CN104387738B - A kind of preparation method of the laser powder of white laser straight forming material - Google Patents
A kind of preparation method of the laser powder of white laser straight forming material Download PDFInfo
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- CN104387738B CN104387738B CN201410661190.1A CN201410661190A CN104387738B CN 104387738 B CN104387738 B CN 104387738B CN 201410661190 A CN201410661190 A CN 201410661190A CN 104387738 B CN104387738 B CN 104387738B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L69/00—Compositions of polycarbonates; Compositions of derivatives of polycarbonates
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/08—Stabilised against heat, light or radiation or oxydation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
- C08L2205/035—Polymer mixtures characterised by other features containing three or more polymers in a blend containing four or more polymers in a blend
Abstract
The present invention relates to the preparation method of the laser powder of a kind of white laser straight forming material.Comprising: comprise the following steps: A: by mole the ratio that (%) is 10:0.1 ~ 2:0.5 ~ 2, pink salt compound, compound nantokite, aluminium salt compound poured in organic solvent and stirred addition 0.05% ~ 1% stabilizer, obtaining the mixed liquor containing pink salt；B: added in the mixed liquor containing pink salt by silicone oil and stir, wherein silicone oil is 1 ~ 20% with the mixed liquor weight ratio containing pink salt；Obtain the pink salt mixed liquor containing silicon；C: add 1 ~ 30% firming agent and join in the pink salt mixed liquor containing silicon, and stir；By the mixed liquor containing firming agent in 30 ~ 100 DEG C of temperature, after being aged 2 ~ 6 hours, obtain a kind of colloidal sol containing pink salt；The colloidal sol of gained is obtained colloid after filtering, colloid is dried, then pulverizes and i.e. obtain finished product.The inventive method is simple, and product temperature tolerance and solvent resistance.
Description
Technical field
The invention belongs to intelligent mobile phone antenna manufacturing technology field, specifically, relate to a kind of white laser straight forming
The preparation method of the laser powder of material.
Background technology
Laser direct structuring technique English abbreviation LDS (LASER DIRECT STRUCTRING), has been widely used for
The manufacture of antenna traces, it utilizes computer according to the motion of the shape TRAJECTORY CONTROL laser of conductive pattern, is thrown by laser and shine
On molded three-dimensional plastic device containing laser powder, at short notice, activated circuit pattern.This technology can be suitable for
In mobile phone industry, medical industry, Aero-Space industry, parts industry, sophisticated sensor, enterprise's printed circuit board row
The relevant industries such as industry, telecommunications；Produce in the industrialization of smart mobile phone industry at present；But prior art can only be made black
Color antenna for mobile phone plastics, and white antenna for mobile phone plastics can not be produced, and white antenna for mobile phone typically uses spraying or its other party
Formula generates, and causes cost to increase, and occurs, during use, the phenomenon that fades.
Summary of the invention
It is an object of the invention to solve the deficiencies in the prior art, it is provided that swashing of a kind of white laser straight forming material
The preparation method of light powder, this laser powder can be applied in engineering plastics Merlon (PC), manufactures white antenna for mobile phone material.
The technical scheme used for achieving the above object is:
The preparation method of the laser powder of a kind of white laser straight forming material, comprises the following steps:
A: by mole the ratio that (%) is 10:0.1 ~ 2:0.5 ~ 2 by pink salt compound, compound nantokite, aluminium salt
Compound is poured in organic solvent and stirs；(i.e. stabilizer accounts for add the stabilizer that weight ratio is 0.05% ~ 1% in whipping process
Now the 0.05% ~ 1% of other materials all wt), obtain the mixed liquor containing pink salt；
Wherein, the weight of described consumption of organic solvent for account for every other material summation (i.e. three kinds of metal salt compounds
Weight summation) 20% ~ 120%；It is preferably in a proportion of: 30% ~ 110%, more preferably ratio: 35% ~ 100%, most preferred ratio 40% ~
90%；
B: added in the mixed liquor containing pink salt by silicone oil and stir, wherein silicone oil is 1% with the mixed liquor weight ratio containing pink salt
~20%；Obtain the pink salt mixed liquor containing silicon；
C: add the firming agent that weight ratio is 1% ~ 30% and join in the pink salt mixed liquor containing silicon, and stir；To contain
The mixed liquor of firming agent, in 30 ~ 100 DEG C of temperature, obtains a kind of colloidal sol containing pink salt after being aged 2 ~ 6 hours；By the colloidal sol of gained
After filtering, obtain colloid, colloid is dried, then pulverizes and i.e. obtain finished product.
Preferably, described pink salt compound is in butter of tin, ethanol stannum, n-butyl alcohol stannum, propanol stannum, four isopropanol stannum
One or more the most several mixture；Mixture can be arbitrary proportion.
Preferably, described compound nantokite is isopropanol copper, basic copper carbonate, basic copper nitrate, copper chloride hydroxide, alkali
One or any several mixture in formula Schweinfurt green, cupric ethylene diamine tetraacetate sodium, alkali formula cupric phosphate；Mixture can be
Arbitrary proportion.
Preferably, described aluminium salt compound is in aluminium secondary butylate, butyl alcohol-tert aluminum, aluminum isopropylate., three aluminum ethylate .s, aluminium oxide
A kind of or the most several mixture；Mixture can be arbitrary proportion.
Preferably, described organic solvent is a kind of monohydric alcohol；It is preferably ethanol；Can also be ethanol, isopropanol, fourth
One or any several mixture in alcohol, isobutanol.
Preferably, described stabilizer be ethylene glycol, propylene glycol, Isosorbide-5-Nitrae butanediol, Α-positive pentanediol, acetic acid, acetyl, third
Mixture a kind of or the most several in ketone.
Preferably, described silicone oil is methyl-silicone oil, ethyl silicon oil, phenyl silicone oil, Methyl Hydrogen Polysiloxane Fluid, aminomethyl phenyl silicon
Oil, methylchlorophenyl silicone oil, MethylethoxylsiliconFluid Fluid, methyl trifluoro propyl silicone oil, methyl vinyl silicon oil, methylhydroxy silicon
One or any several mixture in oil, ethyl containing hydrogen silicone oil, hydroxyl hydrogen silicone oil.
Preferably, described firming agent be a kind of in tap water, pure water, deionized water or sodium hydrate aqueous solution or
The mixture that person is the most several.
Further, pink salt compound, compound nantokite, the molar percentage (%) of aluminium salt compound are: 10:0.2 ~
1.8:0.3~1.6；Preferred proportion is 9:0.3 ~ 1.5:0.3 ~ 1.2；More preferably ratio is 8:0.5 ~ 1:0.3 ~ 0.8.
Further, described silicone oil is 2 ~ 18% with the mixed liquor weight ratio containing pink salt, and preferred proportion 3 ~ 15% is more excellent
Selecting ratio is 5% ~ 10%.
Described stabilizer weight ratio consumption is 0.06% ~ 1.5%, and preferred proportion is 0.08% ~ 1.2%；More preferably ratio
It is 0.2% ~ 1%.
Described firming agent weight ratio consumption is 2% ~ 25%, and preferred proportion is 4% ~ 20%；More preferably ratio be 8% ~
15%。
Wherein, baking temperature is 35 ~ 110 DEG C, and preferable temperature is 35 ~ 100 DEG C；More preferably temperature is 45 ~ 90 DEG C, optimum
Temperature is 50 ~ 80 DEG C.Drying time is more than 0.5 hour.
During pulverizing, disintegrating apparatus is mechanical crusher or jet mill or grinder etc..
A kind of method manufacturing white polycarbonate engineering plastics, it is characterised in that: comprise the following steps:
Step one: by uniform to laser powder, polycarbonate, antioxidant 1010, irgasfos 168, toughener, mix lubricant
Obtaining mixture, its component ratio (weight ratio) is corresponding in turn to as 2% ~ 20%: 75% ~ 90%:0.1% ~ 0.8%:0.1% ~ 0.8%:
1% ~ 5%:0.2% ~ 1%；
Step 2: being extruded through double screw extruder by mixture, double screw extruder processing temperature is 260 ~ 280 DEG C,
Again through tank cooling and dicing；
Wherein, laser powder is the laser powder that said method makes.
The principle of the present invention: by miscellaneous for the compound containing metal alkoxide at pink salt compound, metal alkoxide meets Aquatic product unboiled water
Solve, along with the addition of firming agent constantly occurs polycondensation reaction to obtain cupric, aluminum, sila pink salt compound；Gained mixture warp
Cross drying and crushing.
The invention has the beneficial effects as follows: the cupric that produced, aluminum, silicon doped tin salt compound have the good (heatproof of temperature tolerance
Can reach 600 DEG C), solvent resistance good (having toluene, dimethylbenzene, butanone, butyl ester, ethyl acetate etc. insoluble in conventional organic solvent)
Controlled with particle size；The present invention may be used for engineering plastics, epoxy resin copper-clad plate, polyimide flex wiring board etc. and manufactures
3D stereo circuit, and intelligent mobile phone antenna material, medical device components, RFID RF identification element etc..
The laser powder mixture of the present invention is one kind of multiple doped with metal elements pink salt compounds, and products obtained therefrom particle diameter is can
To control in the widest scope, widen products application scope.
Pink salt compound used in the present invention includes butter of tin, ethanol stannum, n-butyl alcohol stannum, propanol stannum or four isopropanols
Stannum；Compound nantokite is isopropanol copper, basic copper carbonate, basic copper nitrate, copper chloride hydroxide and basic copper acetate, ethylenediamine tetraacetic
Copper acetate sodium or alkali formula cupric phosphate；Aluminium salt compound is aluminium secondary butylate, butyl alcohol-tert aluminum, aluminum isopropylate. three aluminum ethylate. or oxidation
Aluminum；These products the most easily wait until, and cost is cheap；Using organic solvent in step A can the most commercially
Buy；Stabilizer used the most also can have been bought, and the consumption of stabilizer is 0.06 ~ 1.5%, and preferred proportion is 0.08 ~ 1.2%；
More preferably ratio is 0.2 ~ 1%；If stabilizing agent dosage hardly results in uniform dispersion liquid less than 0.2%；If greater than 1% 3
Planting slaine can partly precipitated phenomenon；
Silicone oil used in step B includes methyl-silicone oil, ethyl silicon oil, phenyl silicone oil, Methyl Hydrogen Polysiloxane Fluid, methylbenzene
Base silicone oil, MethylethoxylsiliconFluid Fluid, methyl vinyl silicon oil, methylhydroxy silicone oil, ethyl containing hydrogen silicone oil, hydroxyl hydrogen silicone oil；
It is readily available on these product markets；The usage amount of silicone oil be weight ratio be 2 ~ 18%, preferred proportion 3 ~ 15% more preferably than
Example is 5 ~ 10%；If consumption less than 5% or more than 10% gained mixed liquor all can product cloudiness by-product product.
Firming agent used in step C is water or sodium hydrate aqueous solution；
Can be obtained by, through tri-steps of A B C, the colloidal sol that the present invention needs, be then passed through being dried, baking temperature is best
It is that the product obtained after drying is solid mass at 50 ~ 80 DEG C, then through selecting the reducing mechanism (machine that shearing force is bigger
Tool pulverizer, jet mill or grinder) product that mean diameter is at 1 ~ 30 micron can be obtained.
Detailed description of the invention
Further describe below in conjunction with embodiment.
Embodiment 1:
The preparation method of the laser powder of a kind of white laser straight forming material, comprises the following steps:
Step one, by mole the ratio that (%) is 10:0.1:0.5 by pink salt compound, compound nantokite, aluminium salt
Compound is poured organic solvent into and is obtained in mixed liquor and stir；In whipping process add weight be mixed liquor 0.05% ~
The stabilizer of 0.08%, obtains the mixed liquor containing pink salt；
Wherein, the weight of described consumption of organic solvent for account for every other material summation (i.e. three kinds of metal salt compounds
Weight summation) 20% ~ 25%；
B: added in the mixed liquor containing pink salt by silicone oil and stir, wherein silicone oil is 1% with the mixed liquor weight ratio containing pink salt
~3%；Obtain the pink salt mixed liquor containing silicon；
C: add 1% ~ 30% firming agent that weight is pink salt mixed liquor containing silicon in the pink salt mixed liquor containing silicon, and
Stirring；By the mixed liquor containing firming agent in 30 ~ 32 DEG C of temperature, after being aged 2 ~ 3 hours, obtain a kind of colloidal sol containing pink salt；Will
The colloidal sol of gained obtains colloid after filtering, and is dried colloid, then pulverizes and i.e. obtain mean diameter at 1 ~ 30 micron
Finished product.
Wherein, described pink salt compound is butter of tin, ethanol stannum, the mixture of n-butyl alcohol stannum；Mixture can be
Arbitrary proportion.
Described compound nantokite be basic copper nitrate, copper chloride hydroxide, basic copper acetate, cupric ethylene diamine tetraacetate sodium,
The mixture of alkali formula cupric phosphate；Mixture can be arbitrary proportion.
Described aluminium salt compound is the mixture of butyl alcohol-tert aluminum, aluminum isopropylate., aluminium oxide；Mixture can be arbitrarily than
Example.
Described organic solvent is isopropanol.
Described stabilizer is 1,4 butanediols, Α-positive pentanediol, acetic acid, acetyl, mixture of acetone.
Described silicone oil is methyl trifluoro propyl silicone oil, methyl vinyl silicon oil, methylhydroxy silicone oil, ethyl Silicon Containing Hydrogen
Mixture in oil, hydroxyl hydrogen silicone oil.Mixture can be arbitrary proportion.
Embodiment 2:
The preparation method of the laser powder of a kind of white laser straight forming material, comprises the following steps:
Step one, by mole the ratio that (%) is 10:1:0.5 by pink salt compound, compound nantokite, aluminium salt
Compound is poured in organic solvent and stirs；In whipping process, add 0.06% ~ 7% stabilizer, obtain the mixed liquor containing pink salt；
Wherein, the weight of described consumption of organic solvent for account for every other material summation (i.e. three kinds of metal salt compounds
Weight summation) 50% ~ 65%；
B: added in the mixed liquor containing pink salt by silicone oil and stir, wherein silicone oil is 5% with the mixed liquor weight ratio containing pink salt
~8%；Obtain the pink salt mixed liquor containing silicon；
C: add 10% ~ 12% firming agent of the pink salt mixed liquor that weight is silicon in the pink salt mixed liquor containing silicon, and stir
Mix；By the mixed liquor containing firming agent in 60 ~ 70 DEG C of temperature, after being aged 5 ~ 6 hours, obtain a kind of colloidal sol containing pink salt；By institute
The colloidal sol obtained obtains colloid after filtering, and is dried colloid, then pulverizes and i.e. obtain mean diameter at 1 ~ 30 micron
Finished product.
Wherein, described pink salt compound be n-butyl alcohol stannum, propanol stannum, four isopropanol stannum mixture；Mixture can
To be arbitrary proportion.
Described compound nantokite be basic copper nitrate, copper chloride hydroxide, basic copper acetate, cupric ethylene diamine tetraacetate sodium,
Alkali formula cupric phosphate mixture；Mixture can be arbitrary proportion.
Described aluminium salt compound is aluminium secondary butylate, butyl alcohol-tert aluminum, the mixture of aluminium oxide；Mixture can be arbitrarily than
Example.
Described organic solvent is the mixture of ethanol, isopropanol, butanol, isobutanol.This mixture can be with arbitrary proportion.
Described stabilizer is the mixture in 1,4 butanediols, Α-positive pentanediol, acetic acid, acetyl, acetone.
Described silicone oil is methyl-silicone oil, ethyl silicon oil, phenyl silicone oil, Methyl Hydrogen Polysiloxane Fluid, methyl phenyl silicone oil, hydroxyl
The mixture of containing hydrogen silicone oil.Mixture arbitrary proportion.
Embodiment 3:
The preparation method of the laser powder of a kind of white laser straight forming material, comprises the following steps:
Step one, by mole the ratio that (%) is 10:1.9 ~ 2:1.5 ~ 1.6 by pink salt compound, mantoquita chemical combination
Thing, aluminium salt compound are poured in organic solvent and stir；In whipping process, add 0.7% ~ 0.8% stabilizer, obtain containing pink salt
Mixed liquor；
Wherein, the weight of described consumption of organic solvent for account for every other material summation (i.e. three kinds of metal salt compounds
Weight summation) 110% ~ 120%；
B: being added in the mixed liquor containing pink salt by silicone oil and stir, wherein silicone oil with the mixed liquor weight ratio containing pink salt is
19%~20%；Obtain the pink salt mixed liquor containing silicon；
C: interpolation weight is that 29% ~ 30% firming agent of the pink salt mixed liquor containing silicon joins the pink salt mixed liquor containing silicon
In, and stir；By the mixed liquor containing firming agent in 90 ~ 100 DEG C of temperature, obtain a kind of containing pink salt after being aged 3 ~ 4 hours
Colloidal sol；The colloidal sol of gained is obtained colloid after filtering, colloid is dried, then pulverizes and i.e. obtain finished product.
Wherein, described pink salt compound is n-butyl alcohol stannum.
Described compound nantokite is the mixture of isopropanol copper, basic copper carbonate, basic copper nitrate；Mixture can be
Arbitrary proportion.
Described aluminium salt compound is aluminum isopropylate., three aluminum ethylate .s, the mixture of aluminium oxide；Mixture can be arbitrarily than
Example.
Described organic solvent is isobutanol.Stabilizer is Α-positive pentanediol, acetic acid, acetyl, mixture of acetone.Mixed
Compound can be arbitrary proportion.
Described silicone oil be Methyl Hydrogen Polysiloxane Fluid, methyl phenyl silicone oil, methylchlorophenyl silicone oil, MethylethoxylsiliconFluid Fluid,
Mixture in methyl trifluoro propyl silicone oil, methyl vinyl silicon oil, hydroxyl hydrogen silicone oil.Mixture can be arbitrary proportion.
Embodiment 4:
The preparation method of the laser powder of a kind of white laser straight forming material, comprises the following steps:
Step one, by mole the ratio that (%) is 10:0.2 ~ 0.3:1.8 ~ 2 by pink salt compound, mantoquita chemical combination
Thing, aluminium salt compound are poured in organic solvent and stir；In whipping process, add 0.9% ~ 1% stabilizer, obtain containing pink salt
Mixed liquor；
Wherein, the weight of described consumption of organic solvent for account for every other material summation (i.e. three kinds of metal salt compounds
Weight summation) 40% ~ 50%；
B: being added in the mixed liquor containing pink salt by silicone oil and stir, wherein silicone oil with the mixed liquor weight ratio containing pink salt is
19%~20%；Obtain the pink salt mixed liquor containing silicon；
C: add 28% ~ 30% firming agent that weight is pink salt mixed liquor containing silicon in the pink salt mixed liquor containing silicon,
And stir；By the mixed liquor containing firming agent in 30 ~ 35 DEG C of temperature, after being aged 2 ~ 3 hours, obtain a kind of colloidal sol containing pink salt；
The colloidal sol of gained is obtained colloid after filtering, colloid is dried, then pulverizes and i.e. obtain finished product.
Wherein, described pink salt compound is n-butyl alcohol stannum.Described compound nantokite is basic copper acetate.
Described aluminium salt compound is three aluminum ethylate .s.Described organic solvent is isobutanol.Described stabilizer is 1,4 fourths
Glycol.Described silicone oil is methylchlorophenyl silicone oil.
Embodiment 5:
The preparation method of the laser powder of a kind of white laser straight forming material, comprises the following steps:
Step one, by mole the ratio that (%) is 10:1.7 ~ 1.8:0.6 ~ 0.7 by pink salt compound, mantoquita chemical combination
Thing, aluminium salt compound are poured in organic solvent and stir；In whipping process, add 0.6% ~ 0.7% stabilizer, obtain containing pink salt
Mixed liquor；
Wherein, the weight of described consumption of organic solvent for account for every other material summation (i.e. three kinds of metal salt compounds
Weight summation) 70% ~ 85%；
B: added in the mixed liquor containing pink salt by silicone oil and stir, wherein silicone oil is 1% with the mixed liquor weight ratio containing pink salt
~2%；Obtain the pink salt mixed liquor containing silicon；
C: add 28% ~ 30% firming agent that weight is pink salt mixed liquor containing silicon in the pink salt mixed liquor containing silicon,
And stir；By the mixed liquor containing firming agent in 30 ~ 35 DEG C of temperature, after being aged 2 ~ 3 hours, obtain a kind of colloidal sol containing pink salt；
The colloidal sol of gained is obtained colloid after filtering, colloid is dried, then pulverizes and i.e. obtain finished product.
Wherein, described pink salt compound is propanol stannum.Described compound nantokite is basic copper carbonate.
Described aluminium salt compound is three aluminum ethylate .s.Described organic solvent isopropanol.Described stabilizer is acetone.Institute
The silicone oil stated is MethylethoxylsiliconFluid Fluid.
Embodiment 6:
The preparation method of the laser powder of a kind of white laser straight forming material, comprises the following steps:
Step one, by mole the ratio that (%) is 10:1.1 ~ 1.2:1.3 ~ 1.5 by pink salt compound, mantoquita chemical combination
Thing, aluminium salt compound are poured in organic solvent and stir；In whipping process, add 0.05% ~ 0.07% stabilizer, obtain stanniferous
The mixed liquor of salt；
Wherein, the weight of described consumption of organic solvent for account for every other material summation (i.e. three kinds of metal salt compounds
Weight summation) 100% ~ 120%；
B: being added in the mixed liquor containing pink salt by silicone oil and stir, wherein silicone oil with the mixed liquor weight ratio containing pink salt is
18%~20%；Obtain the pink salt mixed liquor containing silicon；
C: add 1% ~ 3% firming agent that weight is pink salt mixed liquor containing silicon in the pink salt mixed liquor containing silicon, and
Stirring；By the mixed liquor containing firming agent in 90 ~ 100 DEG C of temperature, after being aged 2 ~ 3 hours, obtain a kind of colloidal sol containing pink salt；
The colloidal sol of gained is obtained colloid after filtering, colloid is dried, then pulverizes and i.e. obtain finished product.
Described pink salt compound is the one in butter of tin, ethanol stannum, n-butyl alcohol stannum, propanol stannum, four isopropanol stannum
Or the mixture that any of the above is several；Mixture can be arbitrary proportion.
Described compound nantokite is isopropanol copper, basic copper carbonate, basic copper nitrate, copper chloride hydroxide, alkali formula acetic acid
One or any several mixture in copper, cupric ethylene diamine tetraacetate sodium, alkali formula cupric phosphate；Mixture can be arbitrarily than
Example.
Described aluminium salt compound is the one in aluminium secondary butylate, butyl alcohol-tert aluminum, aluminum isopropylate., three aluminum ethylate .s, aluminium oxide
Or the most several mixture；Mixture can be arbitrary proportion.
Described organic solvent is a kind of monohydric alcohol；It is preferably ethanol；Can also be ethanol, isopropanol, butanol, isobutanol
In one or any several mixture.
Described stabilizer is in ethylene glycol, propylene glycol, 1,4 butanediols, Α-positive pentanediol, acetic acid, acetyl, acetone one
Kind or the most several mixture.
Described silicone oil is methyl-silicone oil, ethyl silicon oil, phenyl silicone oil, Methyl Hydrogen Polysiloxane Fluid, methyl phenyl silicone oil, methyl
Chlorphenyl silicone oil, MethylethoxylsiliconFluid Fluid, methyl trifluoro propyl silicone oil, methyl vinyl silicon oil, methylhydroxy silicone oil, ethyl contain
One or any several mixture in hydrogen silicone oil, hydroxyl hydrogen silicone oil.
Embodiment 7:
The preparation method of the laser powder of a kind of white laser straight forming material, comprises the following steps:
Step one, by mole the ratio that (%) is 10:1.5 ~ 1.6:0.6 ~ 0.7 by pink salt compound, mantoquita chemical combination
Thing, aluminium salt compound are poured in organic solvent and stir；In whipping process, add 0.2% ~ 0.3% stabilizer, obtain containing pink salt
Mixed liquor；
Wherein, the weight of described consumption of organic solvent for account for every other material summation (i.e. three kinds of metal salt compounds
Weight summation) 70% ~ 80%；
B: added in the mixed liquor containing pink salt by silicone oil and stir, wherein silicone oil is 1% with the mixed liquor weight ratio containing pink salt
~2%；Obtain the pink salt mixed liquor containing silicon；
C: add 1% ~ 3% firming agent that weight is pink salt mixed liquor containing silicon in the pink salt mixed liquor containing silicon, and
Stirring；By the mixed liquor containing firming agent in 50 ~ 60 DEG C of temperature, after being aged 3 ~ 4 hours, obtain a kind of colloidal sol containing pink salt；Will
The colloidal sol of gained obtains colloid after filtering, and is dried colloid, then pulverizes and i.e. obtain finished product.
Described pink salt compound is ethanol stannum, n-butyl alcohol stannum, propanol stannum, the mixture of four isopropanol stannum；Mixture can
To be arbitrary proportion.
Described compound nantokite is copper chloride hydroxide, basic copper acetate, cupric ethylene diamine tetraacetate sodium, alkali formula cupric phosphate
Mixture；Mixture can be arbitrary proportion.
Described aluminium salt compound is the one in aluminium secondary butylate, butyl alcohol-tert aluminum, aluminum isopropylate., three aluminum ethylate .s, aluminium oxide
Or the most several mixture；Mixture can be arbitrary proportion.
Described organic solvent is isobutanol.
Described stabilizer is in ethylene glycol, propylene glycol, 1,4 butanediols, Α-positive pentanediol, acetic acid, acetyl, acetone one
Kind or the most several mixture.
Described silicone oil is methyl phenyl silicone oil, methylchlorophenyl silicone oil, MethylethoxylsiliconFluid Fluid, methyl trifluoro propyl silicon
One or any several in oil, methyl vinyl silicon oil, methylhydroxy silicone oil, ethyl containing hydrogen silicone oil, hydroxyl hydrogen silicone oil
Mixture.
Embodiment 8:
Equipped with in the 1000ml beaker of stirring paddle, add 350 grams of butters of tin, 10 grams of isopropanol copper, 20 gram of three ethanol
Aluminum and 300ml ethanol；Blender rotating speed is 1000rpm；Stir 20 minutes until mixed liquor stirs, simultaneously stirred
Journey addition several times is 1.9 grams of ethylene glycol；It is subsequently adding 19 grams of methylhydroxy silicone oil, stirs 20 minutes, be subsequently adding 40 grams
Deionized water；Stirring 10 minutes simultaneously；Gained mixed liquor is placed in the 70 DEG C of waters bath with thermostatic control of preprepared water temperature, ageing
Flaxen solids is obtained after 3 hours；Being that 50% sodium hydroxide solution cleans filtration by concentration, being then placed within temperature is 80
DEG C drying baker dries 30 minutes, is then passed through grinding and obtains the pale yellow powder that mean diameter is 15 microns, this pale yellow powder
It is labeled as a.
Embodiment 9:
350 grams of butters of tin, 10 grams of basic copper carbonates, 20 gram of three second is added in equipped with the 1000ml beaker of stirring paddle
Aluminium alcoholates and 300ml ethanol；Blender rotating speed is 1000rpm, stirs 20 minutes until mixed liquor stirs, simultaneously in stirring
Process addition is 2.5 grams of ethylene glycol；Be subsequently adding 20 grams of methylhydroxy silicone oil, stir 20 minutes, be subsequently adding 40 grams go from
Sub-water；Stirring 10 minutes simultaneously；Being placed in by gained mixed liquor in the 70 DEG C of waters bath with thermostatic control of preprepared water temperature, ageing 3 is little
Flaxen solids is obtained time after；With concentration be 50% sodium hydroxide solution clean filter, be then placed within temperature be 80 DEG C do
Dry case dries 30 minutes, is then passed through grinding and obtains the pale yellow powder that mean diameter is 15 microns, this pale yellow powder labelling
For b.
Embodiment 10:
350 grams of butters of tin, 10 grams of alkali formula cupric phosphates are added (from three combinations in equipped with the 1000ml beaker of stirring paddle
Work Sanlaser 9940), 20 gram of three aluminum ethylate. and 300ml ethanol；Blender rotating speed is 1000rpm, stirs 25 minutes until mixing
Conjunction liquid stirs, and in whipping process, addition is 3 grams of ethylene glycol several times simultaneously；It is subsequently adding 20 grams of methylhydroxy silicon
Oil, stirs 20 minutes, is subsequently adding 40 grams of deionized waters；Stirring 10 minutes simultaneously；Gained mixed liquor is placed in and prepares in advance
In good 70 DEG C of waters bath with thermostatic control of water temperature, after being aged 3 hours, obtain flaxen solids；It is 50% sodium hydroxide solution by concentration
Cleaning and filter, being then placed within temperature is to dry 30 minutes in 80 DEG C of drying baker, and it is 15 micro-for be then passed through grinding obtaining mean diameter
The pale yellow powder of rice, this pale yellow powder is labeled as c.
Embodiment 11:
Add 350 grams of butters of tin in equipped with the 1000ml beaker of stirring paddle, 10 grams of alkali formula cupric phosphates (close from three
Chemical industry Sanlaser 9940), 20 cut aluminium butoxides and 300ml ethanol；Blender rotating speed is 1000rpm, stirs 25 minutes directly
Stir to mixed liquor, be simultaneously 3 grams of ethylene glycol in whipping process addition；It is subsequently adding 20 grams of methylhydroxy silicone oil, stirs
Mix 20 minutes, be subsequently adding 40 grams of deionized waters；Stirring 10 minutes simultaneously；Gained mixed liquor is placed in preprepared water
In 70 DEG C of waters bath with thermostatic control of temperature, after being aged 3 hours, obtain flaxen solids；It is that 50% sodium hydroxide solution is cleaned by concentration
Filter, being then placed within temperature is to dry 30 minutes in 80 DEG C of drying baker, is then passed through grinding that to obtain mean diameter be 15 microns
Pale yellow powder, this pale yellow powder is labeled as d.
Embodiment 12:
350 grams of butters of tin, 10 grams of isopropanol copper, 20 gram of three aluminum ethylate. are added in equipped with the 1000ml beaker of stirring paddle
With 300ml ethanol；Blender rotating speed is 1000rpm, stirs 20 minutes until mixed liquor stirs, simultaneously at whipping process
Addition is 1.9 grams of ethylene glycol；Being subsequently adding 19 grams of methylhydroxy silicone oil, stir 20 minutes, being subsequently adding 40 grams of concentration is 5%
Sodium hydrate aqueous solution；Stirring 10 minutes simultaneously；Gained mixed liquor is placed in the 70 DEG C of waters bath with thermostatic control of preprepared water temperature
In, obtain flaxen solids after being aged 3 hours；It is that 50% sodium hydroxide solution cleans filtration by concentration, is then placed within
Temperature is to dry 30 minutes in 80 DEG C of drying baker, is then passed through grinding and obtains the pale yellow powder that mean diameter is 15 microns, should
Pale yellow powder is labeled as e.
Embodiment 13:
350 gram of four isopropanol stannum, 10 grams of isopropanol copper, 20 gram of three second is added in equipped with the 1000ml beaker of stirring paddle
Aluminium alcoholates and 300ml ethanol；Blender rotating speed is 1000rpm, stirs 20 minutes until mixed liquor stirs, simultaneously in stirring
Process addition is 1.9 grams of ethylene glycol；It is subsequently adding 19 grams of methylhydroxy silicone oil, stirs 20 minutes, be subsequently adding 40 grams of concentration
It it is 5% sodium hydrate aqueous solution；Stirring 10 minutes simultaneously；Gained mixed liquor is placed in 70 DEG C of constant temperature of preprepared water temperature
In water-bath, after being aged 3 hours, obtain flaxen solids；It is that 50% sodium hydroxide solution cleans filtration by concentration, then puts
Put and dry 30 minutes in temperature is 80 DEG C of drying baker, be then passed through grinding and obtain the yellowish toner that mean diameter is 15 microns
End, this pale yellow powder is labeled as f.
Embodiment 14: a kind of method manufacturing white polycarbonate engineering plastics；Comprise the following steps: step one: will swash
Light powder, polycarbonate, antioxidant 1010, irgasfos 168, toughener, mix lubricant uniformly obtain mixture, its composition ratio
Example (weight ratio) is corresponding in turn to as 8% ~ 9%: 88% ~ 90%:0.1% ~ 0.2%:0.1% ~ 0.3%:4% ~ 5%:0.2% ~ 0.3%；
Step 2: being extruded through double screw extruder by mixture, double screw extruder processing temperature is 260 ~ 280 DEG C,
Again through tank cooling and dicing；Obtain white polycarbonate engineering plastics.
Embodiment 15: a kind of method manufacturing white polycarbonate engineering plastics；Comprise the following steps: step one: will swash
Light powder, polycarbonate, antioxidant 1010, irgasfos 168, toughener, mix lubricant uniformly obtain mixture, its composition ratio
Example (weight ratio) is corresponding in turn to as 19% ~ 20%: 80% ~ 85%:0.3% ~ 0.5%:0.6% ~ 0.7%:1% ~ 1.2%:0.9% ~ 1%；
Step 2: being extruded through double screw extruder by mixture, double screw extruder processing temperature is 260 ~ 280 DEG C,
Again through tank cooling and dicing；Obtain white polycarbonate engineering plastics.
Embodiment 16: a kind of method manufacturing white polycarbonate engineering plastics；Comprise the following steps: step one: will swash
Light powder, polycarbonate, antioxidant 1010, irgasfos 168, toughener, mix lubricant uniformly obtain mixture, its composition ratio
Example (weight ratio) is corresponding in turn to as 15% ~ 17%: 78% ~ 82%:0.7% ~ 0.8%:0.2% ~ 0.3%:2% ~ 3%:0.6% ~ 0.7%；
Step 2: being extruded through double screw extruder by mixture, double screw extruder processing temperature is 260 ~ 280 DEG C,
Again through tank cooling and dicing；Obtain white polycarbonate engineering plastics.
Embodiment 17: a kind of method manufacturing white polycarbonate engineering plastics；Comprise the following steps: step one: will swash
Light powder, polycarbonate, antioxidant 1010, irgasfos 168, toughener, mix lubricant uniformly obtain mixture, its composition ratio
Example (weight ratio) is corresponding in turn to as 10% ~ 12%: 83% ~ 85%:0.2% ~ 0.3%:0.7% ~ 0.8%:4% ~ 5%:0.9% ~ 1%；
Step 2: being extruded through double screw extruder by mixture, double screw extruder processing temperature is 260 ~ 280 DEG C,
Again through tank cooling and dicing；Obtain white polycarbonate engineering plastics.
Embodiment 18: a kind of method manufacturing white polycarbonate engineering plastics；Comprise the following steps: step one: will swash
Light powder, polycarbonate, antioxidant 1010, irgasfos 168, toughener, mix lubricant uniformly obtain mixture, its composition ratio
Example (weight ratio) is corresponding in turn to as 19% ~ 20%: 88% ~ 90%:0.7% ~ 0.8%:0.7% ~ 0.8%:4.5% ~ 5%:0.9% ~ 1%；
Step 2: being extruded through double screw extruder by mixture, double screw extruder processing temperature is 260 ~ 280 DEG C,
Again through tank cooling and dicing；Obtain white polycarbonate engineering plastics.
Embodiment 19: a kind of method manufacturing white polycarbonate engineering plastics；Comprise the following steps: step one: will swash
Light powder, polycarbonate, antioxidant 1010, irgasfos 168, toughener, mix lubricant uniformly obtain mixture, its composition ratio
Example (weight ratio) be corresponding in turn to into: 16% ~ 17%: 80% ~ 82%:0.6% ~ 0.7%:0.7% ~ 0.8%:4.5% ~ 4.6%:0.2% ~
0.3%；
Step 2: being extruded through double screw extruder by mixture, double screw extruder processing temperature is 260 ~ 280 DEG C,
Again through tank cooling and dicing；Obtain white polycarbonate engineering plastics.
Embodiment 20: a kind of method manufacturing white polycarbonate engineering plastics；Comprise the following steps: step one: will swash
Light powder, polycarbonate, antioxidant 1010, irgasfos 168, toughener, mix lubricant uniformly obtain mixture, its composition ratio
Example (weight ratio) is corresponding in turn to as 16% ~ 17%: 80% ~ 90%:0.2% ~ 0.3%:0.1% ~ 0.2%:2% ~ 3%:0.2% ~ 0.4%；
Step 2: being extruded through double screw extruder by mixture, double screw extruder processing temperature is 260 ~ 280 DEG C,
Again through tank cooling and dicing；Obtain white polycarbonate engineering plastics.
Embodiment 21: a kind of method manufacturing white polycarbonate engineering plastics；
The most all of letter a, b, c, d, e, f correspond respectively to the code name of the product of embodiment 8 to embodiment 13；?
Application case has with material:
Polycarbonate EGN2030R2 Mitsubishi engineering Plastics Co., Ltd
Antioxidant 1010 is commercially available
Irgasfos 168 is commercially available
Toughener MBS Japan's clock deep pool chemistry
Base company of lubricant PETS Italy
Laser powder Sanlaser 9940 Dongguan City three combination Gong You company (as a comparison case)
Making step is
By product of the present invention and polycarbonate, antioxidant 1076 168, toughener, lubricant is by such as the weight of following table one
Amount is than (%) mix homogeneously；To extrude through double screw extruder (Nanjing Jie Ente electromechanics company limited), processing temperature is 260 ~
280 DEG C, through tank cooling and dicing；
Table one:
| Dispensing component | 1# | 2# | 3# | 4# | 5# | 6# | 7# comparative example |
| PC | 82 | 82 | 82 | 82 | 82 | 82 | 86 |
| MBS | 5 | 5 | 5 | 5 | 5 | 5 | 5 |
| 1010 | 0.3 | 0.3 | 0.3 | 0.3 | 0.3 | 0.3 | 0.3 |
| 168 | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 | 0.2 |
| PETS | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 | 0.5 |
| a | 12 | ||||||
| b | 12 | ||||||
| c | 12 | ||||||
| d | 12 | ||||||
| e | 12 | ||||||
| f | 12 | ||||||
| 9940 | 8 | ||||||
| L* | 75.2 | 73.6 | 76.4 | 72.5 | 70.6 | 74.5 | 60.2 |
Relevant L* illustrate: Lab color space by International Commission on Illumination (CIE) in 1976 formulate, it be with L*,
Tri-mutually perpendicular coordinate axess of a*, b* represent a color space, and L* axle represents lightness, black in bottom, in vain on top.+
A* represents magenta, and ~ a* represents green, and+b* represents yellow, and ~ b* represents blue, and a* axle is red-green colour axis, and b* axle is yellow one
The corresponding relation that color is described in numerically by blue axle Lab with LCH will be discussed in detail at Part III.The color of any color
Can represent with a*, b* numerical value with feature mutually, any color in nature can be described with tri-numerical value of L*, a*, b*
L* value is in the range of 100 (in vain) to 0 (black), and the excursion of a* and b* is from 100 to 100.Arbitrary color can be with in space
L*, a*, b* of corresponding point determine.
From table 1 it follows that the material manufactured with existing laser powder 9940 with the product manufacturing PC engineering plastics of the present invention
Material contrast is closer to white (L* value is the highest more good).
Claims (7)
1. the preparation method of the laser powder of a white laser straight forming material, it is characterised in that: comprise the following steps:
Step one: by mole the ratio that (%) is 10:0.1 ~ 2:0.5 ~ 2 by pink salt compound, compound nantokite, aluminium salt
Compound is poured in organic solvent and stirs；Adding weight ratio in whipping process is the stabilizer of 0.05% ~ 1%, obtains stanniferous
The mixed liquor of salt；
Wherein, the weight of described consumption of organic solvent is the 20% ~ 120% of other all material summations；
Step 2: being added in the mixed liquor containing pink salt by silicone oil and stir, wherein silicone oil with the mixed liquor weight ratio containing pink salt is
1%~20%；Obtain the pink salt mixed liquor containing silicon；
Step 3: add the firming agent that weight ratio is 1% ~ 30% and join in the pink salt mixed liquor containing silicon, and stir；To contain
The mixed liquor of firming agent, in 30 ~ 100 DEG C of temperature, obtains the colloidal sol containing pink salt after being aged 2 ~ 6 hours；The colloidal sol of gained is passed through
Obtain colloid after filtration, colloid is dried, then pulverize and i.e. obtain finished product；
Described pink salt compound be the one in butter of tin, ethanol stannum, n-butyl alcohol stannum, propanol stannum, four isopropanol stannum or with
On the most several mixture；
Described compound nantokite is isopropanol copper, basic copper carbonate, basic copper nitrate, copper chloride hydroxide, basic copper acetate, second
One or any several mixture in ethylenediamine tetraacetic acid (EDTA) copper sodium, alkali formula cupric phosphate；
Described aluminium salt compound is the one in aluminium secondary butylate, butyl alcohol-tert aluminum, aluminum isopropylate., three aluminum ethylate .s, aluminium oxide or appoints
Anticipate several mixture.
The preparation method of the laser powder of a kind of white laser straight forming material the most according to claim 1, its feature
It is: described organic solvent is one or any several mixture in ethanol, isopropanol, butanol, isobutanol.
The preparation method of the laser powder of a kind of white laser straight forming material the most according to claim 1, its feature
Be: described stabilizer be a kind of in ethylene glycol, propylene glycol, 1,4 butanediols, Α-positive pentanediol, acetic acid, acetyl, acetone or
The most several mixture.
The preparation method of the laser powder of a kind of white laser straight forming material the most according to claim 1, its feature
It is: described silicone oil is methyl-silicone oil, ethyl silicon oil, phenyl silicone oil, Methyl Hydrogen Polysiloxane Fluid, methyl phenyl silicone oil, methyl chloride
Phenyl silicone oil, MethylethoxylsiliconFluid Fluid, methyl trifluoro propyl silicone oil, methyl vinyl silicon oil, methylhydroxy silicone oil, ethyl are hydrogeneous
One or any several mixture in silicone oil, hydroxyl hydrogen silicone oil.
The preparation method of the laser powder of a kind of white laser straight forming material the most according to claim 1, its feature
It is: described firming agent is one or any several in tap water, pure water, deionized water or sodium hydrate aqueous solution
Mixture.
The preparation method of the laser powder of a kind of white laser straight forming material the most according to claim 1, its feature
It is: pink salt compound, compound nantokite, the molar percentage (%) of aluminium salt compound be: 10:0.2 ~ 1.8:0.3 ~ 1.6.
7. the method manufacturing white polycarbonate engineering plastics, it is characterised in that: comprise the following steps:
Step one: laser powder, polycarbonate, antioxidant 1010, irgasfos 168, toughener, mix lubricant are uniformly obtained
Mixture, its component ratio weight ratio is corresponding in turn to as 2% ~ 20%: 75% ~ 90%:0.1% ~ 0.8%:0.1% ~ 0.8%:1% ~ 5%:
0.2%~1%；
Step 2: being extruded through double screw extruder by mixture, double screw extruder processing temperature is 260 ~ 280 DEG C, then warp
Cross tank cooling and dicing；
Wherein, laser powder is the laser powder of preparation any one of claim 1 to 6.
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| CN106928682B (en) * | 2017-03-01 | 2019-04-23 | 无锡赢同新材料科技有限公司 | A kind of laser direct forming material and preparation method thereof with good comprehensive performance |
| DE102017106913A1 (en) | 2017-03-30 | 2018-10-04 | Chemische Fabrik Budenheim Kg | Process for the production of electrically conductive structures on a carrier material |
| CN107083040A (en) * | 2017-05-12 | 2017-08-22 | 佛山市合宏泰业科技有限公司 | It is a kind of for PC fire proofings of laser carving and preparation method thereof |
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