CN102515876B - Resin acid titanium-iron-bismuth system yellow-series electro-optic water and preparation method thereof - Google Patents
Resin acid titanium-iron-bismuth system yellow-series electro-optic water and preparation method thereof Download PDFInfo
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Abstract
The invention relates to resin acid titanium-iron-bismuth system yellow-series electro-optic water and a preparation method thereof. The electro-optic water is characterized in that: titanium, iron and bismuth are taken as coloring elements; the electro-optic water comprises the following components in percentage by weight: 3-5 percent of titanium oxide, 25-50 percent of a resin acid titanium solution, 4-5 percent of ferric oxide, 10-25 percent of an iron resinate solution, 4-5 percent of bismuth oxide, 25-35 percent of a bismuth resinate solution and 10-20 percent of a film forming agent; the electro-optic water does not contain any harmful lead or uranium element, so that damages to human bodies and the environment in preparation and subsequent use processes of electro-optic water are eliminated; and in the preparation method, titanium resinate is prepared wet a wet process by reacting an alkoxide of titanium with alcohol rosin, the prepared titanium resinate is uniform and has high ferric oxide content, and the color of electro-optic water is deeper and brighter. By adjusting the content of titanium, iron and bismuth, a series of electro-optic water ranging from lemon yellow to golden brown and having an illusion-color effect can be prepared.
Description
Technical field
The invention belongs to the painted electro-optical water technical field of decorating on the ceramic glaze, be specifically related to a kind of resin acid titanium-iron-bismuth system yellow-series electro-optic water and preparation method thereof.
Background technology
Electro-optical water is liquid decorative material on the ceramic glaze, and it is sprayed on the Ceramic glaze, forms metal or the sull that one deck has strong gloss at Ceramic glaze after the high temperature decoration firing, reaches the purpose of decoration.Electro-optical water is divided into colourless and painted two kinds.Colourless electro-optical water is painted on the ceramic glaze surface, sends extraordinary brilliance after burning till, and the brilliance of nacre or moonlight is arranged.Painted electro-optical water is sent a kind of nacreous pigments by coloring metal.The chromophoric principle of electro-optical water is that resinate decomposes when color roasting, and metal oxide is deposited on the glaze, because bismuth dissolves in the glaze, makes the oxide compound on the glaze show special brilliance.
Color and the light of material are closely related, and it is that material reflects one of physical phenomenon of (or seeing through) to light selecting performance.Various material dialogue reflection of lights are different with absorption, and present distinct colors.At present, the glassy yellow electro-optical water mainly is the coloring element of three kinds of series: coloring element is that chromium is plumbous, coloring element is that uranium and coloring element are cerium, bismuth and vanadium.Coloring element is to have used lead in the plumbous series of chromium, and lead contacts and can be dissolved in to some extent in the food with food for a long time, and meeting affects healthy in the human body when these released ions enter.Coloring element is the yellow electro-optical water of uranium, and uranium element belongs to one of rare elements, and is not only expensive, but also is radioelement, from its production to use, to decorating to porcelain, can affect to surrounding environment again.Coloring element is the yellow electro-optical water of cerium, bismuth and vanadium, because cerium and vanadium are colourless electro-optical water, so coloring element is that the yellow electro-optical water of cerium, bismuth and vanadium can not shinny yellow and be not with illusion-colour.The present invention is directed to the problem that there is not environmental protection of coloring element in current glassy yellow electro-optical water, invent a kind of not leaded and uranium assay and can shinny yellow and with prescription and the preparation technology of the electro-optical water of illusion-colour.
Summary of the invention
The object of the invention provides the preparation method of a kind of environmentally friendly resinous acid ferrotianium bismuth yellow electro-optical water of series and this electro-optical water.
A kind of resin acid titanium-iron-bismuth system yellow-series electro-optic water provided by the invention is characterized in that: take titanium, iron and bismuth as coloring element, the proportioning of electro-optical water is by weight:
Titanium oxide content is 3% ~ 5% resinous acid titanium solution 25% ~ 55%, and iron oxide content is 4% ~ 5% iron resinate solution 10% ~ 20%, and bismuth oxide content is 4% ~ 5% bismuth resinate solution 25% ~ 35%, membrane-forming agent 10% ~ 20%,
Wherein, described resinous acid titanium solution and iron resinate solution are that pimelinketone take mass ratio as 2:1 and turps mixture are as solvent, described bismuth resinate solution is that the common melts heat fused with crystallization bismuth subnitrate and rosin forms in turps, and described membrane-forming agent is formed by rosin and turps modulation; In the proportioning of above-mentioned electro-optical water, each solution oxide thing content is regulated with turps.
The allotment of proportioning can be made from lemon yellow to bright orange serial yellow electro-optical water between above-mentioned electro-optical water take coloring element as the ferrotianium bismuth formed by each, and bright in colour, stable, and with fantasy coloured effect.Used lead in the plumbous bismuth series of chromium, it is healthy that plumbous meeting stripping enters the interior meeting impact of human body, and uranium element has very strong radioactivity in the uranium bismuth series.Yellow electro-optical water series provided by the invention can replace the plumbous bismuth resin salt series of chromium and the yellow electro-optical water of uranium bismuth resin salt series to human body and environmentally friendly.
The present invention also provides a kind of preparation method of resin acid titanium-iron-bismuth system yellow-series electro-optic water, comprise: at first, wet method with the alkoxide of titanium and the reaction of pure rosin solution prepares the resinous acid titanium salt, is dissolved in then that the preparation titanium oxide content is 3% ~ 5% resinous acid titanium solution in pimelinketone and the turps mixture; With FeSO
4The preparation iron oxide content is 4% ~ 5% iron resinate solution in pimelinketone and the turps mixture with being dissolved in behind the rosin acid sodium reaction spanning tree resin acid molysite; Be melted into the crystallization bismuth subnitrate in the rosin of melting, joining in the turps heat fused after solidifying fully, to prepare bismuth oxide content be 4% ~ 5% bismuth resinate solution again; With rosin melting in evaporating dish, splash into turps and be prepared into film; Then, by weight: titanium oxide content is 3% ~ 5% resinous acid titanium solution 25% ~ 55%, iron oxide content is 4% ~ 5% iron resinate solution 10% ~ 20%, bismuth oxide content is 4% ~ 5% bismuth resinate solution 25% ~ 35%, membrane-forming agent 10% ~ 20%, each component is mixed, as electro-optical water soltion viscosity conditioning agent, be mixed with resin acid titanium-iron-bismuth system yellow-series electro-optic water with turps.
The preferred tetra-n-butyl titanate of the alkoxide of above-mentioned titanium, pure rosin solution are formulated by dehydrated alcohol and rosin, and described pimelinketone and turps mixture as solvent, the pimelinketone take mass ratio as 2:1 and turps mixture are as best.
Above-mentioned titanium oxide content is that the concrete preparation method of 3% ~ 5% resinous acid titanium solution can be: become pure rosin solution take dehydrated alcohol and rosin as preparation of raw material, slowly splash into again certain tetrabutyl titanate, stir and to solution, the deep yellow precipitation occurs, then, add a certain amount of warm water, leave standstill for some time, the yellow substance that the upper strata is suspended filters, obtains the resinous acid titanium salt, again with the resinous acid titanium salt repetitive scrubbing of warm water with gained, with flush away water-soluble substances wherein, with the resinous acid titanium salt drying for standby after the washing.And then the pimelinketone of measuring 2:1 and turps are some restrains into solvent, take by weighing a certain amount of dried resinous acid titanium salt and are dissolved in the solvent, and stirring and forming the rear oxidation titanium content is 3% ~ 5% resinous acid titanium solution.
Adopt above-mentioned preparation method to obtain environmentally friendly yellow-series electro-optic water, its advantage is:
(1) this preparation method works in coordination take coloring element as the electro-optical water of ferrotianium bismuth and makes lemon yellow to serial yellow electro-optical water such as bright orange grade, and this series is to human body and environmentally friendly;
(2) adopt Liquid preparation methods resinous acid titanium salt.Compare and traditional titanium tetrachloride is directly joined in the rosin of melting, obtained resinous acid titanium salt is more even, and the content of titanium oxide is high, reaches 15.5%;
(3) with resinous acid titanium content modulation color development effect, the yellow electro-optical water of making along with the increase of titanium content in the prescription is with very strong fantasy coloured effect.
Embodiment
Below in conjunction with embodiment, further set forth the present invention.
Resin acid titanium-iron-bismuth system yellow-series electro-optic water provided by the invention and preparation method thereof, its embodiment can be undertaken by following processing step:
(1) preparation of sodium resinate
Get 80 gram colophonium powders, 88 gram NaOK solution (80 gram water, the aqueous solution that 8 gram NaOH are made into), heating is also constantly stirred, and rosin is dissolved fully, pours 800 gram boiling water dilutions into again, makes transparent rosin acid sodium solution.
(2) preparation of resinate solution
1) preparation of resinous acid titanium solution
Get the 400ml dehydrated alcohol and 40 the gram colophonium powders be mixed with pure rosin solution, slowly splash into again the tetra-n-butyl titanate of 15ml, constantly stirring the deep yellow precipitation appears to the solution and after, wash with warm water, leave standstill for some time, the yellow substance that the upper strata is suspended filters, obtains the resinous acid titanium salt, again with the resinous acid titanium salt repetitive scrubbing of warm water with gained, with flush away water-soluble substances wherein, with the resinous acid titanium salt drying for standby after the washing.And then the pimelinketone of measuring 2:1 and turps are some restrains into solvent, and taking by weighing in proportion a certain amount of dried resinous acid titanium salt, to be dissolved in the rear sinking that stirs in the solvent for subsequent use.
2) preparation of iron resinate solution
Take by weighing a certain amount of FeSO
4The water-soluble FeSO that makes
4The aqueous solution is then with FeSO
4The aqueous solution dropwise drips in the rosin acid sodium solution, constantly stir, to the rosin acid sodium pH be about 7, stop titration, dry after the precipitation with warm water washing gained.Then add pimelinketone and the turps solvent melt into iron resinate solution of 2:1, sinking is for subsequent use.
3) preparation of bismuth resinate solution
Take by weighing crystallization bismuth subnitrate 10 grams, rosin 30 grams.With rosin melting in evaporating dish, under constantly stirring, Bismuth trinitrate is slowly added first.Each amount that adds can not be too many, after current sub-fraction is melted fully, continues to add another part, until till adding.When melts becomes brown, stopped heating.After it solidified fully, the turps that adds again 60 grams was heated fusing, namely obtains bismuth resinate solution.
(3) preparation of membrane-forming agent
Take by weighing each 50 gram of rosin and turps, first with rosin melting in evaporating dish, under constantly stirring, slowly splash into turps, make membrane-forming agent.
(4) electro-optical water preparation
Measure resinous acid titanium solution, iron resinate solution, bismuth resinate solution and membrane-forming agent by described proportioning, fully stir, as electro-optical water soltion viscosity conditioning agent, be mixed with the electro-optical water solution of certain titanium oxide, ferric oxide and bismuth oxide content with turps.
Embodiment one
(1) resinous acid titanium solution, iron resinate solution, the preparation of bismuth resinate solution and membrane-forming agent
Have as described embodiment and prepare the resinous acid titanium solution, iron resinate solution, bismuth resinate solution and membrane-forming agent.Be modulated into turps: titanium oxide content is 3.3% resinous acid titanium solution, and iron oxide content is 4.2% iron resinate solution, and bismuth oxide content is 4.2% bismuth resinate solution, and the rosin solid content is 50% membrane-forming agent.
(2) apply
The electro-optical water prescription forms (wt%): titanium oxide content is 3.3% resinous acid titanium solution 29%, and iron oxide content is 4.2% iron resinate solution 18%, and bismuth oxide content is 4.2% bismuth resinate solution 35%, and the content of rosin is 50% membrane-forming agent 18%.With its mixing and stir and make liquid electro-optical water, then the electro-optical water solution for preparing is coated to uniformly on the porcelain dish after the glaze firing drying.
(3) color roasting
The temperature rise rate that is raised to 400 ℃ from room temperature is 10 ℃/min, and will note the strong oxidation of ventilating.Then be 8 ℃/min from 400 ℃ to 820 ℃ temperature rise rate, at 820 ℃ of insulation 10min.
(4) colour generation
The color on porcelain dish surface is lemon yellow after the color roasting, and with illusion-colour.
Embodiment two
(1) resinous acid titanium solution, iron resinate solution, the preparation of bismuth resinate solution and membrane-forming agent
Have as described embodiment and prepare the resinous acid titanium solution, iron resinate solution, bismuth resinate solution and membrane-forming agent.Be modulated into turps, iron oxide content is 4.2% iron resinate solution, and bismuth oxide content is 4.2% bismuth resinate solution, and the rosin solid content is 50% membrane-forming agent.
(2) apply
The electro-optical water prescription forms (wt%): titanium oxide content is 3.3% resinous acid titanium solution 45%, and iron oxide content is 4.2% iron resinate solution 13%, and bismuth oxide content is 4.2% bismuth resinate solution 29%, and the content of rosin is 50% membrane-forming agent 13%.Above-mentioned resin solution mixed make liquid electro-optical water, then the electro-optical water for preparing is coated to uniformly on the porcelain dish after the glaze firing drying.
(3) color roasting
The temperature rise rate that is raised to 400 ℃ from room temperature is 10 ℃/min, and will note the strong oxidation of ventilating.Then be 8 ℃/min from 400 ℃ to 820 ℃ temperature rise rate, at 820 ℃ of insulation 10min.
(4) colour generation
The color on porcelain dish surface is that chrysanthemum is yellow after the color roasting, and with illusion-colour.
Embodiment three
(1) resinous acid titanium solution, iron resinate solution, the preparation of bismuth resinate solution and membrane-forming agent
Have as described embodiment and prepare the resinous acid titanium solution, iron resinate solution, bismuth resinate solution and membrane-forming agent.Be modulated into turps: titanium oxide content is 3.3% resinous acid titanium solution, and iron oxide content is 4.2% iron resinate solution, and bismuth oxide content is 4.2% bismuth resinate solution, and the rosin solid content is 50% membrane-forming agent.
(2) apply
The electro-optical water prescription forms (wt%): titanium oxide content is 3.3% resinous acid titanium solution 39%, and iron oxide content is 4.2% iron resinate solution 13%, and bismuth oxide content is 4.2% bismuth resinate solution 35%, and the content of rosin is 50% membrane-forming agent 13%.Above-mentioned resin solution mixed make liquid electro-optical water, electro-optical water is left standstill for some time, then the electro-optical water for preparing is coated to uniformly on the porcelain dish after the glaze firing drying.
(3) color roasting
The temperature rise rate that is raised to 400 ℃ from room temperature is 10 ℃/min, and will note the strong oxidation of ventilating.Then be 8 ℃/min from 400 ℃ to 820 ℃ temperature rise rate, at 820 ℃ of insulation 10min.
(4) colour generation
The color on porcelain dish surface is orange after the color roasting, and with illusion-colour.
Embodiment four
(1) resinous acid titanium solution, iron resinate solution, the preparation of bismuth resinate solution and membrane-forming agent
Have as described embodiment and prepare the resinous acid titanium solution, iron resinate solution, bismuth resinate solution and membrane-forming agent.Be modulated into turps: titanium oxide content is 3.3% resinous acid titanium solution, and iron oxide content is 4.2% iron resinate solution, and bismuth oxide content is 4.2% bismuth resinate solution, and the rosin solid content is 50% membrane-forming agent.
(2) apply
The electro-optical water prescription forms (wt%): titanium oxide content is 3.3% resinous acid titanium solution 40%, and iron oxide content is 4.2% iron resinate solution 20%, and bismuth oxide content is 4.2% bismuth resinate solution 25%, and the content of rosin is 50% membrane-forming agent 15%.Above-mentioned resin solution mixed make liquid electro-optical water, electro-optical water is left standstill for some time, then the electro-optical water for preparing is coated to uniformly on the porcelain dish after the glaze firing drying.
(3) color roasting
The temperature rise rate that is raised to 400 ℃ from room temperature is 10 ℃/min, and will note the strong oxidation of ventilating.Then be 8 ℃/min from 400 ℃ to 820 ℃ temperature rise rate, at 820 ℃ of insulation 10min.
(5) colour generation
The color on porcelain dish surface is shallow bright orange after the color roasting, and with illusion-colour.
Embodiment five
(1) resinous acid titanium solution, iron resinate solution, the preparation of bismuth resinate solution and membrane-forming agent
Have as described embodiment and prepare the resinous acid titanium solution, iron resinate solution, bismuth resinate solution and membrane-forming agent.Be modulated into turps: titanium oxide content is 3.3% resinous acid titanium solution, and iron oxide content is 4.2% iron resinate solution, and bismuth oxide content is 4.2% bismuth resinate solution, and the rosin solid content is 50% membrane-forming agent.
(2) apply
The electro-optical water prescription forms (wt%): titanium oxide content is 3.3% resinous acid titanium solution 40%, and iron oxide content is 4.2% iron resinate solution 25%, and bismuth oxide content is 4.2% bismuth resinate solution 25%, and the content of rosin is 50% membrane-forming agent 10%.Above-mentioned resin solution mixed make liquid electro-optical water, electro-optical water is left standstill for some time, then the electro-optical water for preparing is coated to uniformly on the porcelain dish after the glaze firing drying.
(3) color roasting
The temperature rise rate that is raised to 400 ℃ from room temperature is 10 ℃/min, and will note the strong oxidation of ventilating.Then be 8 ℃/min from 400 ℃ to 820 ℃ temperature rise rate, at 820 ℃ of insulation 10min.
(6) colour generation
The color on porcelain dish surface is golden yellow after the color roasting, and with illusion-colour.
Claims (2)
1. the preparation method of a resin acid titanium-iron-bismuth system yellow-series electro-optic water, the proportioning of described resin acid titanium-iron-bismuth system yellow-series electro-optic water is by weight:
Titanium oxide content is 3% ~ 5% resinous acid titanium solution 25% ~ 50%, and iron oxide content is 4% ~ 5% iron resinate solution 10% ~ 25%, and bismuth oxide content is 4% ~ 5% bismuth resinate solution 25% ~ 35%, membrane-forming agent 10% ~ 20%,
It is characterized in that: at first, prepare the resinous acid titanium salt with the alkoxide of titanium and pure rosin solution reaction wet method, be dissolved in then that the preparation titanium oxide content is 3% ~ 5% resinous acid titanium solution in pimelinketone and the turps mixture; With FeSO
4The preparation iron oxide content is 4% ~ 5% iron resinate solution in pimelinketone and the turps mixture with being dissolved in behind the rosin acid sodium reaction spanning tree resin acid molysite; Be melted into the crystallization bismuth subnitrate in the rosin of melting, joining in the turps heat fused after solidifying fully, to prepare bismuth oxide content be 4% ~ 5% bismuth resinate solution again; With rosin melting in evaporating dish, splash into turps and be prepared into film; Then, by weight: titanium oxide content is 3% ~ 5% resinous acid titanium solution 25% ~ 55%, and iron oxide content is 4% ~ 5% iron resinate solution 10% ~ 20%, and bismuth oxide content is 4% ~ 5% bismuth resinate solution 25% ~ 35%, membrane-forming agent 10% ~ 20%; Aforementioned each component is mixed, as electro-optical water soltion viscosity conditioning agent, be mixed with resin acid titanium-iron-bismuth system yellow-series electro-optic water with turps; The alkoxide of described titanium is tetra-n-butyl titanate, and pure rosin solution is formulated by dehydrated alcohol and rosin, and pimelinketone and terebinthine mass ratio are 2:1.
2. the preparation method of described resin acid titanium-iron-bismuth system yellow-series electro-optic water according to claim 1, it is characterized in that: described titanium oxide content is that the preparation method of 3% ~ 5% resinous acid titanium solution is: become pure rosin solution take dehydrated alcohol and rosin as preparation of raw material, slowly splash into again certain tetrabutyl titanate, stir and to solution, the deep yellow precipitation occurs, then, add a certain amount of warm water, leave standstill for some time, the yellow substance that the upper strata is suspended filters, obtain the resinous acid titanium salt, again with the resinous acid titanium salt repetitive scrubbing of warm water with gained, with flush away water-soluble substances wherein, with the resinous acid titanium salt drying for standby after the washing; And then the pimelinketone of measuring 2:1 and turps are some restrains into solvent, take by weighing a certain amount of dried resinous acid titanium salt and are dissolved in the solvent, and stirring and forming the rear oxidation titanium content is 3% ~ 5% resinous acid titanium solution.
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| CN102976789B (en) * | 2012-12-25 | 2015-01-14 | 景德镇陶瓷学院 | Green liquid luster |
| CN112794736B (en) * | 2021-04-09 | 2021-08-10 | 蒙娜丽莎集团股份有限公司 | Ceramic plate with colorful cloud surface decoration effect and preparation method thereof |
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