CN106498454A - A kind of preparation method of biomass cyanideless electro-plating liquid - Google Patents

A kind of preparation method of biomass cyanideless electro-plating liquid Download PDF

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Publication number
CN106498454A
CN106498454A CN201610897240.5A CN201610897240A CN106498454A CN 106498454 A CN106498454 A CN 106498454A CN 201610897240 A CN201610897240 A CN 201610897240A CN 106498454 A CN106498454 A CN 106498454A
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filtrate
biomass
liquid
plating liquid
parts
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吴迪
张晶
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吴迪
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    • CCHEMISTRY; METALLURGY
    • C25ELECTROLYTIC OR ELECTROPHORETIC PROCESSES; APPARATUS THEREFOR
    • C25DPROCESSES FOR THE ELECTROLYTIC OR ELECTROPHORETIC PRODUCTION OF COATINGS; ELECTROFORMING; APPARATUS THEREFOR
    • C25D3/00Electroplating: Baths therefor
    • C25D3/02Electroplating: Baths therefor from solutions
    • C25D3/38Electroplating: Baths therefor from solutions of copper

Abstract

The present invention relates to a kind of preparation method of biomass cyanideless electro-plating liquid, belongs to electroplate liquid preparing technical field.The method takes tamarind and ferments through complex enzyme hydrolysis, obtain extracting solution, and stand still for crystals after sodium carbonate reaction, by Fructus Citri Limoniae in the presence of aspergillus niger fermented extracted fermentation liquid, biomass cyanideless electro-plating liquid is obtained final product after fermentation liquid and crystal are mixed to prepare self-control chelating agent, and other raw material compoundings.Obtained plating liquid energy of the invention effectively prevents the displacement phenomenon of steel and iron parts, and the complex mixture bond strength of formation is high, and solution dispersibility and covering power are stronger, solution composition is nontoxic, coating light is careful, current density range width, with splendid application prospect.

Description

A kind of preparation method of biomass cyanideless electro-plating liquid
Technical field
The present invention relates to a kind of preparation method of biomass cyanideless electro-plating liquid, belongs to electroplate liquid preparing technical field.
Background technology
Metallic copper is widely used in electronics and decoration neck with its good electric conductivity, heat conductivity and ductility etc. Domain.Cyanide of traditional cyanide electroplating using severe toxicity, with very big potential safety hazard and environmental pollution, with environmental consciousness Strengthen, prevent cyanide electroplating and also gradually brought into schedule, people are highly desirable the cyanide-free copper electroplating for substituting cyanide electroplating completely The appearance of system.
In order that electrodeposited coating is smooth firmly, in commercial production, the formula of electroplate liquid is often very complicated.Cyanide was commonly used in the past Electroplate liquid is prepared as chelating agent.But as CN- has severe toxicity, the Health cost to electroplater is very big, meanwhile, discharge contains CN- Sewage, waste gas also serious environment pollution.Therefore, plating mainly uses cyanideless electro-plating now.Cyanideless electro-plating is free from the electricity of CN- Plating solution is electroplated.Traditional cyanide copper plating process and bright copper plating technique can be replaced completely, it is adaptable to any metal base:Fine copper, copper On the base materials such as alloy, ferrum, rustless steel, zinc alloy diecasting, aluminum, Al alloy parts, rack plating or barrel plating.Existing electric without cyanogen Plating solution is had a disadvantage that with cyanide electroplating liquid phase ratio:Electric current density is low(0.5~1.0A/dm2), plating solution is unstable, easily hydrolyzes, Cost is higher.
Content of the invention
Present invention mainly solves technical problem:Make chelating agent for the conventional cyanide of electroplate liquid in current commercial production Electroplate liquid is prepared, but due to CN-There is severe toxicity, the health of electroplater can be damaged, given off containing CN-Sewage, waste gas also serious dirty A kind of defect of dye environment, there is provided preparation method of biomass cyanideless electro-plating liquid.The method takes tamarind and sends out through complex enzyme hydrolysis Ferment, obtains extracting solution, and stands still for crystals after sodium carbonate reaction, by Fructus Citri Limoniae in the presence of aspergillus niger fermented extracted fermentation liquid, will Fermentation liquid and crystal obtain final product biomass cyanideless electro-plating liquid after being mixed to prepare self-control chelating agent, and other raw material compoundings.The present invention Obtained plating liquid energy effectively prevents the displacement phenomenon of steel and iron parts, and the complex mixture bond strength of formation is high, and plating solution point Scattered ability and covering power are stronger, and solution composition is nontoxic, and coating light is careful, and current density range width, with splendid Application prospect.
In order to solve above-mentioned technical problem, the technical solution adopted in the present invention is:
(1)Take tamarind to shell to obtain kernel, putting it into 20~30min of grinding in mortar, to obtain tamarind unqualified, and gained is unqualified Be sequentially loaded in ceramic pot with the dehydrated alcohol for waiting mass ratio, stir to obtain pastel, then pastel is added in ceramic pot The compound enzymic preparation of quality 3~5%, described compound enzymic preparation be by Epoxysuccinic acid hydrolytic enzyme, pectase, cellulase and Amylase is mixed to prepare by grade mass ratio;
(2)After above-mentioned enzyme preparation is added and finished, at 30~35 DEG C, 6~8h of insulation enzymolysis, digests after terminating again by ceramic pot Be placed on temperature for 30~40 DEG C, relative air humidity be 60~70% in the environment of naturally mouldy 9~12 days, mistake after mouldy end Isolated filtrate is filtered, then filtrate is centrifuged the isolated supernatants of 10~15min with centrifuge with 3000~4000r/min rotating speeds Liquid;
(3)Supernatant obtained above is put in reactor, is started agitator after being heated to 100~120 DEG C and is stirred Mix, in the state of stirring, add sodium carbonate up to supernatant pH in neutrality, filtrate is evaporated by the isolated filtrate of filtered while hot Be concentrated into its original volume 1/3 obtains concentrated solution, and concentrated solution is placed on 20~30h of standing in 4~6 DEG C of refrigerator makes its nature Crystallization, is filtrated to get crystallization, standby;
(4)Fresh Lemon section is taken, and is 3 in mass ratio:1 will be put in fermentation tank as fermentation after lemon tablet and Radix Glycyrrhizae mixing Substrate, then aspergillus niger is accessed by inoculum concentration in fermentation substrate for 10%, fermentation tank is put into insulation in 30~40 DEG C of calorstats and is sent out Ferment filtered to get filtrate after 12~14 days, puts it into 20~30min of sterilizing in 120~130 DEG C of high-temperature sterilization box, is sterilized Filtrate;
(5)It is 2 in mass ratio:Standby crystallization and above-mentioned sterilizing filtrate are sequentially loaded into three mouthfuls with agitator and thermometer by 5 The Oleum Camelliae of crystallization gross mass 10% in flask, being added, 30~40min being stirred at 50~60 DEG C, discharging obtains final product self-control complexation Agent;
(6)Count by weight, weigh 25~30 parts of curpic carbonate, 100~150 parts of above-mentioned self-control chelating agent, 5~8 parts of bicarbonates Sodium, 0.01~0.03 part of selenium dioxide and 900~1000 parts of deionized waters are sequentially loaded in colloid mill, at 30~40 DEG C with 1000~2000r/min rotating speeds grind 1~2h after discharge, with concentration be 0.5mol/L sodium hydroxide solutions adjust pH to 9.0~ 1.0, biomass cyanideless electro-plating liquid is obtained final product after tinning.
The concrete application method of the present invention:Biomass cyanideless electro-plating liquid obtained in the present invention is heated to 50 first~ Standby after 60 DEG C, then layer alloy substrate to be plated is accessed on the anode of circuit ingredient, make negative electrode with graphite, will connect Metallic matrix immerse to standby electroplate liquid, turn-on current, with 40~50mA/cm2Electric current density, after 2~3h of plating i.e. Can.Obtained plating liquid energy of the invention effectively prevents the displacement phenomenon of steel and iron parts, and the complex mixture bond strength of formation is high, and And solution dispersibility and covering power are stronger, solution composition is nontoxic, and coating light is careful, imitates with splendid plating Really.
The invention has the beneficial effects as follows:
(1)Biomass cyanideless electro-plating liquid energy obtained in of the invention effectively prevents the displacement phenomenon of steel and iron parts, the complexation mixing of formation Thing bond strength is high;
(2), with biological material as raw material, dispersibility and covering power are stronger for biomass cyanideless electro-plating liquid obtained in of the invention, Solution composition is nontoxic, and coating light is careful, with splendid electroplating effect.
Specific embodiment
Take tamarind to shell to obtain kernel, putting it into 20~30min of grinding in mortar, to obtain tamarind unqualified, and gained is unqualified Be sequentially loaded in ceramic pot with the dehydrated alcohol for waiting mass ratio, stir to obtain pastel, then pastel is added in ceramic pot The compound enzymic preparation of quality 3~5%, described compound enzymic preparation be by Epoxysuccinic acid hydrolytic enzyme, pectase, cellulase and Amylase is mixed to prepare by grade mass ratio;After above-mentioned enzyme preparation is added and is finished, 6~8h of insulation enzymolysis, enzyme at 30~35 DEG C Solution terminate after again by ceramic pot be placed on temperature for 30~40 DEG C, relative air humidity be 60~70% in the environment of naturally mouldy 9~ 12 days, be separated by filtration after mouldy end and obtain filtrate, then by filtrate with centrifuge with 3000~4000r/min rotating speeds centrifugation 10~ The isolated supernatant of 15min;Supernatant obtained above is put in reactor, is started after being heated to 100~120 DEG C Agitator is stirred, and adds sodium carbonate until supernatant pH is in neutrality, the isolated filter of filtered while hot in the state of stirring Liquid, obtains concentrated solution by the 1/3 of filtrate evaporation and concentration to its original volume, concentrated solution is placed in 4~6 DEG C of refrigerator and stands 20 ~30h makes its spontaneous nucleation, is filtrated to get crystallization, standby;Fresh Lemon section is taken, and is 3 in mass ratio:1 by lemon tablet and Be put into as fermentation substrate in fermentation tank after Radix Glycyrrhizae mixing, then aspergillus niger accessed for 10% by inoculum concentration in fermentation substrate, will send out Fermentation tank is put into heat-preservation fermentation in 30~40 DEG C of calorstats and filters to get filtrate after 12~14 days, puts it into 120~130 DEG C of high temperature Sterilize in sterilization tank 20~30min, obtains the filtrate that sterilizes;It is 2 in mass ratio:5 crystallize standby with above-mentioned sterilizing filtrate successively Load in the there-necked flask with agitator and thermometer, add the Oleum Camelliae of crystallization gross mass 10%, stir at 50~60 DEG C 30~40min is mixed, discharging obtains final product self-control chelating agent;Count by weight, weigh 25~30 parts of curpic carbonate, 100~150 parts above-mentioned Self-control chelating agent, 5~8 parts of sodium bicarbonate, 0.01~0.03 part of selenium dioxide and 900~1000 parts of deionized waters are sequentially loaded into glue In body mill, discharge after 1~2h being ground with 1000~2000r/min rotating speeds at 30~40 DEG C, be 0.5mol/L hydrogen-oxygens with concentration Change sodium solution and adjust pH to 9.0~1.0, after tinning, obtain final product biomass cyanideless electro-plating liquid.
Example 1
Take tamarind to shell to obtain kernel, putting it into grinding 20min in mortar, to obtain tamarind unqualified, by unqualified for gained and etc. quality The dehydrated alcohol of ratio is sequentially loaded in ceramic pot, and stir to obtain pastel, then adds pastel quality 3% in ceramic pot Compound enzymic preparation, described compound enzymic preparation be by Epoxysuccinic acid hydrolytic enzyme, pectase, cellulase and amylase by etc. matter Amount ratio is mixed to prepare;After above-mentioned enzyme preparation is added and finished, ceramic pot is put after terminating by insulation enzymolysis 6h at 30 DEG C, enzymolysis again Temperature be 30 DEG C, relative air humidity be 60% in the environment of naturally mouldy 9 days, be separated by filtration after mouldy end and obtain filtrate, Filtrate is centrifuged the isolated supernatant of 10min with centrifuge with 3000r/min rotating speeds again;Supernatant obtained above is put into In reactor, start agitator after being heated to 100 DEG C and be stirred, sodium carbonate is added in the state of stirring until supernatant Liquid pH obtains concentrated solution in neutrality, the isolated filtrate of filtered while hot by the 1/3 of filtrate evaporation and concentration to its original volume, will be dense Contracting liquid is placed in 4 DEG C of refrigerator and stands 20h and make its spontaneous nucleation, is filtrated to get crystallization, standby;Fresh Lemon section is taken, and It is 3 in mass ratio:1 will lemon tablet and Radix Glycyrrhizae mixing after be put into as fermentation substrate in fermentation tank, then by inoculum concentration be 10% to send out Aspergillus niger is accessed in ferment substrate, fermentation tank is put into heat-preservation fermentation in 30 DEG C of calorstats and is filtered to get filtrate after 12 days, put it into Sterilize in 120 DEG C of high-temperature sterilization box 20min, obtains the filtrate that sterilizes;It is 2 in mass ratio:Standby crystallization and above-mentioned sterilizing are filtered by 5 Liquid is sequentially loaded in the there-necked flask with agitator and thermometer, adds the Oleum Camelliae of crystallization gross mass 10%, at 50 DEG C Stirring 30min, discharging obtain final product self-control chelating agent;Count by weight, weigh 25 parts of curpic carbonate, 100 parts of above-mentioned self-control chelating agent, 5 parts of sodium bicarbonate, 0.01 part of selenium dioxide and 900 parts of deionized waters are sequentially loaded in colloid mill, with 1000r/min at 30 DEG C Discharge after rotating speed grinding 1h, be that 0.5mol/L sodium hydroxide solutions adjust pH to 9.0 with concentration, biomass are obtained final product after tinning without cyanogen Electroplate liquid.
The concrete application method of the present invention:Biomass cyanideless electro-plating liquid obtained in the present invention is heated to 50 DEG C first Standby afterwards, then layer alloy substrate to be plated is accessed on the anode of circuit ingredient, make negative electrode with graphite, by the gold for connecting During category matrix is immersed to standby electroplate liquid, turn-on current, with 40mA/cm2Electric current density, plating 2h after.Present invention system The plating liquid energy for obtaining effectively prevents the displacement phenomenon of steel and iron parts, and the complex mixture bond strength of formation is high, and plating solution dispersion Ability and covering power are stronger, and solution composition is nontoxic, and coating light is careful, with splendid electroplating effect.
Example 2
Take tamarind to shell to obtain kernel, putting it into grinding 25min in mortar, to obtain tamarind unqualified, by unqualified for gained and etc. quality The dehydrated alcohol of ratio is sequentially loaded in ceramic pot, and stir to obtain pastel, then adds pastel quality 4% in ceramic pot Compound enzymic preparation, described compound enzymic preparation be by Epoxysuccinic acid hydrolytic enzyme, pectase, cellulase and amylase by etc. matter Amount ratio is mixed to prepare;After above-mentioned enzyme preparation is added and finished, ceramic pot is put after terminating by insulation enzymolysis 7h at 33 DEG C, enzymolysis again Temperature be 35 DEG C, relative air humidity be 65% in the environment of naturally mouldy 11 days, be separated by filtration after mouldy end and filtered Liquid, then filtrate is centrifuged the isolated supernatant of 13min with centrifuge with 3500r/min rotating speeds;By supernatant obtained above Be put in reactor, after being heated to 110 DEG C start agitator be stirred, in the state of stirring add sodium carbonate until Supernatant pH obtains concentrated solution in neutrality, the isolated filtrate of filtered while hot by the 1/3 of filtrate evaporation and concentration to its original volume, Concentrated solution is placed on 20~30h of standing in 5 DEG C of refrigerator makes its spontaneous nucleation, is filtrated to get crystallization, standby;Take Fresh Lemon Section, and be 3 in mass ratio:1 will be put into as fermentation substrate in fermentation tank after lemon tablet and Radix Glycyrrhizae mixing, then by inoculum concentration be 10% accesses aspergillus niger in fermentation substrate, fermentation tank is put into heat-preservation fermentation in 35 DEG C of calorstats and is filtered to get filtrate after 13 days, will Which is put in 125 DEG C of high-temperature sterilization box the 25min that sterilizes, and obtains the filtrate that sterilizes;It is 2 in mass ratio:5 crystallize standby and above-mentioned Sterilizing filtrate is sequentially loaded in the there-necked flask with agitator and thermometer, adds the Oleum Camelliae of crystallization gross mass 10%, 35min is stirred at 55 DEG C, and discharging obtains final product self-control chelating agent;Count by weight, weigh 28 parts of curpic carbonate, 130 parts of above-mentioned self-controls Chelating agent, 7 parts of sodium bicarbonate, 0.02 part of selenium dioxide and 950 parts of deionized waters are sequentially loaded in colloid mill, at 35 DEG C with Discharge after 1500r/min rotating speeds grinding 2h, be that 0.5mol/L sodium hydroxide solutions adjust pH to 9.5 with concentration, obtain final product after tinning Biomass cyanideless electro-plating liquid.
The concrete application method of the present invention:Biomass cyanideless electro-plating liquid obtained in the present invention is heated to 55 DEG C first Standby afterwards, then layer alloy substrate to be plated is accessed on the anode of circuit ingredient, make negative electrode with graphite, by the gold for connecting During category matrix is immersed to standby electroplate liquid, turn-on current, with 45mA/cm2Electric current density, plating 3h after.Present invention system The plating liquid energy for obtaining effectively prevents the displacement phenomenon of steel and iron parts, and the complex mixture bond strength of formation is high, and plating solution dispersion Ability and covering power are stronger, and solution composition is nontoxic, and coating light is careful, with splendid electroplating effect.
Example 3
Take tamarind to shell to obtain kernel, putting it into grinding 30min in mortar, to obtain tamarind unqualified, by unqualified for gained and etc. quality The dehydrated alcohol of ratio is sequentially loaded in ceramic pot, and stir to obtain pastel, then adds pastel quality 5% in ceramic pot Compound enzymic preparation, described compound enzymic preparation be by Epoxysuccinic acid hydrolytic enzyme, pectase, cellulase and amylase by etc. matter Amount ratio is mixed to prepare;After above-mentioned enzyme preparation is added and finished, ceramic pot is put after terminating by insulation enzymolysis 8h at 35 DEG C, enzymolysis again Temperature be 40 DEG C, relative air humidity be 70% in the environment of naturally mouldy 12 days, be separated by filtration after mouldy end and filtered Liquid, then filtrate is centrifuged the isolated supernatant of 15min with centrifuge with 4000r/min rotating speeds;By supernatant obtained above Be put in reactor, after being heated to 120 DEG C start agitator be stirred, in the state of stirring add sodium carbonate until Supernatant pH obtains concentrated solution in neutrality, the isolated filtrate of filtered while hot by the 1/3 of filtrate evaporation and concentration to its original volume, Concentrated solution is placed on standing 30h in 6 DEG C of refrigerator makes its spontaneous nucleation, is filtrated to get crystallization, standby;Take Fresh Lemon to cut Piece, and be 3 in mass ratio:1 will be put into as fermentation substrate in fermentation tank after lemon tablet and Radix Glycyrrhizae mixing, then by inoculum concentration be 10% accesses aspergillus niger in fermentation substrate, fermentation tank is put into heat-preservation fermentation in 40 DEG C of calorstats and is filtered to get filtrate after 14 days, will Which is put in 130 DEG C of high-temperature sterilization box the 30min that sterilizes, and obtains the filtrate that sterilizes;It is 2 in mass ratio:5 crystallize standby and above-mentioned Sterilizing filtrate is sequentially loaded in the there-necked flask with agitator and thermometer, adds the Oleum Camelliae of crystallization gross mass 10%, 40min is stirred at 60 DEG C, and discharging obtains final product self-control chelating agent;Count by weight, weigh 30 parts of curpic carbonate, 150 parts of above-mentioned self-controls Chelating agent, 8 parts of sodium bicarbonate, 0.03 part of selenium dioxide and 1000 parts of deionized waters are sequentially loaded in colloid mill, at 40 DEG C with Discharge after 2000r/min rotating speeds grinding 2h, be that 0.5mol/L sodium hydroxide solutions adjust pH to 1.0 with concentration, obtain final product after tinning Biomass cyanideless electro-plating liquid.
The concrete application method of the present invention:Biomass cyanideless electro-plating liquid obtained in the present invention is heated to 60 DEG C first Standby afterwards, then layer alloy substrate to be plated is accessed on the anode of circuit ingredient, make negative electrode with graphite, by the gold for connecting During category matrix is immersed to standby electroplate liquid, turn-on current, with 50mA/cm2Electric current density, plating 3h after.Present invention system The plating liquid energy for obtaining effectively prevents the displacement phenomenon of steel and iron parts, and the complex mixture bond strength of formation is high, and plating solution dispersion Ability and covering power are stronger, and solution composition is nontoxic, and coating light is careful, with splendid electroplating effect.

Claims (1)

1. a kind of preparation method of biomass cyanideless electro-plating liquid, it is characterised in that concrete preparation process is:
(1)Take tamarind to shell to obtain kernel, putting it into 20~30min of grinding in mortar, to obtain tamarind unqualified, and gained is unqualified With etc. the dehydrated alcohol of quality be sequentially loaded in ceramic pot, stir to obtain pastel, then adds pasty mass in ceramic pot The compound enzymic preparation of amount 3~5%, described compound enzymic preparation is by Epoxysuccinic acid hydrolytic enzyme, pectase, cellulase and shallow lake Powder enzyme is mixed to prepare by grade mass ratio;
(2)After above-mentioned enzyme preparation is added and finished, at 30~35 DEG C, 6~8h of insulation enzymolysis, digests after terminating again by ceramic pot Be placed on temperature for 30~40 DEG C, relative air humidity be 60~70% in the environment of naturally mouldy 9~12 days, mistake after mouldy end Isolated filtrate is filtered, then filtrate is centrifuged the isolated supernatants of 10~15min with centrifuge with 3000~4000r/min rotating speeds Liquid;
(3)Supernatant obtained above is put in reactor, is started agitator after being heated to 100~120 DEG C and is stirred Mix, in the state of stirring, add sodium carbonate up to supernatant pH in neutrality, filtrate is evaporated by the isolated filtrate of filtered while hot Be concentrated into its original volume 1/3 obtains concentrated solution, and concentrated solution is placed on 20~30h of standing in 4~6 DEG C of refrigerator makes its nature Crystallization, is filtrated to get crystallization, standby;
(4)Fresh Lemon section is taken, and is 3 in mass ratio:1 will be put in fermentation tank as fermentation after lemon tablet and Radix Glycyrrhizae mixing Substrate, then aspergillus niger is accessed by inoculum concentration in fermentation substrate for 10%, fermentation tank is put into insulation in 30~40 DEG C of calorstats and is sent out Ferment filtered to get filtrate after 12~14 days, puts it into 20~30min of sterilizing in 120~130 DEG C of high-temperature sterilization box, is sterilized Filtrate;
(5)It is 2 in mass ratio:Standby crystallization and above-mentioned sterilizing filtrate are sequentially loaded into three mouthfuls with agitator and thermometer by 5 The Oleum Camelliae of crystallization gross mass 10% in flask, being added, 30~40min being stirred at 50~60 DEG C, discharging obtains final product self-control complexation Agent;
(6)Count by weight, weigh 25~30 parts of curpic carbonate, 100~150 parts of above-mentioned self-control chelating agent, 5~8 parts of bicarbonates Sodium, 0.01~0.03 part of selenium dioxide and 900~1000 parts of deionized waters are sequentially loaded in colloid mill, at 30~40 DEG C with 1000~2000r/min rotating speeds grind 1~2h after discharge, with concentration be 0.5mol/L sodium hydroxide solutions adjust pH to 9.0~ 1.0, biomass cyanideless electro-plating liquid is obtained final product after tinning.
CN201610897240.5A 2016-10-14 2016-10-14 A kind of preparation method of biomass cyanideless electro-plating liquid Pending CN106498454A (en)

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CN1414142A (en) * 2002-09-13 2003-04-30 袁国伟 Environmental protection type cyanogenless electroplating technology
CN103305880A (en) * 2013-04-24 2013-09-18 湖北恒鑫金属表面处理有限公司 Citrate-tartrate dual-complexing non-cyanide alkaline copper-plating electrolyte on steel substrate
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