CN105199564B - A kind of powder thermosetting electromagnetic screen coating - Google Patents
A kind of powder thermosetting electromagnetic screen coating Download PDFInfo
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- CN105199564B CN105199564B CN201510738122.5A CN201510738122A CN105199564B CN 105199564 B CN105199564 B CN 105199564B CN 201510738122 A CN201510738122 A CN 201510738122A CN 105199564 B CN105199564 B CN 105199564B
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Abstract
The present invention discloses a kind of powder thermosetting electromagnetic screen coating, and its raw material and mass parts are：0.15 1.6 parts of curing agent, 15 30 parts of hybrid resin, 5 20 parts of silver-coated copper powder, 10 40 parts of nickel powder, 1 5.5 parts of levelling agent, 1 2.5 parts of titanate coupling agent, 20 45 parts of mixed solvent, disperse anti-heavy 0.1 0.6 parts of agent, 0.001 0.005 parts of antioxidant.Due to replacing copper-clad silver powder, and the micron order copper-clad silver powder used to replace nanoscale silver-coated copper powder conventional in existing electromagnetic screen coating using nickel powder, cost of material has been greatly reduced.
Description
Technical field
The invention belongs to electromagnetic screen coating technical field, and in particular to a kind of powder thermosetting electromagnetic screen coating.
Background technology
With electronics, the high speed development of electrical equipment industry, various commercial and domestic electronic appliances quantity sharply increase, and one, electricity
Magnetic disturbance has formed a kind of new social effects of pollution to human body with electromagnetic compatibility effect；2nd, between electronic apparatus signal mutual interference also into
For the key issue to be paid close attention to of Product Safety reliability.Due to being miniaturized of electronic circuit and element, integrated, lightweight and
Digitlization, used electric current is weak current, and it controls the power of the power and external electromagnetic wave noise of signal to be close, because
This, which is easily caused, can not identify useful signal even erroneous judgement of useful signal etc.；On the other hand, these electronic products in itself also to
The electromagnetic wave of outer transmitting different frequency, can to electronic computer and other communications, electric equipment of neighbouring operation etc. to cause to do
Disturb.Because the case material of the electronic product used at present instead of by substantial amounts of plastic products or similar high polymer material
Metal or other effective shielding materials originally, and common high molecular materials are insulator, electromagnetic wave can hardly be absorbed and
Reflection, does not possess function of shielding, in order to solve this problem, coating of the research and development with electro-magnetic screen function, coated on electricity
Sub- utensil corresponding site shields electromagnetic interference, is a kind of effective method.
Though existing a small amount of scientific research at present is reported with Lab Products, can practical application there is good electromagnetic shielding to imitate
The industrialization product of fruit steady quality is rare.
Worldwide, current silver system shielding coating product is more ripe, and its is expensive, and general service is difficult to bear
Great number cost, and the defects of essence in itself be present in silver system product：Product easily produces precipitation after matching somebody with somebody glue, and existing with migration
As occurring.Though Recent study gets along with, have no that industrialization matured product is largely used to production practices (Zhao Bin etc., ultra-fine silver
Application of the powder in electrically-conducting paint, coating technology, 2000, (1)：40)；Nickel system shielding coating existing market has certain batch sales,
But it is bad in the low frequency range shield effectiveness less than 30MHz, then because its electric conductivity is poor, shield effectiveness is relatively low, but be current
Shielding coating leading products；Copper system shielding coating shield effectiveness is high, and has price advantage, and silver migration, which is also not present, influences coating
Can problem, therefore gradually exploitation increases copper system product, but causes performance unstable as practical application because copper is easily oxidized
Subject matter；Carbon system and composite coating research at the early-stage do not have industrialization product.Furthermore current existing the said goods
Only formed using acrylic resin or fluorine resin as base-material, limit its scope of application.
The content of the invention
In view of the shortcomings of the prior art, it is an object of the invention to provide a kind of powder thermosetting electromagnetic screen coating, its
The whole occasions that can be used suitable for thermosetting powder coating, there can be electro-magnetic screen function using object.
To achieve the above object, the present invention adopts the following technical scheme that：
A kind of powder thermosetting electromagnetic screen coating, its raw material and mass parts are：Curing agent 0.15-1.6 parts, hybrid resin
15-30 parts, silver-coated copper powder 5-20 parts, nickel powder 10-40 parts, levelling agent 1-5.5 parts, titanate coupling agent 1-2.5 parts, mixed solvent
20-45 parts, disperse anti-heavy agent 0.1-0.6 parts, antioxidant 0.001-0.005 parts；
The nickel powder quality accounts for the 60-70% of the quality sum of whole metal dusts i.e. nickel powder and silver-coated copper powder, further
Preferably 67%；
Silver-colored volumn concentration is 5-30% in the silver-coated copper powder, 38-53 μm of particle diameter；
The nickel powder particle diameter is 38-53 μm；
The curing agent is selected from one or both of 2-methylimidazole, 2- benzylimidazolines；
The hybrid resin is the mixture of polyester resin and epoxy resin, and the mass ratio of polyester resin and epoxy resin is
1:1-4:1, preferred polyester resin:The mass ratio of epoxy resin is 1:1,3:2,7:3,4:1；
The mixed solvent is water, polyethoxy octylphenol ether, the mixture of ethyl carbitol, water, polyethoxy octyl group
Phenolic ether, the mass ratio of ethyl carbitol are 1：1：1；
The antioxidant is selected from three (2,4- di-t-butyls) phenyl-phosphites, double (2,4- di-tert-butyl-phenyls) Ji Wusi
One or both of alcohol diphosphites；
A kind of preparation method of powder thermosetting electromagnetic screen coating, step include：
A, by the silver-coated copper powder cleaned up and nickel powder it is well mixed after, add titanate coupling agent and even with titanate esters
Join the isopropanol of agent equivalent, be uniformly mixed；
B, half amount mixed solvent, a quarter amount levelling agent are added in compound made from step A, are stirred mixed
Close；
C, the hybrid resin powder of half amount and the levelling agent of a quarter amount and remaining mixed solvent are added
Enter in compound made from step B, be stirred mixing；
D, after compound made from step C being dried into processing, carry out fine gtinding and reach more than 300 mesh, sieving；
E, compound made from step D is added into remaining hybrid resin powder and levelling agent, adds scattered anti-heavy agent
And antioxidant, it is put into high-speed stirring mixer stirring and make it that material is well mixed, and then adds curing agent, continues stirring and mix
Close uniform；
F, compound made from step E is subjected to melting extrusion mixed processing, extruded stock is cooled down, crushed, then will squeezed
Discharging carries out pulverization process to 300 mesh.
Silver-coated copper powder overcomes the defects of copper powder is oxidizable, have it is conductive it is good, chemical stability is high, it is not oxidizable,
The good characteristics such as price is low.
Under normal circumstances, shield effectiveness of the nickel powder in powder thermosetting electromagnetic screen coating is not so good as copper powder and silver powder, with
The nickel powder of equal parts substitutes silver-coated copper powder shielding properties and will reduced, but inventor has found that in raw material proportioning of the present invention nickel powder contains
When measuring the 60-70% for the quality sum for accounting for nickel powder and silver-coated copper powder, the shield effectiveness of coating reaches more than 90dB, unexpected to improve
, particularly when nickel powder accounts for whole metal dusts and reaches 67% dosage, cover efficiency and reached 95dB.Due to using nickel powder generation
For copper-clad silver powder, and the micron order copper-clad silver powder used replaces nanometer-level silver copper-clad conventional in existing electromagnetic screen coating
Powder, cost of material has been greatly reduced it.
Embodiment
Embodiment 1
A kind of powder thermosetting electromagnetic screen coating, its raw material and mass parts are：2-methylimidazole, 2- benzylimidazolines are each
0.13 part, hybrid resin (polyester resin：Epoxy resin ratio 1:1, Anhui Shenjian New Material Co., Ltd., mix type ring
Oxygen curing polyester resin, SJ3A) 18.97 parts, silver-coated copper powder (Li Hongjin Science and Technology Ltd.s of Shenzhen, Li-0103) 16.42
Part, 37.25 parts of nickel powder (Beijing Xin Rongyuan Science and Technology Ltd.s, 300 height of eye pure nickel powders), levelling agent (Modaflow Powder
III, U.S. SOLUTIA, N- (1,3-DIMETHYLBUTYL)-N'-PHENYL-P-PHENYLENEDIAMINE) 1.68 parts, titanium
1.32 parts of acid esters coupling agent (Nanjing You Pu Chemical Co., Ltd.s, three iso stearate isopropyl titanates, UP-130), by water, poly- second
Epoxide octylphenol ether, ethyl carbitol are with mass ratio 1：1：30.34 parts of the mixed solvent of 1 composition, disperseing anti-heavy agent, (Linan City is blue or green
The anti-heavy agent of Hong Huagongzhujichang, CP-88.118 solvent based coating) 0.6 part, three (2,4- di-t-butyl) phenyl-phosphites 0.003
Part.
The preparation method of powder thermosetting electromagnetic screen coating is as follows：
Silver-coated copper powder is taken, surface cleaning processing is done in glass jar body with organic solvent-acetone, it is ensured that surface is dirty without greasy dirt
Dye.In kind handle nickel powder.Then the two is evaporated acetone solvent totally at 60 DEG C in low temperature baking oven；
Using V-arrangement metal dust batch mixer, mixed, first (100 turns/min) stirring 5min of low speed, rear high speed (1000
Turn/min) stirring 10min, again (100 turns/min) stirring 5min of low speed, make it well mixed；
Whole amount coupling agent is added, adds the isopropanol with titanate coupling agent equivalent, (120 turns/min) stirrings of low speed
20min, it is standby；
The mixed solvent of half amount is added in above-mentioned mixed powder, the levelling agent of a quarter amount is added, in solid-liquid
Mixing 20min is stirred in mixing and blending machine；
By the levelling agent of the hybrid resin powder of half amount and a quarter amount, and remaining mixed solvent, in addition
Compound made from one step, (1200 turns/min) 10min is mixed in blender；
After mixed material is dried into processing 3h in drying box, fine gtinding is carried out in super fine machine
20min, when reaching more than 300 mesh, sieving；
Remaining polyester resin powder and levelling agent are added in obtained material in rapid one step up, it is scattered anti-heavy to add
Agent, antioxidant, high-speed stirred type mixer is put into, 2800 turns/min of rotating speed, 3min is handled, then adds curing agent, is continued
2min is stirred, is well mixed.
Coating melting extrusion mixing manufacture is carried out using thermosetting powder coating production line, wherein master operation is：Become spiral shell
Line reverse double screw extruder obtained material in previous step is carried out melting extrusion mixed processing (90 DEG C of area's temperature, two
110 DEG C of area's temperature, three area's temperature：100℃；Double-screw extruder screw rotating speed is controlled by main motor, main motor rotating speed 3000r/
Min), the material of extrusion through cooling down, it is broken after, handled into ball mill and micronizer twice technique so that terminal
Product granularity reaches 300 mesh, standby.
Shield effectiveness experiment is carried out using the powder thermosetting electromagnetic screen coating of preparation, the shield effectiveness for detecting coating is
90dB。
Specific detection method is according to GB/T 30142-2013《Plane electromagnetic shielding material shield effectiveness measuring method》It is real
Apply.
Embodiment 2
A kind of powder thermosetting electromagnetic screen coating, its raw material and mass parts are：1.16 parts of 2-methylimidazole, hybrid resin
(polyester resin：Epoxy resin ratio 3:2, Anhui Shenjian New Material Co., Ltd., mixed type curable epoxide polyester resin,
SJ5A) 22.83 parts, 17.75 parts of silver-coated copper powder, nickel powder 27.45 parts (60.7%), 1.33 parts of levelling agent, titanate coupling agent 1.9
Part, by water, polyethoxy octylphenol ether, ethyl carbitol with mass ratio 1：1：33.13 parts of the mixed solvent of 1 composition, disperse anti-
Heavy 0.42 part of agent, three 0.003 part of (2,4- di-t-butyl) phenyl-phosphites；
The preparation method of powder thermosetting electromagnetic screen coating is as follows：
Silver-coated copper powder is taken, surface cleaning processing is done in glass jar body with organic solvent-acetone, it is ensured that surface is dirty without greasy dirt
Dye.In kind handle nickel powder.Then the two is evaporated acetone solvent totally at 60 DEG C in low temperature baking oven；
Using V-arrangement metal dust batch mixer, mixed, first (100 turns/min) stirring 5min of low speed, rear high speed (1000
Turn/min) stirring 10min, again (100 turns/min) stirring 5min of low speed, make it well mixed；
Whole amount coupling agent is added, adds the isopropanol with titanate coupling agent equivalent, (120 turns/min) stirrings of low speed
20min, it is standby；
The mixed solvent of half amount is added in above-mentioned mixed powder, the levelling agent of a quarter amount is added, in solid-liquid
Mixing 20min is stirred in mixing and blending machine；
By the levelling agent of the hybrid resin powder of half amount and a quarter amount, and remaining mixed solvent, in addition
Compound made from one step, (1200 turns/min) 10min is mixed in blender；
After mixed material is dried into processing 5h in drying box, fine gtinding is carried out in super fine machine
20min, when reaching more than 300 mesh, sieving；
Remaining polyester resin powder and levelling agent are added in obtained material in rapid one step up, it is scattered anti-heavy to add
Agent, antioxidant, high-speed stirred type mixer is put into, 2800 turns/min of rotating speed, 5min is handled, then adds curing agent, is continued
1min is stirred, is well mixed.
Coating melting extrusion mixing manufacture, master operation are carried out using thermosetting powder coating production line：It is reverse to become screw thread
Double screw extruder carries out melting extrusion mixed processing (95 DEG C of area's temperature, two area's temperature to obtained material in previous step
115 DEG C, three area's temperature：110℃；Double-screw extruder screw rotating speed is controlled by main motor, main motor rotating speed 2500r/min), squeeze
The material gone out through cooling down, it is broken after, handled into ball mill and micronizer twice technique so that end product granularity
Reach 300 mesh, it is standby.
The shield effectiveness for detecting coating is 92dB.
Embodiment 3
A kind of powder thermosetting electromagnetic screen coating, its raw material and mass parts are：1.5 parts of 2-methylimidazole, hybrid resin
(polyester resin：Epoxy resin ratio 7:3, Anhui Shenjian New Material Co., Ltd., mixed type curable epoxide polyester resin,
SJ6A) 22.83 parts, 20.32 parts of silver-coated copper powder, nickel powder 40.50 parts (66.6%), 5 parts of levelling agent, titanate coupling agent 2.03
Part, by water, polyethoxy octylphenol ether, ethyl carbitol with mass ratio 1：1：40.72 parts of the mixed solvent of 1 composition, disperse anti-
Heavy 0.5 part of agent, three 0.002 part of (2,4- di-t-butyl) phenyl-phosphites；
The preparation method of powder thermosetting electromagnetic screen coating is as follows：
Silver-coated copper powder is taken, surface cleaning processing is done in glass jar body with organic solvent-acetone, it is ensured that surface is dirty without greasy dirt
Dye.In kind handle nickel powder.Then the two is evaporated acetone solvent totally at 60 DEG C in low temperature baking oven；
Using V-arrangement metal dust batch mixer, mixed, first (100 turns/min) stirring 5min of low speed, rear high speed (1000
Turn/min) stirring 10min, again (100 turns/min) stirring 5min of low speed, make it well mixed；
Whole amount coupling agent is added, adds the isopropanol with titanate coupling agent equivalent, (120 turns/min) stirrings of low speed
20min, it is standby；
The mixed solvent of half amount is added in above-mentioned mixed powder, the levelling agent of a quarter amount is added, in solid-liquid
Mixing 20min is stirred in mixing and blending machine；
By the levelling agent of the hybrid resin powder of half amount and a quarter amount, and remaining mixed solvent, in addition
Compound made from one step, (1200 turns/min) 10min is mixed in blender；
After mixed material is dried into processing 5h in drying box, fine gtinding is carried out in super fine machine
20min, when reaching more than 300 mesh, sieving；
Remaining polyester resin powder and levelling agent are added in obtained material in rapid one step up, it is scattered anti-heavy to add
Agent, antioxidant, high-speed stirred type mixer is put into, 2800 turns/min of rotating speed, 4min is handled, then adds curing agent, is continued
2min is stirred, is well mixed.
Coating melting extrusion mixing manufacture, master operation are carried out using thermosetting powder coating production line：It is reverse to become screw thread
Double screw extruder carries out melting extrusion mixed processing (100 DEG C of area's temperature, two area's temperature to obtained material in previous step
120 DEG C, three area's temperature：115℃；Double-screw extruder screw rotating speed is controlled by main motor, main motor rotating speed 3500r/min), squeeze
The material gone out through cooling down, it is broken after, handled into ball mill and micronizer twice technique so that end product granularity
Reach 300 mesh, it is standby.
The shield effectiveness for detecting coating is 95dB.
Embodiment 4
A kind of powder thermosetting electromagnetic screen coating, its raw material and mass parts are：2-methylimidazole, 2- benzylimidazolines are each
0.6 part, hybrid resin (polyester resin：Epoxy resin ratio 4:1, Anhui Shenjian New Material Co., Ltd., mixed type epoxy
Curing polyester resin, SJ6BDT) 26.05 parts, 8.5 parts of silver-coated copper powder, nickel powder 19 parts (69%), 3 parts of levelling agent, titanate esters coupling
1.46 parts of agent, by water, polyethoxy octylphenol ether, ethyl carbitol with mass ratio 1:1:35 parts of the mixed solvent of 1 composition, disperses
Anti- heavy 0.2 part of agent, double 0.004 part of (2,4- di-tert-butyl-phenyl) pentaerythritol diphosphites；
The preparation method of powder thermosetting electromagnetic screen coating is as follows：
Silver-coated copper powder is taken, surface cleaning processing is done in glass jar body with organic solvent-acetone, it is ensured that surface is dirty without greasy dirt
Dye.In kind handle nickel powder.Then the two is evaporated acetone solvent totally at 60 DEG C in low temperature baking oven；
Using V-arrangement metal dust batch mixer, mixed, first (100 turns/min) stirring 5min of low speed, rear high speed (1000
Turn/min) stirring 10min, again (100 turns/min) stirring 5min of low speed, make it well mixed；
Whole amount coupling agent is added, adds the isopropanol with titanate coupling agent equivalent, (120 turns/min) stirrings of low speed
20min, it is standby；
The mixed solvent of half amount is added in above-mentioned mixed powder, the levelling agent of a quarter amount is added, in solid-liquid
Mixing 20min is stirred in mixing and blending machine；
By the levelling agent of the hybrid resin powder of half amount and a quarter amount, and remaining mixed solvent, in addition
Compound made from one step, (1200 turns/min) 10min is mixed in blender；
After mixed material is dried into processing 3h in drying box, fine gtinding is carried out in super fine machine
20min, when reaching more than 300 mesh, sieving；
Remaining polyester resin powder and levelling agent are added in obtained material in rapid one step up, it is scattered anti-heavy to add
Agent, antioxidant, high-speed stirred type mixer is put into, 2800 turns/min of rotating speed, 4min is handled, then adds curing agent, is continued
2min is stirred, is well mixed.
Coating melting extrusion mixing manufacture, master operation are carried out using thermosetting powder coating production line：It is reverse to become screw thread
Double screw extruder carries out melting extrusion mixed processing (90 DEG C of area's temperature, two area's temperature to obtained material in previous step
110 DEG C, three area's temperature：100℃；Double-screw extruder screw rotating speed is controlled by main motor, main motor rotating speed 4000r/min), squeeze
The material gone out through cooling down, it is broken after, handled into ball mill and micronizer twice technique so that end product granularity
Reach 300 mesh, it is standby.
The shield effectiveness for detecting coating is 91dB.
Comparative example：
Coating raw material with when preparation method substantially with embodiment 3, difference be in the silver-coated copper powder for using equivalent respectively and
Nickel powder replaces the compound of silver-coated copper powder and nickel powder, i.e., simple to use silver-coated copper powder, nickel powder then to detect system as shielding metal
The shield effectiveness of the shielding coating obtained, it is 96dB to use silver-coated copper powder merely as the shield effectiveness of the coating of shielding metal；It is single
The shield effectiveness of the pure coating using nickel powder as shielding metal is 75dB.
Claims (8)
1. a kind of powder thermosetting electromagnetic screen coating, its raw material and mass parts are：Curing agent 0.15-1.6 parts, hybrid resin
15-30 parts, silver-coated copper powder 5-20 parts, nickel powder 10-40 parts, levelling agent 1-5.5 parts, titanate coupling agent 1-2.5 parts, mixed solvent
20-45 parts, disperse anti-heavy agent 0.1-0.6 parts, antioxidant 0.001-0.005 parts；The nickel powder quality accounts for whole metal dusts
That is the 60-70% of the quality sum of nickel powder and silver-coated copper powder.
2. electromagnetic screen coating as claimed in claim 1, it is characterised in that：The nickel powder quality accounts for whole metal dusts i.e. nickel
The 67% of the quality sum of powder and silver-coated copper powder.
3. electromagnetic screen coating as claimed in claim 1, it is characterised in that：Silver-colored volumn concentration in the silver-coated copper powder
For 5-30%, 38-53 μm of particle diameter；The nickel powder particle diameter is 38-53 μm.
4. electromagnetic screen coating as claimed in claim 1, it is characterised in that：The curing agent is selected from 2-methylimidazole, 2- benzene
One or both of base imidazoline.
5. electromagnetic screen coating as claimed in claim 1, it is characterised in that：The hybrid resin is polyester resin and asphalt mixtures modified by epoxy resin
The mass ratio of the mixture of fat, polyester resin and epoxy resin is 1:1-4:1.
6. electromagnetic screen coating as claimed in claim 1, it is characterised in that：The mixed solvent is water, polyethoxy octyl group
The mixture of phenolic ether, ethyl carbitol, water, polyethoxy octylphenol ether, the mass ratio of ethyl carbitol are 1：1：1.
7. electromagnetic screen coating as claimed in claim 1, it is characterised in that：The antioxidant is selected from three (bis- tertiary fourths of 2,4-
Base) phenyl-phosphite, one or both of double (2,4- di-tert-butyl-phenyls) pentaerythritol diphosphites.
8. the electromagnetic screen coating as described in claim any one of 1-7, it is characterised in that：The electromagnetic screen coating by with
It is prepared by lower method and step：
A, after being well mixed the silver-coated copper powder cleaned up and nickel powder, titanate coupling agent and and titanate coupling agent are added
The isopropanol of equivalent, is uniformly mixed；
B, half amount mixed solvent, a quarter amount levelling agent are added in compound made from step A, is stirred mixing；
C, the levelling agent and remaining mixed solvent of the hybrid resin of half amount and a quarter amount are added into step B systems
In the compound obtained, mixing is stirred；
D, after compound made from step C being dried into processing, carry out fine gtinding and reach more than 300 mesh, sieving；
E, compound made from step D is added into remaining hybrid resin and levelling agent, adds scattered anti-heavy agent and anti-oxidant
Agent, stirring is put into high-speed stirring mixer so that material is well mixed, curing agent is then added, continues to be uniformly mixed；
F, compound made from step E is subjected to melting extrusion mixed processing, extruded stock is cooled down, crushed, then by extruded stock
Pulverization process is carried out to 300 mesh.
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| CN106010155A (en) * | 2016-07-14 | 2016-10-12 | 夏嘉伟 | Composite electromagnetic shielding conductive coating |
| CN107163629A (en) * | 2017-06-07 | 2017-09-15 | 合肥励仙电力工程有限公司 | It is a kind of for magnetic field shielding coating of distribution transformer and preparation method thereof |
| CN111138956A (en) * | 2019-12-23 | 2020-05-12 | 江阴市玲珑高分子材料有限公司 | Thermosetting powder electromagnetic shielding coating |
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| CN101245201A (en) * | 2008-03-21 | 2008-08-20 | 杨建平 | Thermoplastic powder electrically-conducting paint/printing ink and manufacture method thereof |
| CN101275052A (en) * | 2008-05-14 | 2008-10-01 | 海洋化工研究院 | Corrosion-resistant electromagnetic screen coating and preparation thereof |
| CN102329560A (en) * | 2010-07-14 | 2012-01-25 | 中化化工科学技术研究总院 | Novel electromagnetic shielding paint for surface of silicone rubber |
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