CN103333533A - Magnetic bronze powder preparation method - Google Patents
Magnetic bronze powder preparation method Download PDFInfo
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- CN103333533A CN103333533A CN201310290410XA CN201310290410A CN103333533A CN 103333533 A CN103333533 A CN 103333533A CN 201310290410X A CN201310290410X A CN 201310290410XA CN 201310290410 A CN201310290410 A CN 201310290410A CN 103333533 A CN103333533 A CN 103333533A
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Abstract
The invention discloses a magnetic bronze powder preparation method. The method comprises the following steps: cleaning sheet bronze powder ball-milled in a ball mill in a cleaning tank with a ketone solvent, 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 an acrylate monomer and an azo initiator, adding to the reactor, coating, taking out, press-filtering, and carrying out solid-liquid separation to obtain magnetic bronze powder. The method allows the surfaces of the sheet copper-zinc particles to be coated with the surface of a magnetic material through organic-inorganic double layer coating, so the aqueous copper-zinc particles are magnetic, and a very good stereo artistic effect is formed.
Description
Technical field
The present invention relates to a kind of preparation method of magnetic copper bronze.
Background technology
Deepening constantly along with China's economic reform in recent years, people's standard of living is significantly improved, quality to life has darker understanding and higher requirement, along with weeding out the old and bring forth the new of decoration, the three-dimensional magic art of 3D coating becomes the new lover of fashion decoration, the 3D stereoeffect of its uniqueness as a high-grade paint, fantasy gorgeous moving color, and exclusive metal-like and natural and tripping lines, changeable visual effect is subjected to designer's welcome and the choosing of decoration heat deeply.It gives the three-dimensional line of pure natural grace and pattern, deep visual effect makes product that kind of a fresh and alive sensation true to nature is arranged.
The three-dimensional magic art of 3D coating is to add magneticsubstance in coating, when coating is coated on the workpiece by certain form of construction work, under the effect in magnetic field, magnetic coating aligns according to the direction in magnetic field, after the coating drying, just be fixed up according to certain mode, form solid pattern.
Copper bronze (claiming bronze again) is to be raw material with the copper zinc alloy, make through special machine processing and chemical conversion treatment, it be have scale structure, can be floating in binding material, a kind of metallic pigment of presenting inaurate, having splendid effect.Be widely used in aspects such as plastic cement, senior magazine, high-grade packing, cigarette shell, security printing.And common copper bronze does not have magnetic, and variation that can not active response magnetic field under magnetic field also just can not form good stereo artistic effect.
Summary of the invention
The preparation method who the purpose of this invention is to provide a kind of magnetic copper bronze, the present invention is overlying on sheet of copper zinc particles surface by the organic and inorganic double-coated with magneticsubstance, makes the copper zinc particles have magnetic; The magnetic copper bronze of the inventive method preparation can be applied in the three-dimensional magic art of the 3D coating the three-dimensional dynamic various workpiece shells of preparation, the magic nail varnish, opal nail polish glue, the phantom nail pastes, the automobile applique, liquid wallpaper, wood furniture, pottery, senior magazine, high-grade packing, cigarette shell, multiple field such as security printing.
In order to solve the problems of the technologies described above, the present invention is solved by following technical proposals:
The preparation method of magnetic 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, 3-8 part magnetic powder material, 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 acrylic ester monomer of 4-10 part, 0.015-0.06 part azo-initiator, closed reactor, in reactor, feed protection of inert gas, aforesaid propylene esters of gallic acid monomer and azo-initiator 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 coated magnetic sheet of copper bronze of 70-80%.
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 acrylic ester monomer is methyl methacrylate, methyl acrylate, hydroxyethyl methylacrylate, Hydroxyethyl acrylate, Rocryl 410, Propylene glycol monoacrylate, butyl methacrylate, one or more in the butyl acrylate.
As preferably, described azo-initiator is Diisopropyl azodicarboxylate.
As preferably, described magnetic powder material is r-Fe
2O
3, Fe
3O
4, Co
x-Fe
3-xO
4, Fe (CO)
5, among Co, the Ni one or more.
The present invention has significant technique effect owing to adopted above technical scheme:
Inorganic-the organic bilayer of the present invention's preparation coats the sheet of copper bronze, coats closely, and coating layer is difficult for destroyed, water-tolerant; Acid and alkali-resistance is good; 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 coating and the printing ink.By regulating kind and the ratio of acrylic ester monomer, can be prepared into water-based magnetic copper bronze and oily molten type magnetic copper bronze.
Embodiment
Below in conjunction with specific embodiment the present invention is described in further detail:
Embodiment 1
The preparation method of magnetic 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 ethanol, 0.1 part of sec.-propyl two oleic acid acyloxy (dioctyl phosphoric acid acyloxy) titanic acid ester, 3 parts of Fe
3O
4, 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 dilutions; Get 2.5 parts of tetraethoxys, with 5 parts of 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 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 methyl methacrylate, 0.015 part of Diisopropyl azodicarboxylate feeds protection of inert gas in reactor, and above-mentioned methyl methacrylate 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 coated magnetic sheet of copper bronze of 70%.
Embodiment 2
The preparation method of magnetic 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 35 parts filter cake, 65 parts of n-propyl alcohols, 0.3 part of sec.-propyl three (dioctyl phosphoric acid acyloxy) titanic acid ester, 5 parts of magnetic powder material Fe (CO)
5, 30-40 ℃ is stirred 0.5-1h down;
Step c is got 0.6 part of 25% ammoniacal liquor, and 2.3 parts of distilled water mix ammoniacal liquor with distilled water, with 5 parts of n-propyl alcohols dilutions; Get 3 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 35 parts of copper bronzes, and 65 parts of ether solvents coat the copper bronze with inorganic silicon and are dispersed in the glycol dimethyl ether; Get 7 parts methyl acrylate, 0.03 part of Diisopropyl azodicarboxylate feeds protection of inert gas in reactor, and aforesaid propylene acid methyl esters 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 coated magnetic sheet of copper bronze of 76%.
Embodiment 3
The preparation method of magnetic 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 Virahols, 8 parts of magnetic powder material Ni, 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 isopropanol; Get 3.5 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 40 parts of copper bronzes, and 70 parts of ethylene glycol ethyl ethers coat the copper bronze with inorganic silicon and are dispersed in the ethylene glycol ethyl ether; Get 10 parts Hydroxyethyl acrylate, 0.06 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 coated magnetic 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 (7)
1. the preparation method of magnetic 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, 3-8 part magnetic powder material, and 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 acrylic ester monomer of 4-10 part, 0.015-0.06 part azo-initiator feeds protection of inert gas in reactor, aforesaid propylene esters of gallic acid 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 obtains inorganic-organic bilayer coated magnetic sheet of copper bronze of 70-80%.
2. the preparation method of magnetic 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 magnetic 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 magnetic 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 magnetic copper bronze according to claim 1, it is characterized in that: described acrylic ester monomer is methyl methacrylate, methyl acrylate, hydroxyethyl methylacrylate, Hydroxyethyl acrylate, Rocryl 410, Propylene glycol monoacrylate, butyl methacrylate, one or more in the butyl acrylate.
6. the preparation method of magnetic copper bronze according to claim 1, it is characterized in that: described azo-initiator is Diisopropyl azodicarboxylate.
7. the preparation method of magnetic copper bronze according to claim 1, it is characterized in that: described magnetic powder material is r-Fe
2O
3, Fe
3O
4, Co
x-Fe
3-xO
4, Fe (CO)
5, among Co, the Ni one or more.
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| CN201310290410XA CN103333533A (en) | 2013-07-11 | 2013-07-11 | Magnetic bronze powder preparation method |
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| CN201310290410XA CN103333533A (en) | 2013-07-11 | 2013-07-11 | Magnetic bronze powder preparation method |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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| 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 |
| 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 |
| 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 |
| CN107262710A (en) * | 2017-06-26 | 2017-10-20 | 俞惠英 | A kind of preparation method of cu-zn alloy powder |
| CN107629490A (en) * | 2017-10-18 | 2018-01-26 | 安徽天易金属新材料有限公司 | A kind of preparation method of aqueous architectural exterior wall aluminium pigment |
| CN114539767A (en) * | 2020-11-25 | 2022-05-27 | 合肥杰事杰新材料股份有限公司 | Spraying-free PA6 composite material and preparation method thereof |
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Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
| 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 |
| 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 |
| 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 |
| CN107262710A (en) * | 2017-06-26 | 2017-10-20 | 俞惠英 | A kind of preparation method of cu-zn alloy powder |
| CN107629490A (en) * | 2017-10-18 | 2018-01-26 | 安徽天易金属新材料有限公司 | A kind of preparation method of aqueous architectural exterior wall aluminium pigment |
| CN114539767A (en) * | 2020-11-25 | 2022-05-27 | 合肥杰事杰新材料股份有限公司 | Spraying-free PA6 composite material and preparation method thereof |
| CN114539767B (en) * | 2020-11-25 | 2024-03-29 | 合肥杰事杰新材料股份有限公司 | Spraying-free PA6 composite material and preparation method thereof |
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Application publication date: 20131002 |