CN104031557B - A kind of preparation method of silver-colored sulfo-resinate - Google Patents
A kind of preparation method of silver-colored sulfo-resinate Download PDFInfo
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- CN104031557B CN104031557B CN201410208988.0A CN201410208988A CN104031557B CN 104031557 B CN104031557 B CN 104031557B CN 201410208988 A CN201410208988 A CN 201410208988A CN 104031557 B CN104031557 B CN 104031557B
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Abstract
The invention provides a kind of preparation method of silver-colored sulfo-resinate, comprise following step: steps A: by Venice turpentine and sulphur successive reaction 4-6 hour, temperature of reaction is 160-170 DEG C, adds pimelinketone, obtain sulfuration Venice turpentine after leaving standstill; Step B: stir the sulfuration Venice turpentine adding described steps A and obtain in the solution that silver carbonate and methylene dichloride are formed, after having added, ethanol is added after stirring, the silver resin hydrochlorate of the white oil formed becomes light brown immediately, then be separated, and with distilled water cleaning, obtain silver-colored sulfo-resinate.The silver-colored sulfo-resinate that the present invention obtains, what can be used as solvent has lavandin oil, Oleum lavandula angustifolia, turps, Terpineol 350, rosemary oil and other volatile oil.Decoration component containing Novel silver resinate as melted at relatively low temperature during glass baseplate, and still has good viscosity at Dicoration base material.
Description
Technical field
The present invention relates to the material used in the noble metal preparation production process for the purpose of ceramic decoration, particularly Novel silver sulfo-resinate--the preparation method of sulfhydryl compound.
Background technology
Describe containing the noble metal preparation of golden sulfo-resinate is existing in known references for the purpose of decoration, such as Boudnikoff, Compt. rend., 196,1898 (1933), and Chemnitius, J. Prakt. Chem. 117,245 (1927). the preparation of golden sulfo-resinate has been reacted by the face cream of gold perchloride and sulfur-bearing or natural resin.
The U.S. Patent number write at Zsigmondy for the purpose of ceramic decoration, containing the noble metal preparation of the organic compound of gold and silver-colored sulphur is 682, the Sprechsaal that the patent of 310 and Chemnitius write, 60, be described in 313 (1927).Noble metal preparation containing silver (existence form of silver is silver-colored sulfo-resinate) is by natural product such as rosin ester, rosin derivative, the preparations such as face cream, and its characteristic in component also can change because of the difference of the add-on of the place of production of natural resin, temperature, time and sulphur to some extent.This change may cause the work-ing life of our unpredictable precious metal lotion, and the mobility aspect of precious metal lotion also may can have unforeseen feature simultaneously.
In addition, the Combination of specific silver-colored sulfo-resinate has limitation in a lot of containing in the preparation of precious metal, which limit the usefulness the selection of solvent and the using dosage of silver.Further, the baking temperature that the component containing silver-colored sulfo-resinate requires when ceramic surface bakes is relatively high, and the Ag films that will obtain light after therefore baking is impossible.
The mixture of silver and gold can form decorative effect on ceramic base material (glass, porcelain) surface.The effect color presented after roasting changes according to proportion difference silver-colored in metal mixture.Color after curing can from partially red to partially yellow or lemon yellow, when in mixture not argentiferous time, color effects is partially red, and when the ratio of Yin Bijin is higher, color presents partially yellow or lemon yellow.
Finally, because silver is good electric conductor, therefore conductive film can be formed on insulating substrate.Manufacturers have employed specific silver-colored sulfo-resinate in the noble metal component for decorative porcelain and glass.The preparation of these sulfo-resinates is realized by the reaction of the inorganic silver in the mixture of sulfuration natural derivative, at high temperature by heating natural resin mixture and sulphur, and obtains after the chemical reaction of a few hours.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of method preparing silver-colored sulfo-resinate, comprises following step:
Steps A: by Venice turpentine and sulphur successive reaction 4-6 hour, temperature of reaction is 160-170 DEG C, adds pimelinketone, obtain sulfuration Venice turpentine after leaving standstill;
Step B: stir the sulfuration Venice turpentine adding described steps A and obtain in the solution that silver carbonate and methylene dichloride are formed, after having added, ethanol is added after stirring, the silver resin hydrochlorate of the white oil formed becomes light brown immediately, then be separated, and with distilled water cleaning, obtain silver-colored sulfo-resinate.
Preferably, the mass content of sulphur is 7-15%.
Present invention also offers the method that another prepares silver-colored sulfo-resinate, comprise following step:
Steps A ': in the solution that sulfuration Cuba balm, pimelinketone and dimethylbenzene are formed, drip silver acetate, and temperature rises to 100 DEG C, stirs;
Step B': after leaving standstill, the solution obtained is divided into two-layer, and lower floor is the silver resin acid salt solution being dissolved in dimethylbenzene/pimelinketone, is separated, and with distilled water cleaning, obtains silver-colored sulfo-resinate.
Preferably, the temperature in step B' is 10 DEG C to 20 DEG C.
The present invention adopts above technical scheme, and its advantage is, tamarack or Venice turpentine deposit successive reaction several hours in case at sulphur, and temperature of reaction is 160-170 DEG C, and the content of sulphur should reach 7-15%.The preparation of this silver-colored sulfo-resinate is obtained as silver carbonate reacts under temperature is the environment of 10 DEG C to 20 DEG C with the sulfuration tamarack of equivalent amount or Venice turpentine in inorganic solvent especially methylene dichloride by the salt of silver.
Present invention also offers the method for the silver-colored sulfo-resinate of preparation in addition, comprise following step:
Steps A ": Silver Nitrate is dissolved in dehydrated alcohol and distilled water, then drips the solution formed by tert-dodecyl mercaptan and dehydrated alcohol;
Step B ": obtain partially yellow oily tert-dodecyl mercaptan, be separated and with distilled water cleaning, obtain silver-colored sulfo-resinate.
Preferably, steps A " in, the temperature in dropping process is 10 DEG C to 20 DEG C.
Have been found that the special silver-colored sulfo-resinate coming from tamarack or Venice turpentine advantageously can substitute the compound of the silver previously found, for ceramic decoration.
In addition, the compound using thiol synthesis salt and silver in the formulation is also possible.The organic thinner being applicable to new thiolate comprises benzene hydrocarbon, as toluene and dimethylbenzene.The solvent that silver-colored sulfo-resinate precipitates can be allowed to comprise low-carbon alcohol, as methyl alcohol and ethanol.
Novel silver sulfo-resinate is a highly stable product, and silver content very high (>60 %), is dissolved in a large amount of organic solvent, and the decoration component of the compound usually containing silver can use Novel silver sulfo-resinate.Because silver content is high, the mixture being mixed with golden sulfhydryl compound can present the metal film coatings with lemon yellow after ceramic substrate surface bakes.
The decomposition temperature of Novel silver resinate is lower relative to silver-colored thiolate, is described about this point embodiment in the present invention.In addition, the variation of color and the enhancing of tinting strength may be realized completely by these sulfo-resinates.Further advantage is, the decoration component containing Novel silver resinate as melted at relatively low temperature during glass baseplate, and still has good viscosity at Dicoration base material.
Embodiment
Below preferably embodiment of the present invention is described in further detail: embodiment 1
1998 grams of Venice turpentines and 324 grams of sulphur, in a reservoir with 162 DEG C of heating 4 hours, add pimelinketone afterwards and make its gross weight reach 4048 grams.By analysis, in the finished product, the content of sulphur is 7.3%, obtains sulfuration Venice turpentine.
Embodiment 2
Toward 48 grams of silver carbonates and 70CC(milliliter) the solution that formed of methylene dichloride in stir and add 70 grams of sulfuration Venice turpentines obtained by embodiment 1, experimental temperature controls lower than 20 DEG C.After having added, stir one hour.Finally, the ethanol of 210CC is added.The silver resin hydrochlorate of the white oil formed becomes light brown immediately, is then separated, and cleans with distilled water.It can be dissolved in hexanaphthene, chloroform, benzene,toluene,xylene, mono chloro benzene, oil of mirbane, eucalyptol, terpinol, turps and rosemary oil, and obtaining containing weight concentration is the silver of 39%.
Embodiment 3
Stir in the solution that 101 grams of sulfuration Cuba balms and 50 grams of pimelinketone, 25 grams of dimethylbenzene are formed and add 25 grams of silver acetates (content of silver is 64.6 %).Be added in 5 minutes and complete, and service temperature is risen to 100 DEG C.After 5 minutes, solution becomes two-layer, and wherein one deck is the silver resin acid salt solution being dissolved in dimethylbenzene/pimelinketone.Then be separated, and clean with distilled water, after tested, the mass percent of silver is 20%.
Embodiment 4
Stir in the solution that 58 grams of tert-dodecyl mercaptans and 120CC dehydrated alcohol are formed add be dissolved in 43 grams of Silver Nitrates of 100CC dehydrated alcohol and 100CC distilled water after the solution that formed.Drip and completed in five minutes.Temperature in dropping process should be 20 DEG C or lower than 20 DEG C.Partially yellow oily tert-dodecyl mercaptan is separated and cleans with distilled water.The oily matter obtained weighs 84 grams, and argentiferous 32 WT%, dissolves in hexanaphthene, chloroform, dimethylbenzene, chlorobenzene, oil of mirbane, turps and rosemary oil.
The silver-colored sulfo-resinate that the present invention obtains, what can be used as solvent has lavandin oil, Oleum lavandula angustifolia, turps, Terpineol 350, rosemary oil and other volatile oil.Normally used fusing assistant in early stage component, natural and synthetic resins and this new type resin are compatible.The application method of component is brushing or silk screen printing.For substrate surface provides the method containing gold and silver decoration coating to be by applying new sulfur on substrate surface for resinate, then at one temperature, such as 500-900 DEG C of heating ceramic base materials, will can form one deck tool sticking and containing the coating of gold and silver like this on ceramic base material.
Above content is in conjunction with concrete preferred implementation further description made for the present invention, can not assert that specific embodiment of the invention is confined to these explanations.For general technical staff of the technical field of the invention, without departing from the inventive concept of the premise, some simple deduction or replace can also be made, all should be considered as belonging to protection scope of the present invention.
Claims (2)
1. prepare a method for silver-colored sulfo-resinate, it is characterized in that, comprise following step:
Steps A: by Venice turpentine and sulphur successive reaction 4-6 hour, temperature of reaction is 160-170 DEG C, adds pimelinketone, obtain sulfuration Venice turpentine after leaving standstill;
Step B: stir the sulfuration Venice turpentine adding described steps A and obtain in the solution that silver carbonate and methylene dichloride are formed, after having added, ethanol is added after stirring, the silver resin hydrochlorate of the white oil formed becomes light brown immediately, then be separated, and with distilled water cleaning, obtain silver-colored sulfo-resinate.
2. as claim 1 prepares the method for silver-colored sulfo-resinate, it is characterized in that, the mass content of sulphur is 7-15%.
Priority Applications (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510158180.0A CN104861871A (en) | 2014-05-16 | 2014-05-16 | Preparation method for silver sulphoresinate |
| CN201510204155.1A CN105037227A (en) | 2014-05-16 | 2014-05-16 | Preparation method of silver mercapto compound |
| CN201410208988.0A CN104031557B (en) | 2014-05-16 | 2014-05-16 | A kind of preparation method of silver-colored sulfo-resinate |
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| CN201410208988.0A CN104031557B (en) | 2014-05-16 | 2014-05-16 | A kind of preparation method of silver-colored sulfo-resinate |
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| CN201510204155.1A Division CN105037227A (en) | 2014-05-16 | 2014-05-16 | Preparation method of silver mercapto compound |
| CN201510158180.0A Division CN104861871A (en) | 2014-05-16 | 2014-05-16 | Preparation method for silver sulphoresinate |
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| CN104031557A CN104031557A (en) | 2014-09-10 |
| CN104031557B true CN104031557B (en) | 2015-07-29 |
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| CN201510204155.1A Pending CN105037227A (en) | 2014-05-16 | 2014-05-16 | Preparation method of silver mercapto compound |
| CN201410208988.0A Active CN104031557B (en) | 2014-05-16 | 2014-05-16 | A kind of preparation method of silver-colored sulfo-resinate |
| CN201510158180.0A Pending CN104861871A (en) | 2014-05-16 | 2014-05-16 | Preparation method for silver sulphoresinate |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0486970A1 (en) * | 1990-11-19 | 1992-05-27 | Inax Corporation | Process for producing ceramics having a surface similar to a metal |
| CN1346339A (en) * | 1999-04-09 | 2002-04-24 | W.C.贺利氏股份有限及两合公司 | Bright noble metal preparation |
| CN1242004C (en) * | 2000-10-13 | 2006-02-15 | 费柔股份有限公司 | Noble metal preparation and use thereof for production of noble metal decorations by means of direct and indirect printing |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE19831141C2 (en) * | 1998-07-11 | 2003-02-27 | Dmc2 Degussa Metals Catalysts | Precious metal preparation and its use for the production of precious metal decorations by direct and indirect printing |
| CN101555163A (en) * | 2009-05-13 | 2009-10-14 | 深圳市永丰源实业有限公司 | Noble metal preparation or luster preparation for direct or indirect silk screen printing |
-
2014
- 2014-05-16 CN CN201510204155.1A patent/CN105037227A/en active Pending
- 2014-05-16 CN CN201410208988.0A patent/CN104031557B/en active Active
- 2014-05-16 CN CN201510158180.0A patent/CN104861871A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0486970A1 (en) * | 1990-11-19 | 1992-05-27 | Inax Corporation | Process for producing ceramics having a surface similar to a metal |
| CN1346339A (en) * | 1999-04-09 | 2002-04-24 | W.C.贺利氏股份有限及两合公司 | Bright noble metal preparation |
| CN1242004C (en) * | 2000-10-13 | 2006-02-15 | 费柔股份有限公司 | Noble metal preparation and use thereof for production of noble metal decorations by means of direct and indirect printing |
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| CN105037227A (en) | 2015-11-11 |
| CN104861871A (en) | 2015-08-26 |
| CN104031557A (en) | 2014-09-10 |
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Address after: 518000 Two Yongfengyuan Industrial Zone, Huanguannan South Road, Guanlan Town, Baoan District, Shenzhen City, Guangdong Province Patentee after: Shenzhen Guoci Yongfengyuan Co.,Ltd. Address before: 518000 Two Yongfengyuan Industrial Zone, Huanguannan South Road, Guanlan Town, Baoan District, Shenzhen City, Guangdong Province Patentee before: CHINA YONGFENGYUAN Co.,Ltd. |
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