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CN100372795C - Reduction preparation for silver mirror - Google Patents

Reduction preparation for silver mirror Download PDF

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Publication number
CN100372795C
CN100372795C CNB2005100723143A CN200510072314A CN100372795C CN 100372795 C CN100372795 C CN 100372795C CN B2005100723143 A CNB2005100723143 A CN B2005100723143A CN 200510072314 A CN200510072314 A CN 200510072314A CN 100372795 C CN100372795 C CN 100372795C
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parts
sodium
silver mirror
silver
tensio
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CN1686888A (en
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梁中生
杨晨
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QINHUANGDAO GLASS INDUSTRY RESEARCH AND DESIGN INST
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QINHUANGDAO GLASS INDUSTRY RESEARCH AND DESIGN INST
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Abstract

The present invention relates to a reduction preparation for silver mirrors. Sorbierite, mannitol, hydroxylamine sulfate and/or benzaldehyde are used as reducing agents for silver mirror, and ammonia, potassium sodium tartrate, urea and/or oxalic acid are added to serve as complexing agents. The present invention is characterized in that meglumine is added to serve as reinforcing agents, and surface active agents are added, wherein the surface active agents are sodium dodecylbenzene sulfonate and/or sodium dodecanesulphonate.

Description

A kind of reduction preparation for silver mirror
Technical field
The present invention relates to a kind of reduction preparation for silver mirror, and relate to said preparation forms silver mirror at glass surface method.
Background technology
Mirror is indispensable articles for daily use during people live.Silver mirror reaction is the ultimate principle at silver-plated system mirror on glass, at first is to add ammoniacal liquor to generate clear look silver ammonia coordination ion [Ag (NH in silver nitrate solution 3) 2] +, the ammonia solution of the Silver Nitrate of Xing Chenging is called as Duolun (Tollens) reagent like this.Toillen's reagent and aldehydes or aldose reaction, silver ions is reduced into argent.
Senior silver mirror comes from the America and Europe of the fifties, and the Suo Maka company representative of Krupp, gondola blog article company and the U.S. of Germany the highest level of the senior silver mirror production unit in the world today.Reflectivity height, the color and luster degree of senior silver mirror is good, imaging clear, even film layer true to nature firmly, the back of the body coats with lacquer, simple to operate when producing, production rate is fast, product specification is big, possesses the superiority that the aluminium mirror can not be compared, and is subjected to the very big welcome in current market.
From the beginning of the nineties so far, China introduces tens of silver mirror production lines from countries such as Germany, Italy, the U.S., tens of the production lines that China develops voluntarily are the maximum countries of silver mirror production line in the world, employed silver mirror reduction agent of these production lines and the most dependence on import of back of the body lacquer.
Domestic early stage reduction preparation for silver mirror, the transformation efficiency of silver has only 20~30%, and manufacturer generally uses state's moral products such as Germany, the U.S., Japan.Played the inventor in 1996 and begin to develop reduction preparation for silver mirror,, develop a kind of reduction preparation for silver mirror through research and test in a few years.Reduction preparation for silver mirror of the present invention has substituted glucose, sucrose with sorbyl alcohol, N.F,USP MANNITOL, and has added phenol, Resorcinol, Periodic acid as toughener, selects for use Sodium dodecylbenzene sulfonate as tensio-active agent, and the transformation efficiency of silver is brought up to more than 75%.
Summary of the invention
The invention provides a kind of reduction preparation for silver mirror, it uses sorbyl alcohol, N.F,USP MANNITOL, oxammonium sulfate and/or phenyl aldehyde as the silver mirror reduction agent, except that ammoniacal liquor, also add Seignette salt, urea and/or oxalic acid as complexing agent, it is characterized in that adding meglumine is toughener, preferably use phenol, Resorcinol, Periodic acid and meglumine to be toughener simultaneously, and added tensio-active agent in addition, wherein tensio-active agent is Sodium dodecylbenzene sulfonate and/or sodium laurylsulfonate, the preferred Sodium dodecylbenzene sulfonate of tensio-active agent.
The preferred reduction preparation for silver mirror of the present invention, its component is: reductive agent: 0~50 part of sorbyl alcohol, 0~50 part in N.F,USP MANNITOL, 0~2 part of oxammonium sulfate, 0~2 part of phenyl aldehyde; Complexing agent: 0~1 part of Seignette salt, 0~4 part in urea, 0~4 part of oxalic acid, 5~10 parts of ammoniacal liquor; Toughener: 2~6 parts of phenol, 1~5 part of Resorcinol, 2~6 parts of Periodic acid, 1~5 part of meglumine; Tensio-active agent: 2~8 parts of Sodium dodecylbenzene sulfonatees, 2~5 parts of sodium laurylsulfonates; 40~60 parts of deionized waters, and use 0~20 part in sodium hydroxide, potassium hydroxide to provide alkaline environment for 0~20 part part be weight part wherein, and wherein sodium hydroxide and potassium hydroxide can not be zero simultaneously, N.F,USP MANNITOL and sorbyl alcohol can not be zero simultaneously.
The preferred reduction preparation for silver mirror of the present invention, its component is: reductive agent: 20~30 parts of sorbyl alcohols, 10~20 parts in N.F,USP MANNITOL, 0~2 part of oxammonium sulfate, 0~2 part of phenyl aldehyde; Complexing agent: 0~1 part of Seignette salt, 0~4 part in urea, 0~4 part of oxalic acid, 5~10 parts of ammoniacal liquor; Toughener: 2~6 parts of phenol, 1~5 part of Resorcinol, 2~6 parts of Periodic acid, 2~4 parts of meglumines; Tensio-active agent: 2~8 parts of Sodium dodecylbenzene sulfonatees, 2~5 parts of sodium laurylsulfonates; 40~60 parts of deionized waters, and use 0~20 part in sodium hydroxide, potassium hydroxide to provide alkaline environment for 0~20 part part be weight part wherein, and wherein sodium hydroxide and potassium hydroxide can not be zero simultaneously, N.F,USP MANNITOL and sorbyl alcohol can not be zero simultaneously.
The most preferred reduction preparation for silver mirror of the present invention, its component is: reductive agent: 20 parts of sorbyl alcohols, 20 parts in N.F,USP MANNITOL, 1 part of oxammonium sulfate, 1 part of phenyl aldehyde; Complexing agent: 0.5 part of Seignette salt, 2 parts in urea, 4 parts of oxalic acid, 8 parts of ammoniacal liquor; Toughener: 4 parts of phenol, 2 parts of Resorcinol, 4 parts of Periodic acid, 3 parts of meglumines; Tensio-active agent: 5 parts of Sodium dodecylbenzene sulfonatees, 4 parts of sodium laurylsulfonates; 45 parts of deionized waters, and use 15 parts in sodium hydroxide, potassium hydroxide to provide alkaline environment for 5 parts, wherein part is a weight part.
The invention still further relates to a kind of method of using reduction preparation for silver mirror of the present invention to prepare silver mirror; comprise said components is mixed; obtain silver mirror reduction agent of the present invention; with 15 times of reductive agent dilutions; itself and 1: 1 by volume ratio of silver ammino solution evenly are sprayed at glass surface clean and the process sensitization simultaneously; left standstill 2~3 minutes; it is fully reacted; water washes glass surface then; termination reaction and flush away reaction residue promptly form one deck silverskin, plate one deck copper film on silverskin again; spray protective paint, make silver mirror.
The invention has the advantages that:
1. speed of response is fast, and it is evenly firm to make silver film thickness in 2~3 minutes, the silver mirror of reflectivity more than 85%;
2. Yin transformation efficiency is brought up to more than 75% by 20~30% of domestic early stage prescription.Be used for automatization silver mirror production line or manual preparation silver mirror, satisfy processing parameter fully, quality product reaches the GB requirement.
Embodiment:
Embodiment 1:
With 20 parts of sorbyl alcohols, 20 parts in N.F,USP MANNITOL, 1 part of oxammonium sulfate, 1 part of phenyl aldehyde, 0.5 part of Seignette salt, 2 parts in urea, 4 parts of oxalic acid, 15 parts in sodium hydroxide, 5 parts in potassium hydroxide, 6 parts of ammoniacal liquor, 45 parts of deionized waters, 4 parts of toughener phenol, 2 parts of Resorcinol, 4 parts of Periodic acid, 3 parts of meglumines, 5 parts of tensio-active agent Sodium dodecylbenzene sulfonatees, 4 parts of sodium laurylsulfonates, mix, fully reaction makes reductant solution, get 15 times of 10 milliliters of dilutions, itself and 1: 1 by volume ratio of silver ammino solution are sprayed on glass surface clean and the process sensitization simultaneously, left standstill 2~3 minutes, it is fully reacted, water washes glass surface then, termination reaction, and flush away reaction residue, the silver film thickness that makes silver mirror is 918mg/m 2, the transformation efficiency of silver is 85%, the silver mirror reflectivity is 90.9%.
Embodiment 2:
With 25 parts of sorbyl alcohols, 15 parts in N.F,USP MANNITOL, 1 part of oxammonium sulfate, 1 part of phenyl aldehyde, 0.5 part of Seignette salt, 1 part in urea, 2 parts of oxalic acid, 20 parts in sodium hydroxide, 8 parts of ammoniacal liquor, 40 parts of deionized waters, 4 parts of toughener phenol, 4 parts of Resorcinol, 2 parts of Periodic acid, 2 parts of meglumines, 4 parts of tensio-active agent Sodium dodecylbenzene sulfonatees, 3 parts of sodium laurylsulfonates mix, and fully reaction makes reductant solution.Get 15 times of 10 milliliters of dilutions, itself and 1: 1 by volume ratio of silver ammino solution are sprayed on glass surface clean and the process sensitization simultaneously, left standstill 2~3 minutes, it is fully reacted, water washes glass surface then, termination reaction, and flush away reaction residue, the silver film thickness that makes silver mirror is 885.6mg/m 2, the transformation efficiency of silver is 82%, the silver mirror reflectivity is 89.9%.
Embodiment 3:
With 30 parts of sorbyl alcohols, 10 parts in N.F,USP MANNITOL, 1 part of oxammonium sulfate, 1 part of phenyl aldehyde, 0.5 part of Seignette salt, 2 parts in urea, 4 parts of oxalic acid, 15 parts in sodium hydroxide, 5 parts in potassium hydroxide, 6 parts of ammoniacal liquor, 45 parts of deionized waters, 4 parts of toughener phenol, 2 parts of Resorcinol, 4 parts of Periodic acid, 3 parts of meglumines, 4 parts of tensio-active agent Sodium dodecylbenzene sulfonatees, 2 parts of sodium laurylsulfonates mix, and fully reaction makes reductant solution.Get 15 times of 10 milliliters of dilutions, itself and 1: 1 by volume ratio of silver ammino solution are sprayed on glass surface clean and the process sensitization simultaneously, left standstill 2~3 minutes, it is fully reacted, water washes glass surface then, termination reaction, and flush away reaction residue, the silver film thickness that makes silver mirror is 864 mg/m 2, the transformation efficiency of silver is 80%, the silver mirror reflectivity is 89.5%.
Embodiment 4:
With 30 parts of sorbyl alcohols, 2 parts of oxammonium sulfates, 2 parts in urea, 20 parts in potassium hydroxide, 6 parts of ammoniacal liquor, 40 parts of deionized waters, 4 parts of phenol, 5 parts of meglumines, 2 parts of sodium laurylsulfonates mix, and fully reaction makes reductant solution.Get 15 times of 10 milliliters of dilutions, itself and 1: 1 by volume ratio of silver ammino solution are sprayed on glass surface clean and the process sensitization simultaneously, left standstill 2~3 minutes, it is fully reacted, water washes glass surface then, termination reaction, and flush away reaction residue, the silver film thickness that makes silver mirror is 853.2 mg/m 2, the transformation efficiency of silver is 79%, the silver mirror reflectivity is 88.5%.
Embodiment 5:
With 30 parts in N.F,USP MANNITOL, 2 parts of phenyl aldehydes, 4 parts of oxalic acid, 20 parts in sodium hydroxide, 5 parts of ammoniacal liquor, 50 parts of deionized waters, 4 parts of Resorcinol, 5 parts of meglumines, 2 parts of tensio-active agent Sodium dodecylbenzene sulfonatees mix, and fully reaction makes reductant solution.Get 15 times of 10 milliliters of dilutions, itself and 1: 1 by volume ratio of silver ammino solution are sprayed on glass surface clean and the process sensitization simultaneously, left standstill 2~3 minutes, it is fully reacted, water washes glass surface then, termination reaction, and flush away reaction residue, the silver film thickness that makes silver mirror is 874.8 mg/m 2, the transformation efficiency of silver is 81%, the silver mirror reflectivity is 85.7%.
The comparative example 1:
With 15 parts of sorbyl alcohols, 15 parts in N.F,USP MANNITOL, 1 part of Seignette salt, 20 parts in sodium hydroxide, 5 parts of ammoniacal liquor, 45 parts of deionized waters, 5 parts of toughener Periodic acid, 2 parts of tensio-active agent Sodium dodecylbenzene sulfonatees mix, and fully reaction makes reductant solution.Get 15 times of 10 milliliters of dilutions, itself and 1: 1 by volume ratio of silver ammino solution are sprayed on glass surface clean and the process sensitization simultaneously, left standstill 2~3 minutes, it is fully reacted, water washes glass surface then, termination reaction, and flush away reaction residue, the silver film thickness that makes silver mirror is 810 mg/m 2, the transformation efficiency of silver is 75%, the silver mirror reflectivity is 88.6%.
Do not use the toughener meglumine among the comparative example 1, the transformation efficiency of silver is lower.
The comparative example 2:
The inventor also discloses a kind of reduction preparation for silver mirror on December 29th, 1999 in the application of the CN1301882A that State Intellectual Property Office submits to, its transformation efficiency is lower.Wherein: with 2 parts of glucose, 2 parts of sorbyl alcohols, 2 parts in N.F,USP MANNITOL, 0.1 part of Resorcinol, 0.1 part of phenol, 0.01 part of oxammonium sulfate, 0.05 part of aubepine, 0.5 part of pyrogallol, 0.3 part in urea, 0.01 part of oxalic acid, 2 parts in sodium hydroxide, 0.3 part of ammoniacal liquor, deionized water mixes for 100 parts, fully reaction makes reduction preparation, be sprayed on glass surface clean and the process sensitization simultaneously with 1: 1 by volume ratio of silver ammino solution, left standstill 1~2 minute, it is fully reacted, water washes glass surface then, termination reaction, and the flush away reaction residue, the silver film thickness that makes silver mirror is 788 mg/m 2, the transformation efficiency of silver is 73%, the silver mirror reflectivity is 90.9%.
The invention belongs to improvement,, further improved the transformation efficiency of silver in the silver mirror preparation unexpectedly, effectively reduce production cost, and reduced the discharging of heavy metal silver wherein by adding tensio-active agent to above-mentioned application.
Though the present invention specifies and describes that those skilled in the art are to be understood that: under the prerequisite of not leaving the described spirit and scope of claim of the present invention, can make various changes to form of the present invention and details.

Claims (7)

1. reduction preparation for silver mirror, its main ingredient is reductive agent, complexing agent, toughener and tensio-active agent, wherein reductive agent is: sorbyl alcohol, N.F,USP MANNITOL, oxammonium sulfate and/or phenyl aldehyde; Complexing agent is: be made up of A and B, A is an ammoniacal liquor, and B is Seignette salt, urea and/or oxalic acid; Toughener is: (1) phenol and Portugal's first ammonia, (2) Resorcinol and meglumine or (3) phenol, Resorcinol, Periodic acid and Portugal's first ammonia; Tensio-active agent is: Sodium dodecylbenzene sulfonate and/or sodium laurylsulfonate.
2. the described reduction preparation for silver mirror of claim 1, wherein toughener is phenol, Resorcinol, Periodic acid and meglumine.
3. claim 1 or 2 described reduction preparation for silver mirror, wherein tensio-active agent is Sodium dodecylbenzene sulfonate and/or sodium laurylsulfonate.
4. any described reduction preparation among the claim 1-2, its component is: reductive agent: 0~50 part of sorbyl alcohol, 0~50 part in N.F,USP MANNITOL, 0~2 part of oxammonium sulfate, 0~2 part of phenyl aldehyde; Complexing agent: 0~1 part of Seignette salt, 0~4 part in urea, 0~4 part of oxalic acid, 5~10 parts of ammoniacal liquor; Toughener: 2~6 parts of phenol, 1~5 part of Resorcinol, 2~6 parts of Periodic acid, 1~5 part of meglumine; Tensio-active agent: 2~8 parts of Sodium dodecylbenzene sulfonatees, 2~5 parts of sodium laurylsulfonates; 40~60 parts of deionized waters, and use 0~20 part in sodium hydroxide, potassium hydroxide to provide alkaline environment for 0~20 part part be weight part wherein, and wherein sodium hydroxide and potassium hydroxide can not be zero simultaneously, N.F,USP MANNITOL and sorbyl alcohol can not be zero simultaneously.
5. the described reduction preparation for silver mirror of claim 4, its component is: reductive agent: 20~30 parts of sorbyl alcohols, 10~20 parts in N.F,USP MANNITOL, 0~2 part of oxammonium sulfate, 0~2 part of phenyl aldehyde; Complexing agent: 0~1 part of Seignette salt, 0~4 part in urea, 0~4 part of oxalic acid, 5~10 parts of ammoniacal liquor; Toughener: 2~6 parts of phenol, 1~5 part of Resorcinol, 2~6 parts of Periodic acid, 2~4 parts of meglumines; Tensio-active agent: 2~8 parts of Sodium dodecylbenzene sulfonatees, 2~5 parts of sodium laurylsulfonates; 40~60 parts of deionized waters, and use 0~20 part in sodium hydroxide, potassium hydroxide to provide alkaline environment for 0~20 part part be weight part wherein, and wherein sodium hydroxide and potassium hydroxide can not be zero simultaneously, N.F,USP MANNITOL and sorbyl alcohol can not be zero simultaneously.
6. the described reduction preparation for silver mirror of claim 4, its component is: reductive agent: 20 parts of sorbyl alcohols, 20 parts in N.F,USP MANNITOL, 1 part of oxammonium sulfate, 1 part of phenyl aldehyde; Complexing agent: 0.5 part of Seignette salt, 2 parts in urea, 4 parts of oxalic acid, 8 parts of ammoniacal liquor; Toughener: 4 parts of phenol, 2 parts of Resorcinol, 4 parts of Periodic acid, 3 parts of meglumines; Tensio-active agent: 5 parts of Sodium dodecylbenzene sulfonatees, 4 parts of sodium laurylsulfonates; 45 parts of deionized waters, and use 15 parts in sodium hydroxide, potassium hydroxide to provide alkaline environment for 5 parts, wherein part is a weight part.
7. method of using any described reduction preparation for silver mirror and silver ammino solution among the claim 1-6 to prepare silver mirror.
CNB2005100723143A 2005-05-30 2005-05-30 Reduction preparation for silver mirror Expired - Fee Related CN100372795C (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106894005B (en) * 2015-12-21 2019-11-22 比亚迪股份有限公司 A kind of chemical bronze plating liquid, preparation method and a kind of method of Chemical Plating of Non metal Material

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1105956A (en) * 1994-01-26 1995-08-02 褚宗文 Production method of silver mirror
CN1301882A (en) * 1999-12-29 2001-07-04 国家建材局秦皇岛玻璃工业研究设计院 Silver mirror reduction preparation
JP2001206735A (en) * 2000-01-25 2001-07-31 Central Glass Co Ltd Plating method
CN1386913A (en) * 2002-03-28 2002-12-25 武汉大学 Brightening agent for cyaniding planting of silver

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1105956A (en) * 1994-01-26 1995-08-02 褚宗文 Production method of silver mirror
CN1301882A (en) * 1999-12-29 2001-07-04 国家建材局秦皇岛玻璃工业研究设计院 Silver mirror reduction preparation
JP2001206735A (en) * 2000-01-25 2001-07-31 Central Glass Co Ltd Plating method
CN1386913A (en) * 2002-03-28 2002-12-25 武汉大学 Brightening agent for cyaniding planting of silver

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