CN109294335A - A kind of fluorescent pigment mill base and preparation method thereof - Google Patents

A kind of fluorescent pigment mill base and preparation method thereof Download PDF

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Publication number
CN109294335A
CN109294335A CN201811022625.2A CN201811022625A CN109294335A CN 109294335 A CN109294335 A CN 109294335A CN 201811022625 A CN201811022625 A CN 201811022625A CN 109294335 A CN109294335 A CN 109294335A
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mill base
fluorescent
sulfate
fluorescent powder
pigment
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Inventor
吴子钊
吕海涛
王玉娥
李桂珍
刘立振
赵强
金艳丽
张新南
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Dekma (tianjin) Technology Development Co Ltd
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Dekma (tianjin) Technology Development Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09DCOATING 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
    • C09D17/00Pigment pastes, e.g. for mixing in paints
    • C09D17/001Pigment pastes, e.g. for mixing in paints in aqueous medium

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  • Life Sciences & Earth Sciences (AREA)
  • Engineering & Computer Science (AREA)
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Abstract

The invention belongs to color technology fields, and in particular to a kind of fluorescent pigment mill base and preparation method thereof.The fluorescent pigment mill base, including pigment, fluorescent powder, wetting dispersing agent, various auxiliary material additives and water;The parts by weight of primary raw material are as follows: pigment 30-50, fluorescent powder 3-5, wetting dispersing agent 5-18, moisturizer 10-20, pH adjusting agent 0.1-5, sagging inhibitor 0.1-0.5, preservative 0.1-0.3, water 10-50.The resulting fluorescent pigment mill base of the present invention, which has in Storage period, not to flocculate, and does not precipitate, not stratified;Good fluidity, good with application system compatibility, coloration efficiency is high, at low cost, entirely without dust;Content of beary metal meets limitation requirement, using it is safe and environment-friendly the features such as.

Description

A kind of fluorescent pigment mill base and preparation method thereof
Technical field
The invention belongs to color technology fields, and in particular to a kind of fluorescent pigment mill base and preparation method thereof.
Background technique
With the development of science and technology with the raising of human living standard, people to the diversity requirement of color increasingly It is high.Fluorescent effect is added in dispersible pigment color paste, product applied by dispersible pigment color paste can be made to increase substantially added value, is increased new Newness forms the differentiation with existing market main product, and attract clients purchase.
About fluorescent pigment mill base, CN103572617A discloses a kind of aqueous anti-settling not stratified fluorescent pigment mill base, It is characterized in that, raw material components are according to weight percent are as follows: wetting agent: 2~20%;Dispersing agent: 1~20%;Stabilizer: 0.1 ~10%;Fluorescent pigment: 25~55%;Surplus is deionized water;
Based on above-mentioned formula, the preparation process of aqueous anti-settling not stratified fluorescent pigment mill base are as follows: first deionized water is added In pre-dispersed kettle, add stabilizer while stirring, continue to stir after the completion of addition, then sequentially add while stirring wetting agent, Dispersing agent and fluorescent pigment continue to stir until being uniformly mixed;By above-mentioned mixed liquor by equipped with zirconium pearl horizontal sand mill into Row grinding distribution, the mixed liquor after dispersion, which filters, tests fineness of dispersion, is transferred in toning slot and adjusts coloured light concentration to get production is arrived Product.The technical issues of document above is solved is to obtain a kind of aqueous anti-settling not stratified fluorescent pigment mill base.
Summary of the invention
In order to solve the above technical problems, the present invention provides one kind to have fluorescent characteristic, environmentally friendly, tinting strength, tinting power By force, the strong dispersible pigment color paste and preparation method thereof of stable components, against weather.
The present invention is realized by following technical solutions:
A kind of fluorescent pigment mill base, the parts by weight of primary raw material are as follows in the mill base:
Pigment is everbright fast yellow, permanent yellow, benzidine yellow, forever solid orange, forever solid orange, permanent bordeaux, everbright fast red, lithol that ocean It is red, forever solid it is pink, quinacridone is red, DPP is red, at least one in permanent violet, quinacridone purple, phthalocyanine blue, dark green, carbon black Kind.
Fluorescent powder is by calcium sulfide, magnesium sulfide, barium sulfate, magnesium sulfate, potassium sulfate, sodium sulphate, strontium sulfate, lithium phosphate, nitric acid Strontium, copper nitrate, silver nitrate, potassium nitrate, aluminium sulfide, barium sulphide, potassium sulfate, at least two phosphor raw materials mixing in strontium sulfate And it is made;
Fluorescent powder is the fluorescent powder of capable of emitting red fluorescence, yellow fluorescence, blue fluorescence;
The fluorescent powder of rubescent fluorescence is made of barium sulfate, magnesium sulfate, lithium phosphate, copper nitrate;
Turn blue fluorescence fluorescent powder by calcium sulfide, sodium sulphate, potassium sulfate, strontium sulfate, sodium chloride, silver nitrate, magnesium sulfide system At;
The fluorescent powder of jaundice fluorescence is made of barium sulphide, magnesium sulfide, aluminium sulfide, potassium nitrate.
Wetting dispersing agent is polyacrylate, modified polyacrylate, modified polyurethane, polyacrylate sodium salt, poly- third Olefin(e) acid ester ammonium salt, polycarboxylic acids alkanol ammonium salt, alkyl polyoxyethylene ether, alkyl phenol polyethenoxy ether sodium sulfate salt, alkyl polyoxy second At least one of alkene ether ammonium sulfate salt, alkyl polyoxyethylene ether phosphate, phenyl phenol polyethenoxy ether.
Moisturizer is polyethylene glycol and its derivative, polypropylene glycol and its derivative, glycerine, butantriol, triethylene glycol, four At least one of glycol, triethanolamine, triethylene glycol ether, diethylene glycol dibutyl ether, one ether of triethylene glycol, tetraethylene glycol dimethyl ether.
PH adjusting agent is any one of ammonium hydroxide, urea, sodium hydroxide, potassium hydroxide and triethanolamine.
Sagging inhibitor is at least one of fumed silica, organobentonite and polyethylene wax.
Preservative is 1-2 benzisothiazole-3-ketone, 2-methyl-4-isothiazolin-3-one, 5- chloro-2-methyl -4- different Thiazoline -3- ketone/at least one of 2-methyl-4-isothiazolin-3-one and Kathon CG.
The preparation method of above-mentioned fluorescent pigment mill base, includes the following steps:
(1) water, wetting dispersing agent, moisturizer, pH adjusting agent, sagging inhibitor, preservative are put into pre-dispersed machine It mixes, be uniformly mixed liquid after dispersing speed 300-500r/min, 20min;
(2) pigment is added in above-mentioned uniform mixed liquor, carries out pre-dispersed, dispersing speed 1000-1500r/min, Jitter time is 30min-60min, obtains pre-dispersed slurry;
(3) calcination 50min is heated after mixing phosphor raw material at 133 DEG C, grinder grinding is subsequently placed in, until grain Stop grinding when diameter is distributed d90 less than 1 μm, then be placed in water immersion precipitating, hair different colours are obtained after gained sediment is dry The fluorescent powder of fluorescence;
(4) fluorescent powder is added in pre-dispersed slurry, is ground using grinder, until size distribution d90 is less than 1 μm, Stop grinding;
(5) if the requirement in (4) is not achieved in granularity, step (4) are repeated until mill base granularity reaches requirement;
(6) the ground mill base for reaching granularity requirements, using quality testing, deaeration and filters and packages, is finally produced Product fluorescent pigment mill base.
Grinder employed in step (3) and/or (4) is any in basket type sand grid, vertical sand milling and horizontal sand milling Kind.
The thinking of inventor is in the present invention, by adjusting being formulated and improving technique, provides that a kind of compatibility is good, ingredient is steady Calmly, against weather is strong, keeps pigment coloration, while adding the dispersible pigment color paste of fluorescent component.Wherein, change the production work of fluorescent powder Skill replaces the fluorescent component of traditional rare-earth trichromatic, improves ornamental value, while under the premise of meeting granularity requirements significantly It reduces costs.Fluorescent powder provided by the present invention can combine, the color of fluorescence needed for obtaining.
The beneficial effects of the present invention are the resulting fluorescent pigment mill base of the present invention, which has in Storage period, not to flocculate, and does not sink It forms sediment, it is not stratified;Good fluidity, good with application system compatibility, coloration efficiency is high, at low cost, entirely without dust;Heavy metal contains Amount meet limitation requirement, using it is safe and environment-friendly the features such as.
Detailed description of the invention
Fig. 1 is the viscosity variation diagram after placing one month under the product high temperature in embodiment 1;
Fig. 2 is the viscosity variation diagram after the product in embodiment 2 is exposed to the sun one month.
Specific embodiment
The present invention will be further explained combined with specific embodiments below, so that those skilled in the art knows more about The present invention, but be not intended to limit the present invention.
The manufacturer of each raw material:
Preservative BIT, i.e. 1-2 benzisothiazole-3-ketone, Li Yuan Chemical Co., Ltd. of Foshan City
Preservative MIT, i.e. 2-methyl-4-isothiazolin-3-one, In Luohu District of Shenzhen Municipal Yu Zhe washing material factory
Preservative CMIT, 5-Chloro-2-methyl-4-isothiazolin-3-one/2-methyl-4-isothiazolin-3-one, Hangzhou sieve River Chemical Co., Ltd.
Preservative Kathon CG(Methylchloroisothiazolinone/Methylisothiazolinone combination), model: DL101, Jinan De Lan Chemical Co., Ltd.
Antioxidant BHA (butylated hydroxy anisole), Changzhou Yu Rong Chemical Co., Ltd.
Used material is all from commercially available common raw material;It does not enumerate one by one herein;
Embodiment 1
A kind of dispersible pigment color paste for being added to red fluorescent powder is prepared, specific steps are as follows:
(1) 20 parts of water, 10 parts of wetting dispersing agent, 20 parts of moisturizer, BHA0.3 parts of antioxidant, anti-settling are weighed in proportion 0.3 part of agent fumed silica, BIT0.2 parts of preservative, 0.3 part of pH adjusting agent;By water, wetting dispersing agent, moisturizer, resist Oxidant, sagging inhibitor, preservative are put into pre-dispersed device and are mixed, and obtain uniformly after dispersing speed 500r/min, 20min Mixed liquor;
Wetting dispersing agent is made of polyacrylate, phenyl phenol polyethenoxy ether, polyacrylate sodium salt, polyacrylic acid Ester: phenyl phenol polyethenoxy ether: polyacrylate sodium salt=2:1:1, (w/w);
Moisturizer is made of polyethylene glycol and its derivative and triethylene glycol ether, polyethylene glycol and its derivative: three second two Alcohol ether=2:1, (w/w);
PH adjusting agent is sodium hydroxide (solid particle);
(2) 40 parts of pigment permanent bordeauxs are added in above-mentioned uniform mixed liquor, carry out pre-dispersed, dispersing speed 1500r/ Min, jitter time 50min obtain pre-dispersed slurry;
(3) preparation of red fluorescent powder:
Ratio weighs 55 parts of barium sulfate, 40 parts of magnesium sulfate, 2 parts of lithium phosphate, 3 parts of copper nitrate in parts by weight, after mixing After heating calcination 50min at 133 DEG C, it is put into vertical grinding machine and is ground, stopped when particle diameter distribution d90 is less than 1 μm Grinding, is placed in water immersion for the material after grinding and precipitates, obtain drying precipitate and obtain red fluorescent powder;
(4) preparation of the dispersible pigment color paste of red fluorescent powder is added:
3 parts of red fluorescent powders are added into pre-dispersed slurry, above-mentioned pre-dispersed slurry is ground using horizontal mill Mill, until size distribution d90 less than 1 μm, stops grinding;
(5) if above-mentioned requirement is not achieved in granularity, step (4) are repeated until mill base granularity reaches requirement;
(6) the ground mill base for reaching granularity requirements obtains final after quality testing, deaeration and filtering and packaging Product fluorescent pigment mill base.
The present invention is the original of use with " aqueous anti-settling not stratified fluorescent pigment mill base " maximum difference in background technique Material is not fluorescent pigment, but pigment and fluorescent powder;In the process of the invention, fluorescent powder and pigment are respectively processed; Specific treatment process is:
Pigment is added in above-mentioned uniform mixed liquor, pre-dispersed, dispersing speed 1500r/min, jitter time are carried out For 50min, pre-dispersed slurry is obtained;
Fluorescent powder is added to pre-dispersed mill base, above-mentioned pre-dispersed slurry is ground using grinder, until granularity D90 is distributed less than 1 μm, stops grinding;
Main cause is: mill base is a dispersion, and general pigment keeps prolonged in a liquid with suspended form Stable state is very difficult, because the complexing of pigment particles majority is blocking at offspring accumulation in liquid, works as pigment particles When competition or its charge character of the dispersing agent by other materials of outer package or absorption are destroyed, pigment particles each other by To external force traction when, be all easy to produce cohesion between pigment particles, sedimentation even deposition layering etc. unstable situation Occur, therefore, there are unstable tendencies for itself.The present invention is handled pigment and fluorescent powder by improvement technique respectively, and And adjustment formula, properly mixed dispersing agent (concrete analysis is as follows) is added, enhances the stability of mill base, overcomes due to pigment It is unstable there is a phenomenon where settling in mill base, especially overcome to be more prone to produce to be layered after pigment and fluorescent powder combination and sink This defect of phenomena such as drop.
Dispersing agent of the present invention and moisturizer penetrate into pigment particles by its wetting action and osmosis Oriented attachment occurs on the surface of the particle for gap, to change the surface property of pigment particles and phosphor particles, and makes particle Surface electrification, form electric double layer makes pigment dispersion system form stabilization to prevent the aggregation of particle.It is of the present invention Dispersing agent is not optional, and the selection of dispersing agent is more important for system of the invention, the reason is that, to make pigment and Fluorescent powder can be soaked by decentralized medium, made dispersant adsorption in particle surface, reduced surface free energy, break pigment and fluorescence The secondary structure of powder association, forms stable system.
In addition, the present inventor obtains ideal pigment and fluorescent powder, filters out by investigation and many experiments Color is suitable for, granularity loosely, the small pigment and fluorescent powder for being suitable for dispersion of the degree of polymerization, both make to present in colour paste system good Good " normal distribution " curve, and further reach this purpose, it is necessary in conjunction with specific technique, to pigment in technique of the invention Such as dispersed respectively with fluorescent powder, calcination grinding, redisperse or the technique of decentralized processing repeatedly, makes pigment and fluorescent powder Crystal particle diameter concentrates in the range of a more uniform alternatively relative narrowness, avoid the occurrence of excessive or too small particle from And pigment or fluorescent powder is caused to disperse the problem of unevenness settles.
Judge mill base viscosity at any time with temperature change (such as attached drawing 1):
The main reason for dispersible pigment color paste changes is that ultraviolet light and visible rays are broken to caused by pigment product in sunlight It is bad, in addition to this, temperature and the moist change that can also accelerate color;
Dispersible pigment color paste is mainly manifested in the variation of color, takes off because weather (temperature or ultraviolet light) changes caused by influencing Color, gloss disappearance phenomena such as on;
The present invention has carried out experiment below to examine the weatherability of product in embodiment 1:
Measuring method: mill base product is placed at 60-65 DEG C, and after 3 days, every 3 days, all its viscosity was examined in sampling It surveys, is changed by its viscosity of Data Mining, to judge its high temperature resistance;
As can be seen that manufactured mill base is placed one month at high temperature from attached drawing 1, viscosity changes over time value very Small, after one month, viscosity is substantially unchanged;This illustrates that its high temperature resistance of mill base product of the invention is good, and stability is strong; Viscosity is not to generate biggish variation with high temperature or time;
By above data as can be seen that the product of embodiment 1, relatively stable viscosity (is the item in 6r/min It is measured under part).
In attached drawing 1 and attached drawing 2, abscissa is number of days, and ordinate is viscosity, and the unit of viscosity is (mPaS).
Embodiment 2
A kind of dispersible pigment color paste for adding blue phosphor is prepared, specific steps are as follows:
(1) 20 parts of water, 10 parts of wetting dispersing agent, 20 parts of moisturizer, BHA0.3 parts of antioxidant, anti-settling are weighed in proportion 0.3 part of agent organobentonite, BIT0.2 parts of preservative, 0.3 part of pH adjusting agent;By water, wetting dispersing agent, moisturizer, antioxygen Agent, sagging inhibitor, preservative are put into pre-dispersed device and are mixed, and obtain after dispersing speed 500r/min, 20min and uniformly mix Close liquid;
Wetting dispersing agent is made of modified polyurethane, polycarboxylic acids alkanol ammonium salt, modified polyurethane: polycarboxylic acids alkanol ammonium salt= 1:3;(w/w);
Moisturizer is made of tetraethylene glycol and glycerine, tetraethylene glycol: glycerine=1:1, (w/w);
PH adjusting agent is sodium hydroxide (solid particle);
(2) 35 parts of monastral blue indigo plants are added in above-mentioned uniform mixed liquor, carry out pre-dispersed, dispersing speed 1200r/ Min, jitter time 40min obtain pre-dispersed slurry;
(3) preparation of blue phosphor: 63 parts of calcium sulfide, 5 parts of sodium sulphate, 5 parts of potassium sulfate, strontium sulfate 10 are weighed in proportion Part, 6 parts of sodium chloride, 1 part of silver nitrate, 10 parts of magnesium sulfide, after mixing at 133 DEG C heat calcination 50min after, be put into grinder into Row grinding, until particle diameter distribution d90 is less than 1 μm, stopping grinding impregnating precipitating into the water, obtains drying precipitate and obtain indigo plant Fluorescent powder;
(4) preparation of the dispersible pigment color paste of blue phosphor is added:
3 parts of blue phosphor are added into pre-dispersed slurry, above-mentioned pre-dispersed slurry is ground using horizontal mill Mill, until size distribution d90 less than 1 μm, stops grinding;
(5) if above-mentioned requirement is not achieved in granularity, step (4) are repeated until mill base granularity reaches requirement;
(6) the ground mill base for reaching granularity requirements obtains final after quality testing, deaeration and filtering and packaging Product fluorescent pigment mill base.
Attached drawing 2 be after product is exposed to the sun one month under the sun viscosity (when being exposed to the sun the mean temperature on daytime be 32 DEG C, most High-temperature is 39 DEG C);
As can be seen that the viscosity of product is also more stable from attached drawing 2, light resistance is preferable.
Embodiment 3
A kind of dispersible pigment color paste for being added to yellow fluorescent powder is prepared, its step are as follows:
(1) 20 parts of water, 10 parts of wetting dispersing agent, 20 parts of moisturizer, BHA0.3 parts of antioxidant, anti-settling are weighed in proportion 0.3 part of agent fumed silica, BIT0.2 parts of preservative, 0.3 part of pH adjusting agent;By water, wetting dispersing agent, moisturizer, resist Oxidant, sagging inhibitor, preservative are put into pre-dispersed device and are mixed, and obtain uniformly after dispersing speed 500r/min, 20min Mixed liquor;
Wetting dispersing agent is by alkyl polyoxyethylene ether ammonium sulfate, phenyl phenol polyethenoxy ether, polyacrylate sodium salt group At alkyl polyoxyethylene ether ammonium sulfate: phenyl phenol polyethenoxy ether: polyacrylate sodium salt=1:1:1;(w/w);
Moisturizer is made of polyethylene glycol and its derivative and triethylene glycol ether, polyethylene glycol and its derivative: three second two Alcohol ether=2:1, (w/w);
PH adjusting agent is sodium hydroxide (solid particle);
(2) 40 parts of pigment everbright fast yellows are added in above-mentioned uniform mixed liquor, carry out pre-dispersed, dispersing speed 1500r/ Min, jitter time 30min obtain pre-dispersed slurry;
(3) preparation of yellow fluorescent powder: 55 parts of barium sulphide, 40 parts of magnesium sulfide, 2 parts of aluminium sulfide, potassium nitrate 3 are weighed in proportion Part, after heating calcination 50min at 133 DEG C after mixing, it is put into grinder and is ground, until particle diameter distribution d90 is less than 1 μm, Stop grinding, impregnates precipitating into the water, obtain drying precipitate and obtain yellow fluorescent powder;
(4) preparation of the dispersible pigment color paste of yellow fluorescent powder is added:
3 parts of yellow fluorescent powders are added into pre-dispersed slurry, above-mentioned pre-dispersed slurry is ground using horizontal mill Mill, until size distribution d90 less than 1 μm, stops grinding;
(5) if above-mentioned requirement is not achieved in granularity, step (4) are repeated until mill base granularity reaches requirement;
(6) the ground mill base for reaching granularity requirements obtains final after quality testing, deaeration and filtering and packaging Product fluorescent pigment mill base.
Embodiment 4
A kind of dispersible pigment color paste for being added to red fluorescent powder is prepared, specific steps are as follows:
(1) 20 parts of water, 10 parts of wetting dispersing agent, 20 parts of moisturizer, sagging inhibitor fumed silica 0.3 are weighed in proportion Part, 0.2 part of preservative MIT, 0.25 part of pH adjusting agent;Water, wetting dispersing agent, moisturizer, sagging inhibitor, preservative are thrown Enter into pre-dispersed device and mix, uniform mixed liquor is obtained after dispersing speed 500r/min, 20min;
Wetting dispersing agent is made of polyacrylate, phenyl phenol polyethenoxy ether, polyacrylate sodium salt, polyacrylic acid Ester: phenyl phenol polyethenoxy ether: polyacrylate sodium salt=2:1:1, (w/w);
Moisturizer is made of polyethylene glycol and its derivative and triethylene glycol ether, polyethylene glycol and its derivative: three second two Alcohol ether=2:1, (w/w);
PH adjusting agent is sodium hydroxide (solid particle);
(2) 40 parts of pigment permanent bordeauxs are added in above-mentioned uniform mixed liquor, carry out pre-dispersed, dispersing speed 1500r/ Min, jitter time 50min obtain pre-dispersed slurry;
(3) preparation of red fluorescent powder:
Ratio weighs 55 parts of barium sulfate, 40 parts of magnesium sulfate, 2 parts of lithium phosphate, 3 parts of copper nitrate in parts by weight, after mixing After heating calcination 50min at 133 DEG C, it is put into vertical grinding machine and is ground, stopped when particle diameter distribution d90 is less than 1 μm Grinding, is placed in water immersion for the material after grinding and precipitates, obtain drying precipitate and obtain red fluorescent powder;
(4) preparation of the dispersible pigment color paste of red fluorescent powder is added:
3 parts of red fluorescent powders are added into pre-dispersed slurry, above-mentioned pre-dispersed slurry is ground using horizontal mill Mill, until size distribution d90 less than 1 μm, stops grinding;
(5) if above-mentioned requirement is not achieved in granularity, step (4) are repeated until mill base granularity reaches requirement;
(6) the ground mill base for reaching granularity requirements obtains final after quality testing, deaeration and filtering and packaging Product fluorescent pigment mill base.
Comparative example 1
Wetting dispersing agent is adjusted to 2 parts, remaining is identical with embodiment 1;
Comparative example 2
Wetting dispersing agent is adjusted to 25 parts, remaining is identical with embodiment 1;
Comparative example 3
In comparative example 3,
(2) are as follows: 40 parts of pigment are added in above-mentioned uniform mixed liquor, mixing obtains mixed material;
(4) preparation of the dispersible pigment color paste of red fluorescent powder is added:
3 parts of red fluorescent powders are added in the mixed material into (2), using horizontal mill to above-mentioned pre-dispersed slurry into Row grinding, until size distribution d90 less than 1 μm, stops grinding;
Remaining the step of, is same as Example 1;
Comparative example 4
(3) preparation of yellow fluorescent powder: 55 parts of barium sulphide, 40 parts of magnesium sulfide, 2 parts of aluminium sulfide, potassium nitrate 3 are weighed in proportion Part, it is mixed to get yellow fluorescent powder;Remaining step is same as Example 1;
About present invention mill base obtained, inventor has carried out test experience below:
Detection method: resulting product of the present invention is examined according to GB/T 21473-2008 " tinting system mill base " (wherein specific index is carried out according to the method in above-mentioned standard annex) is surveyed, the result of detection is as follows:
The properties of product contrast table of table 1 embodiment 1-4 and each comparative example
As can be seen from the above data, the hue difference in the present invention in embodiment 1-4 is smaller, chroma difference and luminosity equation also compared with It is small, illustrate that its color fastness of product of the invention is preferable, retention of color is preferable.And the viscosity in embodiment 1-4 is more equal One, numerical value is close, it was demonstrated that and the stability and reproducibility of product are preferable, while the weatherability of product is preferable, have reached 5 grades, and Other Experimental comparison's example 1-4 are compared, weatherability is poor.Comparative example 3,4 has adjusted processing step, not technique through the invention Step is handled, its relative color strength of product obtained is poor, and hue difference is larger.The appearance of product is observed by the naked eye, It was found that the layering and deposited phenomenon in comparative example 3,4 are than more serious.And without lamination in embodiment 1-4.
Detection (mg/kg) of the table 2 about content of beary metal in the product in embodiment 1-4
Dissoluble lead Soluble chromium Soluble cadmium Soluble mercury
Embodiment 1 22 18 43 21
Embodiment 2 20 21 39 25
Embodiment 3 24 22 37 28
Embodiment 4 23 19 45 22
The standard of content of beary metal specified in GB/T 21473-2008 is:
Dissoluble lead≤90mg/kg, soluble cadmium≤75mg/kg, soluble chromium≤60mg/kg, soluble mercury≤60mg/ kg;
The method of heavy metal analysis is: method as defined in appendix C in GB18582-2001;
The data of content of beary metal in above table are respectively less than the specified value in above-mentioned national standard, in the model of safety Within enclosing, product of the invention is to belong to environmentally friendly product.
By above data as can be seen that product of the invention, has preferable mobility, long-time storage is not agglomerated, It is not stratified, do not precipitate, no Signs of Mould generates;The viscosity stablization of product;The features such as strong coloring force, content of beary metal is lower.
The above description is merely a specific embodiment, but scope of protection of the present invention is not limited thereto, because This, protection scope of the present invention should be determined by the scope of protection defined in the claims.

Claims (10)

1. a kind of fluorescent pigment mill base, which is characterized in that the parts by weight of primary raw material are as follows in the mill base:
2. fluorescent pigment mill base as described in claim 1, which is characterized in that pigment be everbright fast yellow, permanent yellow, benzidine yellow, Forever solid orange, forever solid orange, permanent bordeaux, everbright fast red, lithol your fuchsin, it is forever solid it is pink, quinacridone is red, DPP is red, permanent violet, At least one of quinacridone purple, phthalocyanine blue, dark green, carbon black.
3. fluorescent pigment mill base as described in claim 1, which is characterized in that fluorescent powder by calcium sulfide, magnesium sulfide, barium sulfate, Magnesium sulfate, potassium sulfate, sodium sulphate, strontium sulfate, lithium phosphate, strontium nitrate, copper nitrate, silver nitrate, potassium nitrate, aluminium sulfide, barium sulphide, At least two phosphor raw materials in potassium sulfate, strontium sulfate are mixed and are made;
Fluorescent powder is the fluorescent powder of capable of emitting red fluorescence, yellow fluorescence, blue fluorescence;
The fluorescent powder of rubescent fluorescence is made of barium sulfate, magnesium sulfate, lithium phosphate, copper nitrate;
The fluorescent powder of fluorescence of turning blue is made of calcium sulfide, sodium sulphate, potassium sulfate, strontium sulfate, sodium chloride, silver nitrate, magnesium sulfide;
The fluorescent powder of jaundice fluorescence is made of barium sulphide, magnesium sulfide, aluminium sulfide, potassium nitrate.
4. fluorescent pigment mill base as described in claim 1, which is characterized in that wetting dispersing agent is polyacrylate, is modified and gathers Acrylate, modified polyurethane, polyacrylate sodium salt, polyacrylic acid ester ammonium salt, polycarboxylic acids alkanol ammonium salt, alkyl polyoxyethylene Ether, alkyl phenol polyethenoxy ether sodium sulfate salt, alkyl polyoxyethylene ether ammonium sulfate, alkyl polyoxyethylene ether phosphate, phenyl At least one of phenol polyethenoxy ether.
5. fluorescent pigment mill base as described in claim 1, which is characterized in that moisturizer is polyethylene glycol and its derivative, gathers Propylene glycol and its derivative, glycerine, butantriol, triethylene glycol, tetraethylene glycol, triethanolamine, triethylene glycol ether, two fourth of diethylene glycol (DEG) At least one of ether, one ether of triethylene glycol, tetraethylene glycol dimethyl ether.
6. fluorescent pigment mill base as described in claim 1, which is characterized in that pH adjusting agent is ammonium hydroxide, urea, hydroxide Any one of sodium, potassium hydroxide and triethanolamine.
7. fluorescent pigment mill base as described in claim 1, which is characterized in that sagging inhibitor is fumed silica, organic bentonite At least one of profit soil and polyethylene wax.
8. fluorescent pigment mill base as described in claim 1, which is characterized in that preservative be 1-2 benzisothiazole-3-ketone, 2-methyl-4-isothiazolin-3-one, 5-Chloro-2-methyl-4-isothiazolin-3-one/2-methyl-4-isothiazolin-3-one and card At least one of pine.
9. the preparation method of fluorescent pigment mill base as described in claim 1, includes the following steps:
(1) water, wetting dispersing agent, moisturizer, pH adjusting agent, sagging inhibitor, preservative are put into pre-dispersed machine and are mixed, Dispersing speed is 300-500r/min, and be uniformly mixed liquid after 20min;
(2) pigment is added in above-mentioned uniform mixed liquor, carries out pre-dispersed, dispersing speed 1000-1500r/min, dispersion Time is 30min-60min, obtains pre-dispersed slurry;
(3) calcination 50min is heated after mixing phosphor raw material at 133 DEG C, grinder grinding is subsequently placed in, until partial size point Stop grinding when cloth d90 is less than 1 μm, then be placed in water immersion precipitating, hair different colours fluorescence is obtained after gained sediment is dry Fluorescent powder;
(4) it will be added in the pre-dispersed slurry of (2), ground using grinder, until granularity point by the fluorescent powder of (3) processing Cloth d90 stops grinding less than 1 μm;
(5) if the requirement in (4) is not achieved in granularity, step (4) are repeated until mill base granularity reaches requirement;
(6) the ground mill base for reaching granularity requirements, using quality testing, deaeration and filters and packages, it is glimmering to obtain final products Delustering pigment mill base.
10. the preparation method of fluorescent pigment mill base as claimed in claim 9, it is characterised in that: institute in step (3) and/or (4) The grinder used is any one of basket type sand grid, vertical sand milling and horizontal sand milling.
CN201811022625.2A 2018-09-03 2018-09-03 A kind of fluorescent pigment mill base and preparation method thereof Pending CN109294335A (en)

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