CN85108554A - The manufacture method of jadeite-green pigment - Google Patents
The manufacture method of jadeite-green pigment Download PDFInfo
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- CN85108554A CN85108554A CN 85108554 CN85108554A CN85108554A CN 85108554 A CN85108554 A CN 85108554A CN 85108554 CN85108554 CN 85108554 CN 85108554 A CN85108554 A CN 85108554A CN 85108554 A CN85108554 A CN 85108554A
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Abstract
The present invention relates to a kind of and natural jadeite jadeite homeomorphism, consist of Na
1-xLi
xCrSi
2O
6The manufacture method of the jadeite-green pigment of (x=0～1).The present invention is that the material that can produce chromic oxide, Lithium Oxide 98min, sodium oxide and silicon-dioxide obtains jadeite-green pigment with addition of carbon containing reducer through roasting.This method technology is simple, and production cost is lower than chromoxide green.Can be used for enamel, artistic pottery and porcelain, architectural pottery, colored stone rice, stained glass, colored ornamental slab for paving the floor, building coating, also can be used for aspects such as domestic ceramics, paint, plastics, tone is better than chromoxide green.
Description
The present invention relates to a kind of and natural jadeite jadeite homeomorphism, consist of Na
1-XLi
XCrSi
2The manufacture method of jadeite-green pigment O6(X=1～0).
With natural jadeite homeomorphism, consist of Na
1-XLi
XCrSi
2O
6Emerald green pigment, just began one's study in nearly ten years, still be in the development phase at present, go back the unified title of none.At first being called " universe is green ", is because this pigment is at first found at meteoritic abundance.Thereafter being called " You Leishi ", is the in honor of Nobelist, the outstanding thunder of aerolite scholar.The chemist generally is named according to its chemical constitution, but only to name with its chemical constitution be the feature that is difficult to reflect this kind pigment to a kind of pigment.The present invention considers this point just, notices again simultaneously to consist of Na
1-XLi
XCrSi
2O
6The pigment of (X=0～1) and natural jadeite homeomorphism have than the color as the more pleasant emerald of chromoxide green, so be named as emerald green.
Jadeite-green pigment mainly contains dry method and two kinds of manufacturing process of wet method at present, the invention belongs to dry process.Problems such as though the dry process flow process that adopts is simple at present, exists the furnace charge sintering, and reaction is incomplete, and the chromium utilization ratio is low, and color and luster is dark green.As Soviet Union inventor certificate 412144 and 676551, and the invention that provided of United States Patent (USP) 3692735, all there is this class problem.Someone these problems of attempting be situated between to determine propose as European patent 14408, and overcoming above-mentioned shortcoming, but effect is not very good by double roasting.
The present invention aims to provide and a kind ofly can keep the simple advantage of dry process, can overcome the above-mentioned shortcoming that dry process exists again, obtains the manufacture method of quality jade phthalocyanine.
The present invention is the material that can produce chromic oxide, Lithium Oxide 98min, sodium oxide and silicon-dioxide, at least by the stoichiometric ratio mixing, and with addition of carbon containing reducer, charging at a certain temperature, being warming up to maturing temperature then rapidly, to carry out roasting synthetic, the synthetics chilling consists of Na after fine grinding or through embathing dry back fine grinding or not embathing after wet-milling drying again obtains and natural jadeite homeomorphism
1-XLi
XCrSi
2O
6The jadeite-green pigment that ten minutes is liked is made us in (X=0～1), color and luster.
The said material and the carbonaceous material that can produce chromic oxide, silicon oxide, sodium oxide, Lithium Oxide 98min of the present invention, for example, sodium dichromate, lithium dichromate, ammonium dichromate, Sodium chromate, lithium chromate, ammonium chromate, yellow soda ash, Quilonum Retard, chromium trioxide, silicate, quartz, silica gel, white carbon black, gac, charcoal, wood chip, starch, rosin etc. all can be as the raw material and the reductive agents of synthetic emerald phthalocyanine.For example, with sodium dichromate, quartz and gac; Or with chromic anhydride, quartz (or silica gel) and Quilonum Retard, rosin; Or sodium dichromate, quartz, junket acid anhydride, Quilonum Retard and starch is mixed in proportion roasting, all can synthesize the ideal jadeite-green pigment.For the requirement of these raw materials is should not bring into or should not produce water-soluble salt or other detrimental impurity in synthetic.As the quartz of siliceous material, dioxide-containing silica should not be lower than 98%.
The material of above-mentioned various synthetic emerald phthalocyanines will mix by the stoichiometric ratio of resultant at least, and silicon is suitably excessive can to improve the chromium utilization ratio, and the mol ratio of general Si/Cr is 2.0～2.3 best.Reductive agent can be before batch mixing or during batch mixing or behind the batch mixing with addition of, be generally 30～350% moles of theoretical amount, preferably 50～300% of theoretical amount moles.
Analyze from the mechanism of building-up reactions, find, be more conducive to the carrying out that react in charging more than 350 ℃, but the sintering phenomenon of basically eliminate furnace charge.It is considered herein that reactant all can obtain comparatively ideal results 350～800 ℃ of chargings, and 450～650 ℃ is the optimum temps of charging.Certainly the present invention also is not precluded within the possibility of room temperature charging.More progressively be warming up to synthesis reaction temperature and be rapidly heated to the result of synthesis reaction temperature, the quality product that obtains of finding to be rapidly heated is better than the product that progressively intensification obtains.High temperature charging and be rapidly heated to combine and improve the quality of jadeite-green pigment significantly.
The said maturing temperature of the present invention is synthesis reaction temperature.The maturing temperature of jadeite-green pigment is with Na
1-XLi
XCrSi
2O
6The variation of the X value in (X=0～1) and changing.For X=0, maturing temperature is 800～1060 ℃, and optimum temps is 900～1000 ℃; For X=1, maturing temperature is 950～1350 ℃, and optimum temps is 1000～1200 ℃.For 0＜X＜1, maturing temperature is at 850～1350 ℃, and optimum temps is 950～1200 ℃.Maturing temperature raises with the increase of X value.
Because NaCrSi
2O
6With LiCrSi
2O
6Can be partly molten mutually, the value of X is preferably in the scope of 0＜X≤0.2 and 0.7≤X＜1.
Roasting time was at least two hours, generally was no more than 6 hours, can reach the optimum response effect in 3～4 hours.
The granularity and the mixing situation of employed various raw materials of synthetic emerald phthalocyanine and reductive agent, not only influence speed of response, and influence productive rate and quality product, especially when using quartz as silicon-containing material, the influence of its granularity is more obvious, and the silica powder particle diameter is to be advisable less than 74 μ.The granularity of other raw material such as sodium dichromate, Quilonum Retard, chromium trioxide, charcoal, starch etc. is little to the reaction influence, but their particle diameter must be less than 150 μ.The abundant mixing of material, favourable to building-up reactions.When use contains the raw material of crystal water, too not fierce when batch mixing as two water dichromic acids, in case the separating out of crystal water, thereby cause the material caking.The material caking is quite deleterious to such solid phase synthesis.Have been found that if give elder generation and dry the crystal water of removing in the starting material, thorough mixing then is beneficial to building-up reactions then.
The present invention had both kept dry process flow process characteristic of simple, had avoided the sintering of furnace charge again, thereby reaction is carried out fully, the pigment tone that obtains is pure, gives happy sense, and is catchy, do not have the sort of dark green sense of chromoxide green, price is well below chromoxide green pigment.
The jadeite-green pigment that the present invention makes, be mainly used in aspects such as enamel, artistic pottery and porcelain, architectural pottery, colored stone rice, stained glass, colored ornamental slab for paving the floor, building coating, also can be used for domestic ceramics, paint, plastics, clear boiled soap and produce aspects such as hybrid pigment.If require the Cr of pigment in actual applications
6+When content is the PPm level, then can adopts and embathe after the roasting or the methods such as wet-milling of product of roasting reach service requirements.
Example 1
56 parts of industrial sodium dichromates, 45 parts of silica powders, with addition of 125% the gac that is theoretical amount, with raw material in 100 ℃ of bakings 12 hours, grinding in ball grinder 30 minutes, roasting in retort furnace, is crossed 320 mesh sieves at chilling, corase grind, fine grinding after the roasting.Product does the X-ray material phase analysis and examination is measured and used to spectral reflectivity.
Example 2
Claim sample with example 1, with addition of 50% the starch that is theoretical amount, following steps are with example 1.
Example 3
Claim sample with example 1, with addition of 160% the wood chip that is theoretical amount, following steps are with example 1.
Example 4
Claim sample with example 1, with addition of 200% the wood chip that is theoretical amount, following steps are with example 1.
Example 5
Take by weighing 89.5 parts of industrial sodium dichromates, 81 parts of silica powders, 25 parts of Quilonum Retards, 10.1 parts of chromic anhydrides, with addition of 200% the wood chip that is theoretical amount, following steps are with example 1.
Example 6
Take by weighing 80 parts of industrial chromic anhydrides, 15 parts of Quilonum Retards, 96 parts of silica powders, with addition of 50% rosin of theoretical amount, following steps are with example 1.
The reaction conditions of above-mentioned example and the results are shown in Table 1.
Claims (8)
1, a kind of Na that consists of
1-xLi
xCrSi
2O
6The manufacture method of the jadeite-green pigment of (x=0～1), be to produce chromic oxide, Lithium Oxide 98min, the material of sodium oxide and silicon-dioxide, at least by the stoichiometric ratio mixing, through roasting, burned material fine grinding or embathe dry back fine grinding or do not embathe after wet-milling dry again, it is characterized in that before above-mentioned reaction mass mixing or during mixing or behind the mixing with addition of 30% the carbon containing reducer that is no less than theoretical amount, reaction mass enters stoving oven under greater than 350 ℃, and temperature is risen to 800～1350 ℃ rapidly and carry out roasting, roasting time is no less than 2 hours, and material is chilled to room temperature after the roasting.
2, in accordance with the method for claim 1, it is characterized in that said carbon containing reducer is gac, charcoal, wood chip, starch, rosin etc.
3, in accordance with the method for claim 1, it is characterized in that said carbon containing reducer can be before batch mixing or during batch mixing or behind the batch mixing with addition of, add-on is 30～350% of a theoretical amount, optimal addn is 50～300% of a theoretical amount.
4, in accordance with the method for claim 1, it is characterized in that the Si/Cr mol ratio is preferably 2.0～2.3 in the stoichiometric ratio of said reaction mass.
5, in accordance with the method for claim 1, it is characterized in that said reaction mass feeding temperature is 350～800 ℃, best feeding temperature is 450～650 ℃.
6, in accordance with the method for claim 1, it is characterized in that said reaction mass 350～800 ℃ enter stoving oven after, be rapidly heated to 800～1350 ℃.
7, in accordance with the method for claim 1, it is characterized in that said maturing temperature, should be 800～1060 ℃ for the reaction mass of X=0, optimum calcination temperature is 900～1000 ℃; Reaction mass for X=1 should be 950～1350 ℃, and optimum calcination temperature is 1000～1200 ℃; For the reaction mass of 0＜X＜1, maturing temperature should be 850～1350 ℃, and optimum calcination temperature is 950～1200 ℃.
8, in accordance with the method for claim 1, it is characterized in that said roasting time is 2～6 hours, best roasting time is 3～4 hours.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN85108554A CN85108554B (en) | 1985-11-25 | 1985-11-25 | Preparation of producing jadeite-green pigment |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN85108554A CN85108554B (en) | 1985-11-25 | 1985-11-25 | Preparation of producing jadeite-green pigment |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN85108554A true CN85108554A (en) | 1987-06-17 |
| CN85108554B CN85108554B (en) | 1987-10-14 |
Family
ID=4796071
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN85108554A Expired CN85108554B (en) | 1985-11-25 | 1985-11-25 | Preparation of producing jadeite-green pigment |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN85108554B (en) |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100410335C (en) * | 2005-12-21 | 2008-08-13 | 浙江大学 | Green porous solid pigment synthesis |
| CN106185835A (en) * | 2016-06-30 | 2016-12-07 | 中南大学 | A kind of method using starch low-temperature reduction to prepare sodium sulfide |
Families Citing this family (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102942168B (en) * | 2012-11-30 | 2014-09-17 | 苏州大学 | Phosphate inorganic material, method for producing same and application |
-
1985
- 1985-11-25 CN CN85108554A patent/CN85108554B/en not_active Expired
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100410335C (en) * | 2005-12-21 | 2008-08-13 | 浙江大学 | Green porous solid pigment synthesis |
| CN106185835A (en) * | 2016-06-30 | 2016-12-07 | 中南大学 | A kind of method using starch low-temperature reduction to prepare sodium sulfide |
Also Published As
| Publication number | Publication date |
|---|---|
| CN85108554B (en) | 1987-10-14 |
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