CN105037227A - Preparation method of silver mercapto compound - Google Patents
Preparation method of silver mercapto compound Download PDFInfo
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- CN105037227A CN105037227A CN201510204155.1A CN201510204155A CN105037227A CN 105037227 A CN105037227 A CN 105037227A CN 201510204155 A CN201510204155 A CN 201510204155A CN 105037227 A CN105037227 A CN 105037227A
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- silver
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- sulfhydryl compound
- mercapto compound
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Abstract
The invention provides a preparation method of a silver mercapto compound, wherein the method includes the following steps: (A) performing a continuous reaction to Venetian turpentine and sulfur for 4-6 h at 160-170 DEG C, allowing the mixture to stand and adding cyclohexanone to prepare sulfurized venetian turpentine; and (B) adding the sulfurized venetian turpentine prepared in the step (A) to a solution which is formed by silver carbonate and dichloromethane with stirring, and then stirring the mixed solution and adding ethanol, wherein the white oily silver resinate is instantly changed into a light-brown color, and separating the silver resinate and washing the silver resinate in distilled water to obtain the silver mercapto compound. The silver mercapto compound can be used as solvent in lavendin oil, lavender oil, turpentine, terpilenol, rosemary oil and other essential oils. A decorative component containing the novel silver resin hydrochloride can be melted when being used for decorating a base material, such as glass, and can maintain an excellent stickiness even at a low temperature.
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
We know that the mixture of the compound of organic silver and gold possesses decorative effect, such as relative to the product only having gold, can form different colours by its mixture, and be not only gold on glass and ceramic base material goods.In mixture, the ratio difference of silver can make different colours, from partially golden, to glassy yellow, and lemon yellow, even partially green.If in mixture not argentiferous time, color effects is partially red.
Due to the electrical conductor that silver is good, by assigning it as a kind of pigment, and being heated to very high temperature, the good conductive film of sticking power can be formed on insulating substrate.
For reaching above effect, silver is added in formula in different forms.Such as: argent (fine grinding), organic salt or inorganic salt, be dissolved in the silver compound in organic solvent.
Manufacturers employ silver-colored sulfhydryl compound in the 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 the sulphurated derivatives of natural resin.Such as: resinoid, sesquiterpene, sobrerone etc.These natural resins, because be not synthesis, can well can not define product because its stability is different, a defect can affect whole component and their use.
From trialkyl mercaptan, found a kind of silver-colored thiolate, can replace before use silver compound and more advanced.Both for decorating the preparation with conducting stratum surface.
According to invention, new thiolate general formula is as follows: 2,3,3,4,4,5-hexamethyl-2-hexane mercaptan, this compound comprises 12 carbon atoms.Silver thiolate is reacted by silver salt to be prepared.As silver-colored nitrate or carbonate, insert as in water or organic water solvent, especially in aqueous ethanolic solution, come together to prepare with the tert-alkyl thiol mentioned in the preceding formulations of same dosage.Solution after the reaction obtained completes can be selected, so that silver-colored thiolate obtains from organic solvent or organic solvent mixed solution, and water insoluble.The silver-colored thiolate that this mode obtains can be directly used in the preparation of decoration formula.
The precipitation solvent of silver thiolate comprises, and especially low-carbon alcohol is as methyl alcohol and ethanol, ketone as acetone, and about the mixture of water.
Be applicable to dissolving the solvent of new thiolate and comprise stable hydrocarbon as pimelinketone and its alkyl derivative, aromatic hydrocarbon is benzene hydrocarbon especially, as benzene, toluene, ethylbenzene, chlorine, azepine derivatives as trichloromethane, chlorobenzene and pyridine
New silver-colored vitriol is highly stable, can be dissolved in a variety of organic solvent for the decoration component containing silver compound.They be also applied to conductivity silver layer preparation in.In fact, the commercial mixture obtaining thiolate from tert-alkyl thiol is applicable.This molecule providing package is containing a large amount of thiolate containing 12 carbon atoms.Due to they good solubilities in all kinds of SOLVENTS, new compound can allow them enter in the preparation of same attribute component more easily, has more advantage than levigate dispersion silver compound
New silver-colored thiolate alkyl is lower than the decomposition temperature of known silver-colored mercaptan resin, it can be made to be applied on low-melting material, such as glass.
As everyone knows, the component for decorating in this product comprises solvent, gloss oil, resin.In fact, can comprise in the component of decorating the organic gold compound be dissolved in organic solvent.
Summary of the invention
Technical problem to be solved by this invention is to provide a kind of method preparing silver-colored sulfhydryl compound, 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 sulfhydryl compound.
Preferably, the mass content of sulphur is 7-15%.
Present invention also offers the method that another prepares silver-colored sulfhydryl compound, 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 sulfhydryl compound.
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 sulfhydryl compound 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 a kind of silver-colored sulfhydryl compound, general formula is as follows: 2,3,3,4,4,5-hexamethyl-2-hexane mercaptan.
Preferably, silver-colored thiolate alkyl comprises 12 carbon atoms altogether.
Present invention also offers the method for the silver-colored sulfhydryl compound 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 sulfhydryl compound.
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 sulfhydryl compound 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 sulfhydryl compound precipitates can be allowed to comprise low-carbon alcohol, as methyl alcohol and ethanol.
Novel silver sulfhydryl compound 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 sulfhydryl compound.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.
The silver-colored sulfhydryl compound obtained in the present invention, can than the more widespread use mentioned in the past, and as turps, Oleum lavandula angustifolia, lavender spike oil, Rosmarinus officinalis has and other volatile oil.Normally used solubility promoter in early stage component, natural is compatible with synthetic resins and this new type resin.The application method of component is brushing spraying or silk screen printing.
Belonging to the present invention, for pottery or glass centralized procurement surface provide the method containing silver coating to be by applying new sulfo-resinate separately on substrate surface, as previously mentioned, by base material heating to certain temperature, as 580-850 DEG C, like this can substrate surface formed one deck tool sticking and containing silver coating.
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, argentiferous 32WT%, dissolves in hexanaphthene, chloroform, dimethylbenzene, chlorobenzene, oil of mirbane, turps and rosemary oil.
Embodiment 5
In 200 grams of tert-dodecyl mercaptans and 200 grams of cyclohexanone solution, stir and add the Silver Nitrate that 170 grams are dissolved in 350CC distilled water.Whole process approximately continues 5 minutes, and temperature rises to 40 DEG C by 20 DEG C of degree.After arrest reaction several minutes, the tert-dodecyl mercaptan of silver forms precipitation in cyclohexanone solution.Then be separated, and clean with distilled water.The silver of 20WT% can be obtained.
The silver-colored sulfhydryl compound 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 (4)
1. a silver-colored sulfhydryl compound, is characterized in that, general formula is as follows: 2,3,3,4,4,5-hexamethyl-2-hexane mercaptan.
2. as right 1 requires the silver-colored sulfhydryl compound as described in 1, it is characterized in that, silver-colored thiolate alkyl comprises 12 carbon atoms.
3. prepare a method for silver-colored sulfhydryl compound, it is characterized in that, 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 sulfhydryl compound.
4. as claim 3 prepares the method for silver-colored sulfhydryl compound, it is characterized in that, described steps A " in, the temperature in dropping process is 10 DEG C to 20 DEG C.
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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 Pending CN105037227A (en) | 2014-05-16 | 2014-05-16 | Preparation method of silver mercapto compound |
| CN201510158180.0A Pending CN104861871A (en) | 2014-05-16 | 2014-05-16 | Preparation method for silver sulphoresinate |
| CN201410208988.0A Active CN104031557B (en) | 2014-05-16 | 2014-05-16 | A kind of preparation method of silver-colored sulfo-resinate |
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| CN201410208988.0A Active CN104031557B (en) | 2014-05-16 | 2014-05-16 | A kind of preparation method of silver-colored sulfo-resinate |
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN1531577A (en) * | 2000-10-13 | 2004-09-22 | �����ɷ� | Noble metal preparation and use thereof for production of noble metal decorations by means of direct and indirect printing |
Family Cites Families (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 |
| 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 |
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2014
- 2014-05-16 CN CN201510204155.1A patent/CN105037227A/en active Pending
- 2014-05-16 CN CN201510158180.0A patent/CN104861871A/en active Pending
- 2014-05-16 CN CN201410208988.0A patent/CN104031557B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| CN1531577A (en) * | 2000-10-13 | 2004-09-22 | �����ɷ� | Noble metal preparation and use thereof for production of noble metal decorations by means of direct and indirect printing |
Non-Patent Citations (1)
| Title |
|---|
| 上海进出口商品检验局: "《进出口商品检验方法 化工原料及化工产品分册》", 30 September 1996, 上海科学普及出版社 * |
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| CN104031557A (en) | 2014-09-10 |
| CN104031557B (en) | 2015-07-29 |
| CN104861871A (en) | 2015-08-26 |
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