CN103333532A - Aqueous bronze powder preparation method - Google Patents
Aqueous bronze powder preparation method Download PDFInfo
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- CN103333532A CN103333532A CN2013102904097A CN201310290409A CN103333532A CN 103333532 A CN103333532 A CN 103333532A CN 2013102904097 A CN2013102904097 A CN 2013102904097A CN 201310290409 A CN201310290409 A CN 201310290409A CN 103333532 A CN103333532 A CN 103333532A
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Abstract
The invention discloses an aqueous bronze powder preparation method. The method comprises the following steps: cleaning sheet bronze powder ball-milled in a ball mill with a ketone solvent in a cleaning tank, press-filtering, and carrying out solid-liquid separation to obtain a filter cake; adding the filter cake, an alcoholic solvent and a titanate coupling agent to a reaction container, and stirring; taking ammonia water and distilled water, and mixing ammonia water with distilled water for dilution; taking ethyl orthosilicate, and diluting with the alcoholic solvent; simultaneously adding to the reaction container in a dropwise manner; ageing for 6-10h, taking out, press-filtering, and carrying out solid-liquid separation to obtain inorganic silicon coated bronze powder; taking the inorganic silicon coated bronze powder and an ether solvent, and uniformly dispersing the inorganic silicon coated bronze powder in the ether solvent; and taking a hydrophilic ester monomer and an azo initiator, adding to the reactor, coating, taking out, press-filtering, and carrying out solid-liquid separation to obtain aqueous bronze powder. The method adopts an organic-inorganic double layer coating modifying treatment process to prepare the aqueous bronze powder, so the aqueous bronze powder has a high controlled release efficiency and does not change its color for a long time in alkaline printing ink.
Description
Technical field
The present invention relates to a kind of preparation method of aqueous copper bronze.
Background technology
The copper bronze is to be main raw material with copper, zinc, through the extremely trickle scaled metal powder end that special machine is processed and chemical conversion treatment is made, sheet is thick generally at 01 ~ 1 μ m, it is called in a certain proportion of blending oil (become printing ink in order to be in harmonious proportion the copper bronze, carry out the low-melting ink vehicle that bronze printing is used) or varnish, flavous gold lacquer, make the outer packaging of product reach the effect of golden wall splendidness, very popular.
At present, the widely used printing ink of packages printing industry is carrier with the organic solvent, and organic volatile in the printing ink (VOC) content is 30% ~ 70%, produces environmental pollution, the infringement HUMAN HEALTH.Water color ink can reduce significantly that VOC is specially adapted to the package printed matter of health conditions requiring strictnesses such as food, medicine to airborne volatilization in the printing process, and with water as solvent, reduced cost.
Along with people's sound and perfect to the reinforcement of environmental protection consciousness and environmental regulation, solvent type ink will partly be replaced by water color ink.Because the pH value of water color ink is weakly alkaline, oxidation and corrosion take place in copper bronze easily in weakly alkaline water-based printing medium, make Jin Mo produce many problems from the hydrotropic transformation of solvent-borne type, as the copper bronze tarnish, difficulties in dispersion, golden black viscosity are higher etc.In order fundamentally to solve the corrosion discoloration problem that the copper bronze is used in the weakly alkaline water-based system, need carry out the research of rust inhibition aspect, improve that it is anti-corrosion and stable, the simulating golden colour that keeps the copper bronze is mutually and high glossiness.There are two kinds of technologies can make metallic pigment have stability at present: one, at the suitable corrosion inhibitor of metallic pigment surface adsorption; Two, the microcapsule pigment that has protective coating (microcapsule method).
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of aqueous copper bronze, the inventive method is by adopting the aqueous copper bronze of organic and inorganic double-coated modification processing method preparation, in the alkaline printing ink of pH-8.5, slowly-releasing efficient is 95%, nondiscoloration in 12 hours under 250 ℃ temperature.
In order to solve the problems of the technologies described above, the present invention is solved by following technical proposals:
The preparation method of aqueous copper bronze comprises the steps:
The sheet of copper bronze that step a. is good with the ball mill ball milling cleans in rinse bath with ketones solvent, behind the cleaning 1-2h, and press filtration, solid-liquid separation obtains the filter cake that solid content is 80-85%;
Step b. adds filter cake, 60-70 part alcoholic solvent, the 0.1-0.5 part titanate coupling agent that weight part is 30-40 part in reaction vessel, 30-40 ℃ is stirred 0.5-1h down;
Step c is got ammoniacal liquor 0.3-1.0 part of 25%, and distilled water 2-2.5 part is mixed ammoniacal liquor with distilled water, with 5 parts of alcoholic solvent dilutions; Get tetraethoxy 2.5-3.5 part, with 5 parts of alcoholic solvent dilutions; With above-mentioned both be added drop-wise to simultaneously in the reaction vessel, keep 0.5-1h to dropwise, temperature of reaction is 35-45 ℃;
Steps d. ageing 6-10h, take out, press filtration, solid-liquid separation, obtaining solid content is the inorganic silicon coating copper bronze of 80-85%;
Step e. gets inorganic silicon and coats copper bronze 30-40 part, and ether solvent 60-70 part coats the copper bronze with inorganic silicon and is dispersed in the ether solvent; Get the wetting ability esters monomer of 4-10 part, 0.015-0.06 part azo-initiator feeds protection of inert gas in reactor, above-mentioned wetting ability esters monomer and azo-initiator are added reactor in the mode that drips, temperature of plate coats time 2-4h at 70-80 ℃;
Step f. takes out, press filtration, and solid-liquid separation, the inorganic-organic bilayer that obtains 70-80% coats water-based sheet of copper bronze.
As preferably, described alcoholic solvent is ethanol, n-propyl alcohol, and Virahol mixes in the propyl alcohol one or more.
As preferably, described titanate coupling agent is any in sec.-propyl two oleic acid acyloxy (dioctyl phosphoric acid acyloxy) titanic acid ester, sec.-propyl three (dioctyl phosphoric acid acyloxy) titanic acid ester, sec.-propyl three oleic acid acyloxy titanic acid ester, three stearic acid isopropyl titanate compounds, sec.-propyl three (dioctyl phosphoric acid acyloxy) titanic acid ester, two (dioctyl phosphoric acid acyloxy) ethylene titanic acid ester, tetra isopropyl two (the dioctyl phosphoric acid acyloxy) titanic acid ester.
As preferably, described ether solvent is one or more in ethylene glycol monobutyl ether, glycol dimethyl ether, ethylene glycol ethyl ether, ethylene glycol monomethyl ether, the butyl glycol ether.
As preferably, described wetting ability esters monomer is hydroxyethyl methylacrylate, Hydroxyethyl acrylate, Rocryl 410, one or more in the Propylene glycol monoacrylate.
As preferably, described azo-initiator is Diisopropyl azodicarboxylate.
The present invention has significant technique effect owing to adopted above technical scheme:
Of the present invention inorganic-organic bilayer coats water-based sheet of copper bronze, coats closely, coating layer is difficult for destroyed, water-tolerant; Good water solubility, directly dilute with water; Coating is thin and even, and is little to the influence of copper bronze metalluster; Multilayer coats, outer field organic layer be easy to coating in macromolecule resin mix good dispersity in coating.Be mainly used in various water-borne coatingss and the water color ink.
Embodiment
Below in conjunction with specific embodiment the present invention is described in further detail:
Embodiment 1
The preparation method of aqueous copper bronze comprises the steps:
The sheet of copper bronze that step a. is good with the ball mill ball milling cleans in rinse bath with ketones solvent, behind the cleaning 1-2h, and press filtration, solid-liquid separation obtains the filter cake that solid content is 80-85%;
Step b. adds weight part in reaction vessel be 30 parts filter cake, 60 parts of alcohol solvents, 0.1 part of sec.-propyl two oleic acid acyloxy (dioctyl phosphoric acid acyloxy) titanic acid ester, and 30-40 ℃ is stirred 0.5-1h down;
Step c is got 0.3 part of 25% ammoniacal liquor, and 2 parts of distilled water mix ammoniacal liquor with distilled water, with 5 parts of alcohol solvents dilutions; Get tetraethoxy 2.5-3.5 part, with 5 parts of alcohol solvent dilutions; With above-mentioned both be added drop-wise to simultaneously in the reaction vessel, keep 0.5-1h to dropwise, temperature of reaction is 45 ℃;
Steps d. ageing 6-10h, take out, press filtration, solid-liquid separation, obtaining solid content is the inorganic silicon coating copper bronze of 80-85%;
Step e. gets inorganic silicon and coats 30 parts of copper bronzes, and 60 parts of ethylene glycol monobutyl ethers coat the copper bronze with inorganic silicon and are dispersed in the ethylene glycol monobutyl ether; Get 4 parts hydroxyethyl methylacrylate, 0.015 part Diisopropyl azodicarboxylate feeds protection of inert gas in reactor, above-mentioned hydroxyethyl methylacrylate and Diisopropyl azodicarboxylate are added reactor in the mode that drips, temperature of plate coats time 2-4h at 70-80 ℃;
Step f. takes out, press filtration, and solid-liquid separation obtains inorganic-organic bilayer coating water-based sheet of copper bronze of 70%.
Embodiment 2
The preparation method of aqueous copper bronze comprises the steps:
The sheet of copper bronze that step a. is good with the ball mill ball milling cleans in rinse bath with ketones solvent, behind the cleaning 1-2h, and press filtration, solid-liquid separation obtains the filter cake that solid content is 80-85%;
Step b. adds the filter cake that weight part is 30-40 part, 65 parts of Virahols, 0.3 part of sec.-propyl three oleic acid acyloxy titanic acid ester in reaction vessel, 30-40 ℃ is stirred 0.5-1h down;
Step c is got 0.6 part of 25% ammoniacal liquor, and 2 parts of distilled water mix ammoniacal liquor with distilled water, with 5 parts of isopropanol; Get 3 parts of tetraethoxys, with 5 parts of isopropanol; With above-mentioned both be added drop-wise to simultaneously in the reaction vessel, keep 0.5-1h to dropwise, temperature of reaction is 45 ℃;
Steps d. ageing 6-10h, take out, press filtration, solid-liquid separation, obtaining solid content is the inorganic silicon coating copper bronze of 80-85%;
Step e. gets inorganic silicon and coats copper bronze 30-40 part, and 65 parts of ethylene glycol ethyl ethers coat the copper bronze with inorganic silicon and are dispersed in the ethylene glycol ethyl ether; Get the Hydroxyethyl acrylate of 4-10 part, 0.03 part of Diisopropyl azodicarboxylate feeds protection of inert gas in reactor, and aforesaid propylene acid hydroxyl ethyl ester and Diisopropyl azodicarboxylate are added reactor in the mode that drips, and temperature of plate coats time 2-4h at 70-80 ℃;
Step f. takes out, press filtration, and solid-liquid separation obtains inorganic-organic bilayer coating water-based sheet of copper bronze of 75%.
Embodiment 3
The preparation method of aqueous copper bronze comprises the steps:
The sheet of copper bronze that step a. is good with the ball mill ball milling cleans in rinse bath with ketones solvent, behind the cleaning 1-2h, and press filtration, solid-liquid separation obtains the filter cake that solid content is 80-85%;
Step b. adds weight part in reaction vessel be 40 parts filter cake, 70 parts of n-propyl alcohols, 0.5 part of three stearic acid isopropyl titanate compound, and 30-40 ℃ is stirred 0.5-1h down;
Step c is got 1.0 parts of 25% ammoniacal liquor, and 2.5 parts of distilled water mix ammoniacal liquor with distilled water, with 5 parts of n-propyl alcohols dilutions; Get 3.5 parts of tetraethoxys, with 5 parts of n-propyl alcohol dilutions; With above-mentioned both be added drop-wise to simultaneously in the reaction vessel, keep 0.5-1h to dropwise, temperature of reaction is 45 ℃;
Steps d. ageing 6-10h, take out, press filtration, solid-liquid separation, obtaining solid content is the inorganic silicon coating copper bronze of 80-85%;
Step e. gets inorganic silicon and coats 40 parts of copper bronzes, and 70 parts of ethylene glycol monomethyl ether coat the copper bronze with inorganic silicon and are dispersed in the ethylene glycol monomethyl ether; Get 10 parts Propylene glycol monoacrylate, 0.06 part of Diisopropyl azodicarboxylate feeds protection of inert gas in reactor, and aforesaid propylene acid hydroxypropyl acrylate and Diisopropyl azodicarboxylate are added reactor in the mode that drips, and temperature of plate coats time 2-4h at 70-80 ℃;
Step f. takes out, press filtration, and solid-liquid separation obtains inorganic-organic bilayer coating water-based sheet of copper bronze of 80%.
In a word, the above only is preferred embodiment of the present invention, and all equalizations of doing according to the present patent application claim change and modify, and all should belong to the covering scope of patent of the present invention.
Claims (6)
1. the preparation method of aqueous copper bronze is characterized in that, comprises the steps:
The sheet of copper bronze that step a. is good with the ball mill ball milling cleans in rinse bath with ketones solvent, behind the cleaning 1-2h, and press filtration, solid-liquid separation obtains the filter cake that solid content is 80-85%;
Step b. adds filter cake, 60-70 part alcoholic solvent, the 0.1-0.5 part titanate coupling agent that weight part is 30-40 part in reaction vessel, 30-40 ℃ is stirred 0.5-1h down;
Step c is got ammoniacal liquor 0.3-1.0 part of 25%, and distilled water 2-2.5 part is mixed ammoniacal liquor with distilled water, with 5 parts of alcoholic solvent dilutions; Get tetraethoxy 2.5-3.5 part, with 5 parts of alcoholic solvent dilutions; With above-mentioned both be added drop-wise to simultaneously in the reaction vessel, keep 0.5-1h to dropwise, temperature of reaction is 35-45 ℃;
Steps d. ageing 6-10h, take out, press filtration, solid-liquid separation, obtaining solid content is the inorganic silicon coating copper bronze of 80-85%;
Step e. gets inorganic silicon and coats copper bronze 30-40 part, and ether solvent 60-70 part coats the copper bronze with inorganic silicon and is dispersed in the ether solvent; Get the wetting ability esters monomer of 4-10 part, 0.015-0.06 part azo-initiator feeds protection of inert gas in reactor, above-mentioned wetting ability esters monomer and azo-initiator are added reactor in the mode that drips, temperature of plate coats time 2-4h at 70-80 ℃;
Step f. takes out, press filtration, and solid-liquid separation, the inorganic-organic bilayer that obtains 70-80% coats water-based sheet of copper bronze.
2. the preparation method of aqueous copper bronze according to claim 1, it is characterized in that: described alcoholic solvent is ethanol, n-propyl alcohol, Virahol mixes in the propyl alcohol one or more.
3. the preparation method of aqueous copper bronze according to claim 1, it is characterized in that: described titanate coupling agent is any in sec.-propyl two oleic acid acyloxy (dioctyl phosphoric acid acyloxy) titanic acid ester, sec.-propyl three (dioctyl phosphoric acid acyloxy) titanic acid ester, sec.-propyl three oleic acid acyloxy titanic acid ester, three stearic acid isopropyl titanate compounds, sec.-propyl three (dioctyl phosphoric acid acyloxy) titanic acid ester, two (dioctyl phosphoric acid acyloxy) ethylene titanic acid ester, tetra isopropyl two (the dioctyl phosphoric acid acyloxy) titanic acid ester.
4. the preparation method of aqueous copper bronze according to claim 1, it is characterized in that: described ether solvent is one or more in ethylene glycol monobutyl ether, glycol dimethyl ether, ethylene glycol ethyl ether, ethylene glycol monomethyl ether, the butyl glycol ether.
5. the preparation method of aqueous copper bronze according to claim 1, it is characterized in that: described wetting ability esters monomer is hydroxyethyl methylacrylate, Hydroxyethyl acrylate, Rocryl 410, one or more in the Propylene glycol monoacrylate.
6. the preparation method of aqueous copper bronze according to claim 1, it is characterized in that: described azo-initiator is Diisopropyl azodicarboxylate.
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Cited By (16)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103613961A (en) * | 2013-12-06 | 2014-03-05 | 扬州大学 | Method for reducing interfacial tension of water-soluble inorganic oxidant or water-soluble inorganic salt in oil-soluble material |
| CN104263087A (en) * | 2014-09-29 | 2015-01-07 | 合肥旭阳铝颜料有限公司 | Anti-corrosion bronze powder pigment and preparation method thereof |
| CN104277559A (en) * | 2014-10-20 | 2015-01-14 | 合肥旭阳铝颜料有限公司 | Water-based copper-gold powder pigment for decoration and preparation method thereof |
| CN104312296A (en) * | 2014-10-25 | 2015-01-28 | 合肥旭阳铝颜料有限公司 | Bronze powder pigment for decoration and preparation method of bronze powder pigment |
| CN104371384A (en) * | 2014-09-29 | 2015-02-25 | 合肥旭阳铝颜料有限公司 | Antibiotic bronze powder pigment and preparation method thereof |
| CN104629090A (en) * | 2013-11-06 | 2015-05-20 | 金发科技股份有限公司 | Copper powder coated polymer microspheres and preparation method and application thereof |
| CN104974591A (en) * | 2015-06-27 | 2015-10-14 | 铜陵铜基粉体科技有限公司 | High-toughness ultraviolet-resistant aqueous copper zinc alloy powder, and preparation method thereof |
| CN104974556A (en) * | 2015-06-27 | 2015-10-14 | 铜陵铜基粉体科技有限公司 | High-efficiency flame-retardant aqueous copper zinc alloy powder and preparation method thereof |
| CN105017816A (en) * | 2015-06-27 | 2015-11-04 | 铜陵铜基粉体科技有限公司 | High temperature resistant waterborne copper-zinc alloy powder and making method thereof |
| CN105038332A (en) * | 2015-06-27 | 2015-11-11 | 铜陵铜基粉体科技有限公司 | Long-service-life water-based copper-zinc alloy powder and manufacturing method thereof |
| CN105038333A (en) * | 2015-06-27 | 2015-11-11 | 铜陵铜基粉体科技有限公司 | Wear-resisting water-based copper-zinc alloy powder and production method thereof |
| CN105038378A (en) * | 2015-06-27 | 2015-11-11 | 铜陵铜基粉体科技有限公司 | Water-based copper-zinc alloy powder with excellent color stability and production method thereof |
| CN105957642A (en) * | 2016-06-08 | 2016-09-21 | 天津大学 | Preparation method for silicon-dioxide-coated copper electronic paste used for LTCC substrate |
| CN105968887A (en) * | 2016-05-11 | 2016-09-28 | 广东德丽雅漆业有限公司 | Preparation method of organic-inorganic double-cladding water-borne bronze powder |
| CN107321975A (en) * | 2017-06-05 | 2017-11-07 | 苏州博卡金属颜料有限公司 | A kind of aqueous Cu-Zn alloy powder preparation method and aqueous copper metallic ink and coating |
| CN108097974A (en) * | 2018-01-15 | 2018-06-01 | 合肥旭阳铝颜料有限公司 | A kind of preparation method of minute surface gold paste |
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| CN104629090A (en) * | 2013-11-06 | 2015-05-20 | 金发科技股份有限公司 | Copper powder coated polymer microspheres and preparation method and application thereof |
| CN103613961A (en) * | 2013-12-06 | 2014-03-05 | 扬州大学 | Method for reducing interfacial tension of water-soluble inorganic oxidant or water-soluble inorganic salt in oil-soluble material |
| CN103613961B (en) * | 2013-12-06 | 2015-08-19 | 扬州大学 | A kind ofly reduce water-soluble inorganic oxygenant or the water-soluble inorganic salt method at oil-soluble material median surface tension force |
| CN104263087A (en) * | 2014-09-29 | 2015-01-07 | 合肥旭阳铝颜料有限公司 | Anti-corrosion bronze powder pigment and preparation method thereof |
| CN104371384A (en) * | 2014-09-29 | 2015-02-25 | 合肥旭阳铝颜料有限公司 | Antibiotic bronze powder pigment and preparation method thereof |
| CN104263087B (en) * | 2014-09-29 | 2016-03-23 | 合肥旭阳铝颜料有限公司 | A kind of protection against corrosion Cu-Zn alloy powder pigment and preparation method thereof |
| CN104277559A (en) * | 2014-10-20 | 2015-01-14 | 合肥旭阳铝颜料有限公司 | Water-based copper-gold powder pigment for decoration and preparation method thereof |
| CN104312296A (en) * | 2014-10-25 | 2015-01-28 | 合肥旭阳铝颜料有限公司 | Bronze powder pigment for decoration and preparation method of bronze powder pigment |
| CN104974556A (en) * | 2015-06-27 | 2015-10-14 | 铜陵铜基粉体科技有限公司 | High-efficiency flame-retardant aqueous copper zinc alloy powder and preparation method thereof |
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| CN105038332A (en) * | 2015-06-27 | 2015-11-11 | 铜陵铜基粉体科技有限公司 | Long-service-life water-based copper-zinc alloy powder and manufacturing method thereof |
| CN105038333A (en) * | 2015-06-27 | 2015-11-11 | 铜陵铜基粉体科技有限公司 | Wear-resisting water-based copper-zinc alloy powder and production method thereof |
| CN105038378A (en) * | 2015-06-27 | 2015-11-11 | 铜陵铜基粉体科技有限公司 | Water-based copper-zinc alloy powder with excellent color stability and production method thereof |
| CN104974591A (en) * | 2015-06-27 | 2015-10-14 | 铜陵铜基粉体科技有限公司 | High-toughness ultraviolet-resistant aqueous copper zinc alloy powder, and preparation method thereof |
| CN105968887A (en) * | 2016-05-11 | 2016-09-28 | 广东德丽雅漆业有限公司 | Preparation method of organic-inorganic double-cladding water-borne bronze powder |
| CN105957642A (en) * | 2016-06-08 | 2016-09-21 | 天津大学 | Preparation method for silicon-dioxide-coated copper electronic paste used for LTCC substrate |
| CN105957642B (en) * | 2016-06-08 | 2017-11-28 | 天津大学 | A kind of preparation method of coated with silica copper electric slurry for ltcc substrate |
| CN107321975A (en) * | 2017-06-05 | 2017-11-07 | 苏州博卡金属颜料有限公司 | A kind of aqueous Cu-Zn alloy powder preparation method and aqueous copper metallic ink and coating |
| CN108097974A (en) * | 2018-01-15 | 2018-06-01 | 合肥旭阳铝颜料有限公司 | A kind of preparation method of minute surface gold paste |
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Application publication date: 20131002 |