CN105131653A - Iron oxide black pigment used for printing ink and preparation method thereof - Google Patents
Iron oxide black pigment used for printing ink and preparation method thereof Download PDFInfo
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- CN105131653A CN105131653A CN201510441232.5A CN201510441232A CN105131653A CN 105131653 A CN105131653 A CN 105131653A CN 201510441232 A CN201510441232 A CN 201510441232A CN 105131653 A CN105131653 A CN 105131653A
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Abstract
The invention discloses an iron oxide black pigment used for printing ink, which is prepared from following raw materials, by weight, 80-100 parts of modified iron oxide black, 5-10 parts of graphite powder, 1-2 parts of hydroxyethyl cellulose, 6-8 parts of sodium silicate, 0.1-0.2 parts of azodiisobutyronitrile, 0.1-0.2 parts of starch sodium octenyl succinate, 10-15 parts of styrene, 1-2 parts of microcrystalline wax and 1-2 parts of glycerol triacetate. The iron oxide black pigment has strong tinting strength, is excellent in temperature and weather resistance, is easy to disperse, is good in processing performance, is strong in adhesive fastness, is not liable to fall off, is good in abrasion resistance and use performances, and is suitable for printing ink pigments.
Description
Technical field
The present invention relates to iron oxide pigment field, be specifically related to a kind of ink black iron oxide pigment and preparation method thereof.
Background technology
Iron oxide black is the one of iron pigment, and its moiety is Z 250, has saturated indigo plant ink light blue.Black iron oxide pigment has good weathering resistance, to light and atmospheric stability, opacifying power and tinting strength high, form and aspect are pure, with low cost, can be widely used in the industries such as building, plastics, pottery, coating.Along with the development of economy, the requirement of market to black iron oxide pigment also improves constantly, and its Application Areas and purposes are just constantly widened.But in actual applications, because the heat resistance of iron oxide black is poor, can fade at relatively high temperatures, the phenomenon such as variable color, easily reunite in addition, be difficult to problems such as being uniformly dispersed, limit the use range of iron oxide black.Therefore, need to carry out surface treatment to black iron oxide pigment, to reach lifting use properties, enrich product function, the object of meeting the market requirement.
Summary of the invention
The object of this invention is to provide a kind of ink black iron oxide pigment, have good temperature tolerance and erosion resistance, be easy to dispersion in the base, attachment fastness is strong, and printing difficult drop-off, crocking resistance is good, and use properties is good.
The present invention is achieved by the following technical solutions:
A kind of ink black iron oxide pigment, it is obtained by the raw material of following weight parts:
Modified oxidized iron black 80-100, Graphite Powder 99 5-10, Natvosol 1-2, water glass 6-8, Diisopropyl azodicarboxylate 0.1-0.2, starch Sodium Octenyl Succinate 0.1-0.2, vinylbenzene 10-15, Microcrystalline Wax 1-2, glycerine triacetate 1-2;
Wherein modified oxidized iron oxide black is obtained by the raw material of following weight parts: ferrous sulfate 40-50, imidazoline quaternary ammonium salt 0.3-0.5, citric acid 0.3-0.5, dimethyl silicone oil 0.2-0.4; Citric acid is added to the water by solid-liquid weight ratio 1:100-1:150 to dissolve completely by the preparation method of described modified oxidized iron oxide black, and all the other raw materials 800-1000r/min added outside sulfuric acid ferrous iron stirs 5-10min, obtains modification liquid; Ferrous sulfate is added to the water the solution being mixed with 150-200g/L, in solution, adds described modification liquid, pH regulator is stirred to 7-8, pass into oxygen to be oxidized under 80-90 DEG C of condition, react the iron oxide black of terminating in rear separating slurry, through washing, oven dry, pulverize, to obtain final product.
A preparation method for ink black iron oxide pigment, comprises the following steps:
(1) grinding after modified oxidized iron oxide black, Graphite Powder 99 and Natvosol mixing evenly, is then added the water of 2-3 times of weight, obtains iron oxide black slurries after dispersed with stirring;
(2) water glass is added to the water the solution being mixed with 20-30g/L, is then added dropwise in the iron oxide black slurries in (1) and stirs, by pH regulator to 8-8.5, then ageing 2-3h, filters, washs and obtain coated with silica iron oxide black after drying;
(3) Diisopropyl azodicarboxylate is dissolved in a small amount of toluene obtains initiation solution; Coated with silica iron oxide black in (2) and vinylbenzene to be added jointly in appropriate dehydrated alcohol and to be uniformly dispersed; pass into nitrogen protection and temperature is adjusted to 70-80 DEG C; drip initiation solution reaction 2-4h; mix with all the other raw materials after filtration, washing and grind evenly, after drying, namely obtaining ink black iron oxide pigment.
Advantage of the present invention is:
The present invention utilizes the properties-correcting agent such as imidazoline quaternary ammonium salt and citric acid to carry out modification to iron oxide black, plays good dissemination in particle formation, effectively improves the tinting strength of iron oxide black, has corrosion inhibition simultaneously; Then carry out silicon-dioxide and vinylbenzene double-coated, both improved the temperature tolerance of black iron oxide pigment, make it have again good erosion resistance, improve its dispersing property in the base simultaneously; Composite by raw material, makes the black iron oxide pigment tinting strength that obtains high, temperature tolerance and weathering resistance good, be easy to dispersion, good processability, attachment fastness is strong, and printing difficult drop-off, crocking resistance is good, and use properties is good, is applicable to ink pigment.
Embodiment
Non-limiting examples of the present invention is as follows:
A kind of ink black iron oxide pigment, is prepared from by the component raw material of following weight (kg):
Modified oxidized iron black 90, Graphite Powder 99 8, Natvosol 1.5, water glass 7, Diisopropyl azodicarboxylate 0.15, starch Sodium Octenyl Succinate 0.15, vinylbenzene 12, Microcrystalline Wax 1.5, glycerine triacetate 1.5;
Wherein modified oxidized iron oxide black is obtained by the raw material of following weight parts: ferrous sulfate 45, imidazoline quaternary ammonium salt 0.4, citric acid 0.4, dimethyl silicone oil 0.3; Citric acid is added to the water by solid-liquid weight ratio 1:100 to dissolve completely by the preparation method of described modified oxidized iron oxide black, and all the other raw materials 1000r/min added outside sulfuric acid ferrous iron stirs 5min, obtains modification liquid; Ferrous sulfate is added to the water the solution being mixed with 150g/L, in solution, adds described modification liquid, pH regulator is stirred to 7-8, pass into oxygen to be oxidized under 80 DEG C of conditions, react the iron oxide black of terminating in rear separating slurry, through washing, oven dry, pulverize, to obtain final product.
The preparation method of ink black iron oxide pigment comprises the following steps:
(1) grinding after modified oxidized iron oxide black, Graphite Powder 99 and Natvosol mixing evenly, is then added the water of 3 times of weight, obtains iron oxide black slurries after dispersed with stirring;
(2) water glass is added to the water the solution being mixed with 25g/L, is then added dropwise in the iron oxide black slurries in (1) and stirs, by pH regulator to 8-8.5, then ageing 2h, filters, washs and obtain coated with silica iron oxide black after drying;
(3) Diisopropyl azodicarboxylate is dissolved in a small amount of toluene obtains initiation solution; Coated with silica iron oxide black in (2) and vinylbenzene to be added jointly in appropriate dehydrated alcohol and to be uniformly dispersed; pass into nitrogen protection and temperature is adjusted to 80 DEG C; drip initiation solution reaction 2h; mix with all the other raw materials after filtration, washing and grind evenly, after drying, namely obtaining ink black iron oxide pigment.
Above-mentioned obtained black iron oxide pigment performance is as following table:
| Project | Analytical results |
| 105 DEG C of volatile matter/% | 1.2 |
| Screenings (320 mesh sieve) | 0.3 |
| Tinctorial strength/% | 97.1 |
| Coloured light (with standard specimen ratio) | Slightly |
| Resistance to 260 DEG C/30min △ E | 0.39 |
Claims (2)
1. an ink black iron oxide pigment, is characterized in that, it is obtained by the raw material of following weight parts:
Modified oxidized iron black 80-100, Graphite Powder 99 5-10, Natvosol 1-2, water glass 6-8, Diisopropyl azodicarboxylate 0.1-0.2, starch Sodium Octenyl Succinate 0.1-0.2, vinylbenzene 10-15, Microcrystalline Wax 1-2, glycerine triacetate 1-2;
Described modified oxidized iron oxide black is obtained by the raw material of following weight parts: ferrous sulfate 40-50, imidazoline quaternary ammonium salt 0.3-0.5, citric acid 0.3-0.5, dimethyl silicone oil 0.2-0.4; Citric acid is added to the water by solid-liquid weight ratio 1:100-1:150 to dissolve completely by the preparation method of described modified oxidized iron oxide black, and all the other raw materials 800-1000r/min added outside sulfuric acid ferrous iron stirs 5-10min, obtains modification liquid; Ferrous sulfate is added to the water the solution being mixed with 150-200g/L, in solution, adds described modification liquid, pH regulator is stirred to 7-8, pass into oxygen to be oxidized under 80-90 DEG C of condition, react the iron oxide black of terminating in rear separating slurry, through washing, oven dry, pulverize, to obtain final product.
2. the preparation method of a kind of ink black iron oxide pigment according to claim 1, is characterized in that, comprise the following steps:
(1) grinding after modified oxidized iron oxide black, Graphite Powder 99 and Natvosol mixing evenly, is then added the water of 2-3 times of weight, obtains iron oxide black slurries after dispersed with stirring;
(2) water glass is added to the water the solution being mixed with 20-30g/L, is then added dropwise in the iron oxide black slurries in (1) and stirs, by pH regulator to 8-8.5, then ageing 2-3h, filters, washs and obtain coated with silica iron oxide black after drying;
(3) Diisopropyl azodicarboxylate is dissolved in a small amount of toluene obtains initiation solution; Coated with silica iron oxide black in (2) and vinylbenzene to be added jointly in appropriate dehydrated alcohol and to be uniformly dispersed; pass into nitrogen protection and temperature is adjusted to 70-80 DEG C; initiation solution reaction 2-4h described in dropping; mix with all the other raw materials after filtration, washing and grind evenly, after drying, namely obtaining ink black iron oxide pigment.
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Application publication date: 20151209 |