CN1008374B - Mfr. of an inorganic mo-w yellow dye - Google Patents

Mfr. of an inorganic mo-w yellow dye

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Publication number
CN1008374B
CN1008374B CN 85100779 CN85100779A CN1008374B CN 1008374 B CN1008374 B CN 1008374B CN 85100779 CN85100779 CN 85100779 CN 85100779 A CN85100779 A CN 85100779A CN 1008374 B CN1008374 B CN 1008374B
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CN
China
Prior art keywords
inorganic
pigment
equal
yellow dye
precipitation agent
Prior art date
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Expired
Application number
CN 85100779
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Chinese (zh)
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CN85100779A (en
Inventor
张文朴
张爱军
周宏才
冯瑞琴
于润湖
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Beijing Normal University
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Beijing Normal University
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Application filed by Beijing Normal University filed Critical Beijing Normal University
Priority to CN 85100779 priority Critical patent/CN1008374B/en
Publication of CN85100779A publication Critical patent/CN85100779A/en
Publication of CN1008374B publication Critical patent/CN1008374B/en
Expired legal-status Critical Current

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Abstract

The present invention relates to novel inorganic Mo-W yellow dye. The chemical formula of the inorganic Mo-W yellow dye is Bi [1-(x+y)/3]M0xWyV[1-(X+Y)]O4 in the production process of the inorganic Mo-W yellow dye, wherein (x+y) is more than or equal to 0.1 and is less than or equal to 0.35; hot water at the temperature of 30 to 70 DGE C is used as the solvent of a precipitant, concentrated ammonia liquor is used for adjusting the reaction acidity of which the pH is more than or equal to 1.5 and is less than or equal to 3.5 so as to shorten the synthesis period; meanwhile, titanium dioxide containing less than 0.1 part of Fe2O3 is used as a bulking agent, not only the cost is reduced, but also the hiding power is obviously improved under the condition that the color saturation of the dye is influenced.

Description

Mfr. of an inorganic Mo-W Yellow dye
The invention belongs to the manufacturing technology field of mineral dye.
The nontoxic inorganic yellow pigment that with the pucherite is matrix is a noticeable regeneration product in the world today, it is the yellow pigment of matrix with the pucherite that United States Patent (USP) (US-4316746) has proposed two kinds, but technology more complicated, mainly show following 2 points: first, because the solvent of dilute alkaline soln (pH=8~14) as precipitation agent adopted in this invention, for avoiding because Bi 3+Ionic hydrolysis and have influence on reaction uniformity, the adding of precipitation agent must be to drip mode slowly in the reaction process.The second, sodium salt and caustic soda have been adopted in this invention, must make Na +Ion enters in the throw out.Because Na +Ionic is residual to be deleterious to pigment performance, so must be through repetitive scrubbing to remove Na after solid-liquid separation +The ionic step.On the other hand, this invention pigment is with BaSO 4As weighting agent, be a kind of simple blending, only play diluting effect, and pigment performance is not had help.
The objective of the invention is to propose a kind of new be the inorganic molybdenum tungsten yellow pigment of matrix with the pucherite so that adopt fairly simple rational production method; Optimize simultaneously pigment performance, particularly hide the weighting agent that performance has good influence.
Inorganic molybdenum tungsten yellow pigment proposed by the invention has following composition:
Bi〔 1-(x+y)/3〕Mo xW yV〔 1-(x+y)〕O 4
Wherein, 0.1≤x+y≤0.35.
The method for making of this yellow pigment is as follows:
Solubility trivalent bismuth salt is dissolved in (molten intact back pH≤1.25) in the salpeter solution, is made into reaction solution.Ammonium meta-vanadate, ammonium molybdate can be dissolved in then in 30~70 ℃ the hot water, and mix mutually, be made into precipitation agent with the ammonium tungstate solution that obtains behind the ammonia decompose tunstite.This precipitation agent is added in the reaction solution, following reaction mainly takes place:
Because these reactions all produce hydrogen ion, the adding of precipitation agent can not cause Bi 3+Local hydrolysis, so can under well-beaten prerequisite, directly precipitation agent be poured in the reaction solution.After this, continue to stir 15~30 minutes, at this moment pH≤0.6.Can acidity be transferred to 1.5≤pH≤3.5 with strong aqua, restir 15~30 minutes, but stopped reaction then.Place suction filtration after 1 hour, in 90~120 ℃ of oven dry down.Then, calcine more than half an hour down, be cooled to room temperature, grind and then obtain molybdenum tungsten yellow pigment product at 450~700 ℃.
Experiment shows that above-mentioned synthesis reaction temperature can be chosen in 5~95 ℃ of scopes, its optimum temps is 25~60 ℃.
Calcination process must carry out in irreducibility atmosphere.Therefore, must keep calcining under the condition of secluding air not, to finish.
For the opacifying power that improves pigment and reduce cost, can in above-mentioned reaction solution, add and contain 1%(weight) following Fe 2O 3Titanium dioxide.After reaction is finished, calcine more than half an hour down at 550 ℃.The add-on of this kind titanium dioxide can be chosen below (weight) in 4 times of amounts of pigment.
The present invention is owing to adopt hot water to make the solvent of precipitation agent, and adjusts reaction solution acidity with strong aqua, not only can be with in the direct impouring reaction solution of precipitation agent, and saved the remaining NH of flush away 4NO 3Step (NH 4NO 3The time can decompose and influence the performance of product in calcining) thus the synthetic cycle shortened.
The present invention is because the titanium dioxide of introducing contains a small amount of ferric iron, can reduce cost simultaneously and to have significantly improved the opacifying power of pigment under to the very little situation of the influence of paint color saturation ratio.
Inorganic its predominant wavelength of molybdenum tungsten yellow pigment of making according to aforesaid method can be made by lemon yellow tandem product to middle Huang under the condition that changes x, y value etc. between 573~590nm.The colorimetric purity of these pigment series product can reach 83.96%; Producing the primrose yellow pigmenting power with Japan is 100%, and its tinting strength is 60~80g/m 2
Molybdenum tungsten yellow pigment so that aforesaid method is made is applicable to coloring plastics such as polyolefins.Its color, light fastness are good.This pigment is applicable to that also preparation various coating and paraffin wax product are painted.
Embodiment 1.Bi (0.9)Mo (0.3)V (0.7)O 4Synthetic
The HNO that in the beaker of a 3000ml, adds 2N 3300ml takes by weighing five water Bismuth trinitrate 62.1g and is dissolved in wherein, adds 800ml water mixing then and promptly gets reaction solution.Take by weighing ammonium meta-vanadate 11.6g, ammonium molybdate 7.53g joins in the 1200ml water, and 50 ℃ of heating down, stirring makes it dissolving and makes precipitation agent.Stir and record pH=0.55 after 15 minutes, regulate acidity to pH=2.0 with strong aqua, continuation is stirred then to react after 15 minutes and is stopped.Place the question response mixeding liquid temperature and reduce to room temperature, the supernatant liquid that inclines, suction filtration, oven dry is pulverized, and calcines 1 hour down at 600 ℃, naturally cools to room temperature, grinds the pigment that promptly gets x=0.3.
Colo(u)rant dispersion in acrylic latex, is coated on the plotting paper, measures its colourimetric number following (light source is a standard light source) with AUD-CH-1 type colour examining colour-difference-metre:
X Y Z λD P% L a b
69.33????76.24????11.20????574.1????81.4????89.97????-11.39????91.55
Embodiment 2. pigment consist of Bi (0.9)Mo (0.15)W (0.15)U (0.7)O 4(this titanium dioxide contains 0.81% Fe to add 1 times titanium dioxide 2O 3).
Calculate batching according to this color chemistry formula and form, add 45g titanium dioxide in reaction solution, 550 ℃ of calcinings, other step is with embodiment 1 after the reaction.
The pigment colourimetric number that obtain this moment is as follows:
X Y Z λD P% L
69.02????74.52????16.27????574.74????73.0????89.16
a b
Figure 85100779_IMG1
-8.55????78.06
Annotate, colourimetric number parameter meaning: X, Y, Z are tristimulus values; L*, a*, b* are CIE1976 colorimeter system metric system lightness (L*) and metric system colourity (a*, b*);
Figure 85100779_IMG2
Be predominant wavelength (nm); P%, excitation purity (saturation ratio that is equivalent to color).

Claims (2)

1, a kind of inorganic molybdenum tungsten yellow pigment that is made of elements such as vanadium, molybdenum, tungsten, bismuth, oxygen is characterized in that to consist of:
Bi[1-(x+y)/3]MoxWyV1-(x+y)O 4
The material of (wherein x, y value can be chosen in the scope of 0.1≤x+y≤0.35) is a main ingredient, contains the following Fe of 1% (weight) with this substance weight below 4 times 2O 3Titanium dioxide be weighting agent.
2, a kind of making method with inorganic molybdenum tungsten yellow pigment of claim 1 composition is characterized in that:
2.1 solubility trivalent bismuth salt is dissolved in salpeter solution, makes the reaction solution of pH≤1.25.
2.2 ammonium meta-vanadate, ammonium molybdate are dissolved in 30~70 ℃ of hot water, are mixed and made into precipitation agent with ammonium tungstate solution.
2.3 under fully stirring directly with precipitation agent impouring reaction solution in, and with strong aqua conditioned reaction acidity in 1.5≤pH≤3.5, continue to stir 15~30 minutes, place back suction filtration, oven dry, and promptly obtained said pigment principal constituent in the claim 1 in 30 minutes 450~700 ℃ of calcinings.
CN 85100779 1985-04-01 1985-04-01 Mfr. of an inorganic mo-w yellow dye Expired CN1008374B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN 85100779 CN1008374B (en) 1985-04-01 1985-04-01 Mfr. of an inorganic mo-w yellow dye

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN 85100779 CN1008374B (en) 1985-04-01 1985-04-01 Mfr. of an inorganic mo-w yellow dye

Publications (2)

Publication Number Publication Date
CN85100779A CN85100779A (en) 1986-08-20
CN1008374B true CN1008374B (en) 1990-06-13

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Family Applications (1)

Application Number Title Priority Date Filing Date
CN 85100779 Expired CN1008374B (en) 1985-04-01 1985-04-01 Mfr. of an inorganic mo-w yellow dye

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Families Citing this family (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101914310B (en) * 2010-07-21 2013-11-20 株洲冶炼集团股份有限公司 Environmental-friendly pigment bismuth yellow and production method thereof
CN107629483B (en) * 2017-08-04 2020-08-18 佛山市力合通新材料有限公司 Preparation method of doped nano bismuth vanadate yellow pigment

Also Published As

Publication number Publication date
CN85100779A (en) 1986-08-20

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