CN102604445A - Preparation method of aluminum pigment with high voltage breakdown resistance - Google Patents
Preparation method of aluminum pigment with high voltage breakdown resistance Download PDFInfo
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- CN102604445A CN102604445A CN2012100354261A CN201210035426A CN102604445A CN 102604445 A CN102604445 A CN 102604445A CN 2012100354261 A CN2012100354261 A CN 2012100354261A CN 201210035426 A CN201210035426 A CN 201210035426A CN 102604445 A CN102604445 A CN 102604445A
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Abstract
The invention discloses a preparation method of an aluminum pigment with high voltage breakdown resistance. The method comprises the steps of putting raw materials including spherical aluminum powder, a grinding medium, an environment-friendly solvent oil, oleic acid or erucic acid, and a silicane coupling agent into a ball mill; sealing the ball mill, performing ball milling, and discharging the materials with the environment-friendly solvent oil; conveying the materials through a pipeline into a vibration screen to be screened, removing screen tailings, and putting the materials into a frame filter press to conduct filter pressing, so as to obtain filter cakes with a solid content of 75%; feeding the filter cakes and an alcohol, ether or ester solvent into a reaction kettle, sealing the reaction kettle, increasing temperature under the protection of inert gases, then simultaneously dripping acrylic acid or acrylate monomer and an azo type initiator, continuously increasing the temperature of the reaction kettle, keeping the temperature, discharging materials, and performing filter pressing, so as to obtain the finished product. The aluminum pigment has the characteristic of high voltage breakdown resistance, the construction is convenient, the environment-friendly solvent oil is adopted for ball milling, and detection of all hazardous substances meets standards established by European Union.
Description
Technical field
The present invention relates to a kind of preparation method of household electrical appliances outside surface coating, particularly a kind of preparation method of high withstand voltage performance aluminium pigment.
Background technology
Along with China's rapid economic development; Domestic household electric appliances develop rapidly; Household electrical appliances manufacturing technology and household electrical appliances outside surface application techniques and level constantly rise; The main silvery white metallic pigment that flaky aluminum pigment adopts as the appliance finishes industry, its market demand had obtained fast development in recent years, and the aluminium pigment technology constantly develops to high withstand voltage performance, high hiding rare, good flash effect and special property direction.
But traditional non-coated aluminum pigment has also exposed some problems that self are difficult to overcome in use in recent years.For example; Household electrical appliances outside surface resistant voltage performance with its preparation is significantly not enough; Along with present household appliances structure develops towards lighting, densification, maximum space utilization ratio direction; The transient voltage on casing surface also raises to some extent in the household appliances switching on and shutting down process, because the restriction of traditional non-coated aluminum pigment production technique can not have higher withstand voltage properties.For this reason; External aluminium pigment production merchant active research novel high-performance aluminium pigment; Researched and developed out coated aluminum pigment with its advanced scientific and technological level and huge financial strength; This novel product has high withstand voltage properties, good coating, has started the novel production process of aluminium pigment and the new situation of coating process technology.The non-coated aluminum pigment of tradition contains objectionable impuritiess such as condensed-nuclei aromatics because of it, it is withdrawed from by the leading position in market as appliance finishes argentine pigment gradually.
Summary of the invention
The invention provides a kind of preparation method of high withstand voltage breakdown performance aluminium pigment, the aluminium pigment product of this method preparation has high withstand voltage properties, easy construction, and each item objectionable impurities detects the standard that European Union formulates that reaches.
The present invention realizes through following technical scheme, the present invention relates to a kind of preparation method of high withstand voltage breakdown performance aluminium pigment, may further comprise the steps:
Step 1 is got in raw material ball aluminum powder, grinding medium, environmentally friendly solvent oil, oleic acid or erucic acid, the silane coupling agent input ball mill;
Step 2 seals said ball mill, and ball milling is with the discharging of environmentally friendly solvent oil;
Step 3 with sieving in the said material inputted vibration sieve, is removed screenings through pipeline, gets into plate and frame(type)filter press and carries out press filtration, obtains solid content and be 75% filter cake;
Step 4, with said filter cake, alcohols, ethers or esters solvent add in the reaction kettle together; Seal said reaction kettle, under the protection of rare gas element, said temperature of reaction kettle is elevated to 45 ℃-55 ℃, then while dropwise addition of acrylic acid or acrylic ester monomer and azo-initiator; After dropwising, said temperature of reaction kettle is elevated to 70-80 ℃, insulation; Discharging gets into plate and frame(type)filter press and carries out press filtration, obtains finished product.
Preferably, in said step 2, the detailed process of said ball milling is earlier with the rotating speed ball milling of 60r/min 10 hours, is adjusted to 20r/min to said drum's speed of rotation then, and ball milling is 2 hours again.
Preferably, in said step 1, said grinding medium is that diameter is the steel ball of 0.8mm-1.5mm; In said step 4, the time of said dropping process is 1 hour, and the time of said insulation is 2.5-3.5 hour.
Preferably, described silane coupling agent is selected from a kind of in γ-methacryloxypropyl trimethoxy silane, vinyltriethoxysilane, vinyltrimethoxy silane, vinyl three (2-methoxy ethoxy) silane, the vinyl trimethoxysilane oligomer.
Preferably, the weight part of described ball aluminum powder, environmentally friendly solvent oil, oleic acid or erucic acid, each composition of silane coupling agent is: ball aluminum powder 40-80 weight part; Environmentally friendly solvent oil 80-160 weight part; Oleic acid or erucic acid 0.2-0.5 weight part; Silane coupling agent 0.1-0.3 weight part.
Preferably, the weight part of said alcohols, ethers or esters solvent, said azo-initiator is: alcohols, ethers or esters solvent 120-200 weight part; Azo-initiator 0.05-0.09 weight part.
Preferably, said environmentally friendly solvent grease separation one or more in D30, D40, D60, D70, D80 solvent oil.
Preferably, said vinylformic acid or acrylic ester monomer are two or more in vinylformic acid, methylacrylic acid, TEB 3K, methyl acrylate, Bing Xisuandingzhi, Isooctyl methacrylate, lauryl methacrylate(LMA), isobornyl methacrylate, Rocryl 400, Rocryl 410, Viscoat 295, the trimethylolpropane trimethacrylate.
Preferably; Said alcoholic solvent is selected from one or more in ethanol, n-propyl alcohol, the Virahol; Said ether solvent is selected from one or more in ethylene glycol monobutyl ether, diethylene glycol monobutyl ether, propylene glycol monomethyl ether, Ucar 35 butyl ether, dipropylene glycol methyl ether, the dipropylene glycol ether, and said esters solvent is selected from one or both in N-BUTYL ACETATE, the 1-Methoxy-2-propyl acetate.
Preferably, described azo-initiator is selected from Diisopropyl azodicarboxylate, 2,2-azo two (methylbutyronitrile), 2, a kind of in the 2-azo (2, the 4-methyl pentane nitrile).
When ball milling, add silane coupling agent, the alkoxyl group hydrolysis in the silane coupling agent generates silanol, and aluminium powder surface when ball milling produces a large amount of hydroxyls; The hydroxyl on aluminium powder surface can with the silanol generation condensation reaction on the silane coupling agent, thereby make silane coupling agent be attached to the aluminum particulate surface firmly, the silane coupling agent the other end of selection has two keys; Can produce copolyreaction with acrylic monomer; Thereby can make the polymeric membrane of copolyreaction generation be coated on the aluminum particulate surface tightly, like this, coating is tight; Be difficult for being destroyed by soda acid or mechanical force; Polymeric membrane has the good insulation performance performance simultaneously, and therefore, the aluminium pigment of the present invention's preparation has higher proof voltage breakdown performance; In addition, this product has good dispersiveness in coating and printing ink, thereby, easy construction; Simultaneously, adopt environmentally friendly solvent oil ball milling, each item objectionable impurities detects the standard that European Union formulates that reaches.
Embodiment
Embodiment 1
Present embodiment comprises the steps:
Step 1 is got 60 kilograms of raw material ball aluminum powder, diameter is in 0.2 kilogram of input ball mill of 0.36 kilogram of 120 kilograms of 1.2 tons of grinding medium steel balls, D80 solvent oils, oleic acid, vinyltriethoxysilane of 0.8mm;
Step 2, the ball sealer grinding machine with the rotating speed ball milling of 60r/min 10 hours, is adjusted to 20r/min to drum's speed of rotation, and ball milling 2 hours is with the discharging of environmentally friendly solvent oil;
Step 3, through pipeline sieve in the material inputted vibration sieve, classification, remove screenings, get into plate and frame(type)filter press and carry out press filtration, obtain solid content and be 75% filter cake;
Step 4 is filter cake and 160 kilograms of 1-Methoxy-2-propyl acetate solvents of 75% with the solid content that obtains, and adds in the reaction kettle together; Sealed reactor under protection of nitrogen gas, is elevated to 45 ℃ with temperature of reaction kettle; Beginning drips 0.5 kilogram of vinylformic acid, 6.5 kilograms of Bing Xisuandingzhis and 70 gram Diisopropyl azodicarboxylate initiators simultaneously, about 1 hour dropping time, after dropwising; Temperature of reaction kettle is elevated to 70 ℃, is incubated 2.5 hours, discharging; Get into plate and frame(type)filter press and carry out press filtration, solid-liquid separation obtains massfraction and is 60% high withstand voltage breakdown performance aluminium pigment.
Embodiment 2
Present embodiment comprises the steps:
Step 1 is got 50 kilograms of raw material ball aluminum powder, diameter and is in 0.20 kilogram of 80 kilograms of 1.2 tons of grinding medium steel balls, D70 solvent oils, oleic acid, 0.1 kilogram of input ball mill of vinyl three (2-methoxy ethoxy) silane of 1.0mm;
Step 2, the ball sealer grinding machine with the rotating speed ball milling of 60r/min 10 hours, is adjusted to 20r/min to drum's speed of rotation, and ball milling 2 hours is with the discharging of environmentally friendly solvent oil;
Step 3, through pipeline sieve in the material inputted vibration sieve, classification, remove screenings, get into plate and frame(type)filter press and carry out press filtration, obtain solid content and be 75% filter cake;
Step 4 is filter cake and 120 kilograms of N-BUTYL ACETATE solvents of 75% with the solid content that obtains, and adds in the reaction kettle sealed reactor together; Under protection of nitrogen gas, temperature of reaction kettle is elevated to 50 ℃, beginning drips 0.5 kilogram of vinylformic acid, 6.5 kilograms of methyl acrylates, 50 grams 2 simultaneously; 2-azo two (methylbutyronitrile) initiator is about 1 hour dropping time, after dropwising; Temperature of reaction kettle is elevated to 75 ℃, is incubated 3 hours, discharging; Get into plate and frame(type)filter press and carry out press filtration, solid-liquid separation obtains massfraction and is 60% high withstand voltage breakdown performance aluminium pigment
Embodiment 3
Present embodiment comprises the steps:
Step 1 is got 40 kilograms of raw material ball aluminum powder, diameter and is in 1.2 tons of the grinding medium steel balls, D60 solvent oil double centner, 0.30 kilogram of oleic acid, 0.15 kilogram of input ball mill of γ-methacryloxypropyl trimethoxy silane of 1.2mm;
Step 2, the ball sealer grinding machine with the rotating speed ball milling of 60r/min 10 hours, is adjusted to 20r/min to drum's speed of rotation, and ball milling 2 hours is with the discharging of environmentally friendly solvent oil;
Step 3, through pipeline sieve in the material inputted vibration sieve, classification, remove screenings, get into plate and frame(type)filter press and carry out press filtration, obtain solid content and be 75% filter cake;
Step 4 is filter cake and 140 kilograms of alcohol solvents of 75% with the solid content that obtains, and adds in the reaction kettle sealed reactor together; Under protection of nitrogen gas, temperature of reaction kettle is elevated to 55 ℃, beginning drips 0.5 kilogram of vinylformic acid, 6.5 kilograms of Isooctyl methacrylates, 60 grams 2,2-azo (2 simultaneously; The 4-methyl pentane nitrile) initiator is about 1 hour dropping time, after dropwising; Temperature of reaction kettle is elevated to 80 ℃, is incubated 3.5 hours, discharging; Get into plate and frame(type)filter press and carry out press filtration, solid-liquid separation obtains massfraction and is 60% high withstand voltage breakdown performance aluminium pigment.
Embodiment 4
Present embodiment comprises the steps:
Step 1 is got 70 kilograms of raw material ball aluminum powder, diameter is in 0.25 kilogram of input ball mill of 0.40 kilogram of 140 kilograms of 1.2 tons of grinding medium steel balls, D40 solvent oils, erucic acid, vinyltrimethoxy silane of 1.4mm;
Step 2, the ball sealer grinding machine with the rotating speed ball milling of 60r/min 10 hours, is adjusted to 20r/min to drum's speed of rotation, and ball milling 2 hours is with the discharging of environmentally friendly solvent oil;
Step 3, through pipeline sieve in the material inputted vibration sieve, classification, remove screenings, get into plate and frame(type)filter press and carry out press filtration, obtain solid content and be 75% filter cake;
Step 4 is 75% filter cake and 180 kg ethylene glycol monobutyl ether solvents with the solid content that obtains, and adds in the reaction kettle together; Sealed reactor under protection of nitrogen gas, is elevated to 50 ℃ with temperature of reaction kettle; Beginning drips 0.2 kilogram of methylacrylic acid, 5 kilograms of Bing Xisuandingzhis, 0.2 kilogram of Viscoat 295 and 80 gram Diisopropyl azodicarboxylate initiators simultaneously, about 1 hour dropping time, after dropwising; Temperature of reaction kettle is elevated to 75 ℃, is incubated 3 hours, discharging; Get into plate and frame(type)filter press and carry out press filtration, solid-liquid separation obtains massfraction and is 60% high withstand voltage breakdown performance aluminium pigment.
Embodiment 5
Present embodiment comprises the steps:
Step 1 is got 80 kilograms of raw material ball aluminum powder, diameter is in 0.30 kilogram of input ball mill of 0.50 kilogram of 160 kilograms of 1.2 tons of grinding medium steel balls, D30 solvent oils, erucic acid, vinyl trimethoxysilane oligomer of 1.5mm;
Step 2, the ball sealer grinding machine with the rotating speed ball milling of 60r/min 10 hours, is adjusted to 20r/min to drum's speed of rotation, and ball milling 2 hours is with the discharging of environmentally friendly solvent oil;
Step 3, through pipeline sieve in the material inputted vibration sieve, classification, remove screenings, get into plate and frame(type)filter press and carry out press filtration, obtain solid content and be 75% filter cake;
Step 4 is filter cake and 200 kilograms of propylene glycol monomethyl ether solvents of 75% with the solid content that obtains, and adds in the reaction kettle sealed reactor together; Under protection of nitrogen gas, temperature of reaction kettle is elevated to 45 ℃, beginning drips 0.2 kilogram of methylacrylic acid, 5 kilograms of Bing Xisuandingzhis, 0.2 kilogram of lauryl methacrylate(LMA) and 90 grams 2 simultaneously; 2-azo two (methylbutyronitrile) initiator is about 1 hour dropping time, after dropwising; Temperature of reaction kettle is elevated to 70 ℃, is incubated 2.5 hours, discharging; Get into plate and frame(type)filter press and carry out press filtration, solid-liquid separation obtains massfraction and is 60% high withstand voltage breakdown performance aluminium pigment.
With the aluminium pigment finished product that above-mentioned each embodiment obtains, measure its product performance according to the conventional sense means, its each performance index are following:
(1) withstand voltage properties: >=8000V
(2) tail over rate (75 μ m sieve aperture) :≤1.0%
(3) foreign metal total amount :≤1.0%
(4) acidic fog resistance property (hour): >=1000
What should explain at last is: above embodiment only in order to the explanation the present invention and and unrestricted technical scheme described in the invention; Therefore, although this specification sheets has carried out detailed explanation to the present invention with reference to each above-mentioned embodiment,, those of ordinary skill in the art should be appreciated that still and can make amendment or be equal to replacement the present invention; And all do not break away from the technical scheme and the improvement thereof of the spirit and scope of the present invention, and it all should be encompassed in the claim scope of the present invention.
Claims (10)
1. the preparation method of a high withstand voltage breakdown performance aluminium pigment is characterized in that, may further comprise the steps:
Step 1 is got in raw material ball aluminum powder, grinding medium, environmentally friendly solvent oil, oleic acid or erucic acid, the silane coupling agent input ball mill;
Step 2 seals said ball mill, and ball milling is with the discharging of environmentally friendly solvent oil;
Step 3 with sieving in the said material inputted vibration sieve, is removed screenings through pipeline, gets into plate and frame(type)filter press and carries out press filtration, obtains solid content and be 75% filter cake;
Step 4, with said filter cake, alcohols, ethers or esters solvent add in the reaction kettle together; Seal said reaction kettle, under the protection of rare gas element, said temperature of reaction kettle is elevated to 45 ℃-55 ℃, then while dropwise addition of acrylic acid or acrylic ester monomer and azo-initiator; After dropwising, said temperature of reaction kettle is elevated to 70-80 ℃, insulation; Discharging gets into plate and frame(type)filter press and carries out press filtration, obtains finished product.
2. the preparation method of high withstand voltage breakdown performance aluminium pigment according to claim 1; It is characterized in that: in said step 2; The detailed process of said ball milling is earlier with the rotating speed ball milling of 60r/min 10 hours, is adjusted to 20r/min to said drum's speed of rotation then, and ball milling is 2 hours again.
3. the preparation method of high withstand voltage breakdown performance aluminium pigment according to claim 1 and 2 is characterized in that: in said step 1, said grinding medium is that diameter is the steel ball of 0.8mm-1.5mm; In said step 4, the time of said dropping process is 1 hour, and the time of said insulation is 2.5-3.5 hour.
4. the preparation method of high withstand voltage breakdown performance aluminium pigment according to claim 1 is characterized in that: described silane coupling agent is selected from a kind of in γ-methacryloxypropyl trimethoxy silane, vinyltriethoxysilane, vinyltrimethoxy silane, vinyl three (2-methoxy ethoxy) silane, the vinyl trimethoxysilane oligomer.
5. the preparation method of high withstand voltage breakdown performance aluminium pigment according to claim 1 is characterized in that: the weight part of described ball aluminum powder, environmentally friendly solvent oil, oleic acid or erucic acid, each composition of silane coupling agent is: ball aluminum powder 40-80 weight part; Environmentally friendly solvent oil 80-160 weight part; Oleic acid or erucic acid 0.2-0.5 weight part; Silane coupling agent 0.1-0.3 weight part.
6. the preparation method of high withstand voltage breakdown performance aluminium pigment according to claim 1, it is characterized in that: the weight part of said alcohols, ethers or esters solvent, said azo-initiator is: alcohols, ethers or esters solvent 120-200 weight part; Azo-initiator 0.05-0.09 weight part.
7. the preparation method of high withstand voltage breakdown performance aluminium pigment according to claim 1 is characterized in that: said environmentally friendly solvent grease separation one or more in D30, D40, D60, D70, D80 solvent oil.
8. the preparation method of high withstand voltage breakdown performance aluminium pigment according to claim 1 is characterized in that: said vinylformic acid or acrylic ester monomer are two or more in vinylformic acid, methylacrylic acid, TEB 3K, methyl acrylate, Bing Xisuandingzhi, Isooctyl methacrylate, lauryl methacrylate(LMA), isobornyl methacrylate, Rocryl 400, Rocryl 410, Viscoat 295, the trimethylolpropane trimethacrylate.
9. the preparation method of high withstand voltage breakdown performance aluminium pigment according to claim 1; It is characterized in that: said alcoholic solvent is selected from one or more in ethanol, n-propyl alcohol, the Virahol; Said ether solvent is selected from one or more in ethylene glycol monobutyl ether, diethylene glycol monobutyl ether, propylene glycol monomethyl ether, Ucar 35 butyl ether, dipropylene glycol methyl ether, the dipropylene glycol ether, and said esters solvent is selected from one or both in N-BUTYL ACETATE, the 1-Methoxy-2-propyl acetate.
10. the preparation method of high withstand voltage breakdown performance aluminium pigment according to claim 1, it is characterized in that: described azo-initiator is selected from Diisopropyl azodicarboxylate, 2,2-azo two (methylbutyronitrile), 2, a kind of in the 2-azo (2, the 4-methyl pentane nitrile).
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Application publication date: 20120725 |