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09BORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
    • C09B67/00Influencing 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
    • C09B67/006Preparation of organic pigments
    • C09B67/0063Preparation of organic pigments of organic pigments with only macromolecular substances

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Organic Chemistry (AREA)
  • Health & Medical Sciences (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Processes Of Treating Macromolecular Substances (AREA)

Abstract

The invention relates to a method for preparing a pre-dispersing pigment by using ethylene-vinyl acetate copolymer (EVA3) wax as a dehydrating agent. The method comprises the steps of adding a pigment filter cake, EVA3 wax and cocoanut oil amine when the temperature of a kneader is increased to 50-60 DEG C; starting stirring, continuously heating till the material temperature is 95-100 DEG C, and starting the vacuum dehydration of the kneader, wherein the vacuum degree is 500-600 mmHg; determining a qualified package by detecting that the water content of a material is less than or equal to 0.1%. According to the pre-dispersing pigment produced by adopting the method, the appearance is in a granule shape; because the middle process that the pigment press cake is dried and crushed and then stirred at a high speed with the EVA3 wax is omitted, the problem of pollution of pigment dry powder is thoroughly solved; the energy consumption comparison is as follows: the pigment filter cake is prepared into dry powder by being dried and crushed, one ton of pigment needs three tons of fuel coal with the cost of about 2000 yuan, and the electrical energy consumption is 300 yuan. The new method disclosed by the invention is obvious in template and bright in color and enhances the coloring power by 5%-10%.

Description

Do the method that dewatering agent is prepared pigment preparations with ethene-vinyl acetate copolymer wax
Technical field
The present invention is a kind of manufacture method of pigment preparations, is applied to and produces the painted Masterbatch of using of food product packing film.Pigment filter cake in raw material choose organic or inorganic pigment last handling process, and ethene-vinyl acetate copolymer wax (hereinafter to be referred as: EVA3 wax.) do dewatered and dispersed agent, the pigment preparations commodity that adopt water squeezing phase conversion method production technique to manufacture.
Background technology
Pigment is a kind of important industrial chemicals, is widely used in the industries such as plastics, ink, paint, coating, rubber with regard to colouring function.Commodity pigment on market is dry powder mostly, dry powder is by pigment filter cake drying, pulverizing is made, and the pigment obtaining like this has following several large defect: 1. power consumption: dry and need a large amount of fire coals, the dispersion process in pulverizing and later stage application also needs very large energy consumption.2. pollute: existing coal burning pollution, the dust pollution that has again crushing process and later stage application processing to produce.3. the degradation of pigment: in the drying process of pigment, the primary partical of pigment produces to be assembled, makes it in the production application in later stage, be difficult for disperseing, and the vividness of product and tinting strength are not up to standard.Thus, make production cost increase, the class of user's goods declines.
In order to address the above problem, colleague both domestic and external has done a large amount of research work, and that makes with regard to pigment is energy-conservation, environmental protection, and high-quality has obtained multiple solution.Wherein make pigment preparations (processed-pigment) and be considered to one of successful commodity.Method is water squeezing phase conversion method preferably, is the main method of producing pigment preparations by pigment filter cake.This pigment preparations is also the intermediate of manufacturing colour batch.The look female class that conventional dry is manufactured is lower, is further not suitable for the market requirement.Method is that pigment dry powder and resin, dispersion agent (polyethylene wax, EVA3 wax etc.) are dropped in proportion after high-speed stirring machining, then is a granulated into commodity through twin screw extruder.Wherein the function such as polyethylene wax and EVA3 wax is dispersion agent.The Masterbatch kind of different purposes is used different dispersion agents, refers to the difference of plastic material and the difference of finished product range of application here.Such as: painted common plastics industrial goods with just make a big difference aspect technical requirements for food packing composite film.
The pigment preparations that the present invention manufactures is with regard to Masterbatch this specific range of application for food packaging film, through a large amount of test and Selection repeatedly suitable feedstock and production method, that is: EVA3 wax+pigment filter cake (moisture) turns to method with water squeezing.Relatively female with the look of common dry production, although the roughly the same qualitative difference that truly having of materials.This is that wet method is different substances transmission between pigment primary partical (particle is very little) in chemical property because dry method is the different substances transmission between pigment flocculate (particle is larger) under external force.The latter has also taken into account the requirement of the physical and mechanical property of user's goods under the prerequisite that guarantees excellent tinctorial property.According to the requirement of GB (GB/T10004-2008) such as: peeling force, the indexs such as pull-off force have 13.In selecting single EVA3 wax as dewatered and dispersed agent, it is again a kind of functional material, and this is emphasis of the present invention.Its function one: the primordial condition that has guaranteed to greatest extent pigment particles is not damaged, is perfectly applicable to food packaging film, composite membrane and plastics polar material painted.Function two: can combine with the plastic material of many kinds and the physical index of good assurance filmogen.Function three: be applied in mineral dye aspect and have than better dispersion effects such as polyethylene waxs.
Summary of the invention
EVA3 wax and pigment filter cake are the pigment preparations that main raw material is manufactured, and complete (water squeezing phase conversion method) by a kind of wet processing.
Technical scheme of the present invention is as follows:
Do the method that dewatering agent is prepared pigment preparations with ethene-vinyl acetate copolymer wax, when kneader is warming up to 50 ℃-60 ℃, drop into pigment filter cake, ethylene-vinyl acetate copolymer wax and coco amine; Open and stir, persistently overheating 95 ℃-100 ℃ of the temperature of charge that make, the vacuum hydro-extraction of opening kneader, vacuum tightness is 500-600mmHg, detecting material moisture≤0.1% is qualified packing.
Solid weight in pigment filter cake: EVA3 wax=1:0.4~0.8; Coco amine is 2% of pigment solids weight.
The equipment adopting is common equipment: Z-type vacuum kneader, homogenizer, twin screw extruder, plastic injection equipment.
The pigment preparations of producing by present method, outward appearance is particulate state (0.5~3 millimeter of diameter).Owing to having removed pigment filter cake drying, pulverizing, the pilot process of high-speed stirring together with EVA3 wax again, the pollution problem of pigment dry powder thoroughly solves.Energy consumption comparison: dry powder is made in pigment filter cake drying, pulverizing, one ton of pigment needs 2000 yuan of left and right of coal-fired three tons of costs, 300 yuan of power consumptions.Approximately 800 yuan of the power consumptions dewatering through kneading by this law.Save thus 1500 yuan of costs.Coloring effect contrast: the Masterbatch of getting the Masterbatch of produced in conventional processes and producing with pigment preparations, make model check with plastic injection equipment, novel method model is obviously bright in luster, and tinting strength improves 5%~10%.Relevant heterochromatic point, mechanics index of physics is qualified through subscriber checking.
Embodiment
Implementation column 1:
Permanent bordeaux filter cake (CI PR48:2) pigment content 40%, kneader is warming up to 50 ℃, by 62.5 kilograms of permanent bordeaux filter cakes (containing 25 kilograms, pigment dry powder), 10 kilograms, EVA3 wax, 0.5 kilogram of coco amine drops into together, open stirring persistently overheating to 110 degree (jacket temperature), when temperature of charge 95 is spent, open the vacuum pump dehydration being connected with kneader, vacuum tightness 600mmhg, detects material moisture and is less than 0.1%, product is qualified, makes the pigment preparations of 35.5 kilograms of pigment contents 70%.
Implementation column 2:
Permanent bordeaux filter cake (CI PR48:2) pigment content 40%, kneader is warming up to 50 ℃, by 62.5 kilograms of permanent bordeaux filter cakes (containing 25 kilograms, pigment dry powder), 12.5 kilograms, EVA3 wax, 0.5 kilogram of coco amine drops into together, open stirring persistently overheating to 113 degree (jacket temperature), when temperature of charge 97 is spent, open the vacuum pump dehydration being connected with kneader, vacuum tightness 600mmhg, detects material moisture and is less than 0.1%, product is qualified, makes the pigment preparations of 38 kilograms of pigment contents 65%.
Implementation column 3:
Permanent yellow filter cake (CI PY17) pigment content 40%, kneader is warming up to 55 ℃, by 62.5 kilograms of permanent yellow filter cakes (containing 25 kilograms, pigment dry powder), 12.5 kilograms, EVA3 wax, 0.5 kilogram of coco amine drops into together, open stirring persistently overheating to 113 degree (jacket temperature), when temperature of charge 97 is spent, open the vacuum pump dehydration being connected with kneader, vacuum tightness 600mmhg, detects material moisture and is less than 0.1%, product is qualified, makes the pigment preparations of 38 kilograms of pigment contents 65%.
Implementation column 4:
Permanent yellow filter cake (CI PY17) pigment content 40%, kneader is warming up to 55 ℃, by 62.5 kilograms of permanent yellow filter cakes (containing 25 kilograms, pigment dry powder), 15 kilograms, EVA3 wax, 0.5 kilogram of coco amine drops into together, open stirring persistently overheating to 115 degree (jacket temperature), when temperature of charge 98 is spent, open the vacuum pump dehydration being connected with kneader, vacuum tightness 550mmhg, detects material moisture and is less than 0.1%, product is qualified, makes the pigment preparations of 40.5 kilograms of pigment contents 62%.
Implementation column 5:
Blue or green blue filter cake (CI PB15:3) pigment content 40% of phthalein, kneader is warming up to 60 ℃, by 62.5 kilograms of blue or green phthalein blue filter cakes (containing 25 kilograms, pigment dry powder), 17.5 kilograms, EVA3 wax, 0.5 kilogram of coco amine drops into together, open and stir, persistently overheating to 118 degree (jacket temperature), when spending, opens temperature of charge 98 the vacuum pump dehydration being connected with kneader, vacuum tightness 550mmhg, detect material moisture and be less than 0.1%, product is qualified, makes the pigment preparations of 43 kilograms of pigment contents 58%.
Implementation column 6:
Blue or green blue filter cake (CI PB15:3) pigment content 40% of phthalein, kneader is warming up to 60 ℃, by 62.5 kilograms of blue or green phthalein blue filter cakes (containing 25 kilograms, pigment dry powder), 20 kilograms, EVA3 wax, 0.5 kilogram of coco amine drops into together, open stirring persistently overheating to 120 degree (jacket temperature), when temperature of charge 100 is spent, open the vacuum pump dehydration being connected with kneader, vacuum tightness 500mmhg, detects material moisture and is less than 0.1%, product is qualified, makes the pigment preparations of 45.5 kilograms of pigment contents 55%.

Claims (2)

1. do with ethene-vinyl acetate copolymer wax the method that dewatering agent is prepared pigment preparations, it is characterized in that dropping into when kneader is warming up to 50 ℃-60 ℃ pigment filter cake, ethylene-vinyl acetate copolymer wax (EVA3 wax) and coco amine; Open and stir, persistently overheating 95 ℃-100 ℃ of the temperature of charge that make, the vacuum hydro-extraction of opening kneader, vacuum tightness is 500-600mmHg, detects material moisture≤0.1% packing.
2. the method for claim 1, is characterized in that solid weight in pigment filter cake: EVA3 wax=1:0.4~0.8; Coco amine is 2% of pigment solids weight.
CN201410041876.0A 2014-01-28 2014-01-28 Method for preparing pre-dispersing pigment by using ethylene-vinyl acetate copolymer wax as dehydrating agent Pending CN103788469A (en)

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Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3980488A (en) * 1972-03-07 1976-09-14 The Sherwin-Williams Company Pigment conditioning and vehicle flushing process
JPS5512472B2 (en) * 1977-06-06 1980-04-02
US4300954A (en) * 1980-01-03 1981-11-17 Basf Wyandotte Corporation Flushing process for pigments
CN1597791A (en) * 2003-09-17 2005-03-23 宗世栋 Predispersion pigment and its preparation process
CN101392078A (en) * 2008-10-28 2009-03-25 宁波色母粒有限公司 Universal white master batch and preparation method thereof
CN102558611A (en) * 2011-12-26 2012-07-11 上海捷虹颜料化工集团股份有限公司 Pigment prepared product and preparation method thereof

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3980488A (en) * 1972-03-07 1976-09-14 The Sherwin-Williams Company Pigment conditioning and vehicle flushing process
JPS5512472B2 (en) * 1977-06-06 1980-04-02
US4300954A (en) * 1980-01-03 1981-11-17 Basf Wyandotte Corporation Flushing process for pigments
CN1597791A (en) * 2003-09-17 2005-03-23 宗世栋 Predispersion pigment and its preparation process
CN101392078A (en) * 2008-10-28 2009-03-25 宁波色母粒有限公司 Universal white master batch and preparation method thereof
CN102558611A (en) * 2011-12-26 2012-07-11 上海捷虹颜料化工集团股份有限公司 Pigment prepared product and preparation method thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
张天永,等: "挤水转相法有机颜料脱水的研究", 《精细化工》 *

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Application publication date: 20140514