CN107189445A - One kind is used for highly conductive liquid silicon rubber composition of injection moulding and preparation method thereof - Google Patents
One kind is used for highly conductive liquid silicon rubber composition of injection moulding and preparation method thereof Download PDFInfo
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- CN107189445A CN107189445A CN201710358087.3A CN201710358087A CN107189445A CN 107189445 A CN107189445 A CN 107189445A CN 201710358087 A CN201710358087 A CN 201710358087A CN 107189445 A CN107189445 A CN 107189445A
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- organopolysiloxane
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- 239000000203 mixture Substances 0.000 title claims abstract description 60
- 229920002379 silicone rubber Polymers 0.000 title claims abstract description 39
- 238000001746 injection moulding Methods 0.000 title claims abstract description 31
- 239000007788 liquid Substances 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 17
- 229920001296 polysiloxane Polymers 0.000 claims abstract description 61
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims abstract description 52
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 38
- 229920001971 elastomer Polymers 0.000 claims abstract description 34
- 229910052751 metal Inorganic materials 0.000 claims abstract description 28
- 239000002184 metal Substances 0.000 claims abstract description 28
- 229910052697 platinum Inorganic materials 0.000 claims abstract description 26
- 239000011231 conductive filler Substances 0.000 claims abstract description 22
- 239000003054 catalyst Substances 0.000 claims abstract description 19
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000003112 inhibitor Substances 0.000 claims abstract description 9
- 238000000465 moulding Methods 0.000 claims abstract description 8
- 238000003756 stirring Methods 0.000 claims description 29
- 229910052739 hydrogen Inorganic materials 0.000 claims description 28
- 229920002545 silicone oil Polymers 0.000 claims description 27
- 239000001257 hydrogen Substances 0.000 claims description 25
- 229910052710 silicon Inorganic materials 0.000 claims description 20
- 238000007711 solidification Methods 0.000 claims description 19
- 230000008023 solidification Effects 0.000 claims description 19
- 239000000843 powder Substances 0.000 claims description 16
- 239000012530 fluid Substances 0.000 claims description 15
- 239000011521 glass Substances 0.000 claims description 15
- 239000000377 silicon dioxide Substances 0.000 claims description 14
- 239000002904 solvent Substances 0.000 claims description 13
- 239000010703 silicon Substances 0.000 claims description 12
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 claims description 11
- 125000004435 hydrogen atom Chemical group [H]* 0.000 claims description 11
- 125000003342 alkenyl group Chemical group 0.000 claims description 9
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims description 8
- -1 polysiloxanes Polymers 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 7
- 238000004073 vulcanization Methods 0.000 claims description 7
- 238000010792 warming Methods 0.000 claims description 7
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 claims description 6
- 229920002554 vinyl polymer Polymers 0.000 claims description 6
- 239000003795 chemical substances by application Substances 0.000 claims description 5
- 229910052737 gold Inorganic materials 0.000 claims description 3
- 239000010931 gold Substances 0.000 claims description 3
- 150000001336 alkenes Chemical class 0.000 claims description 2
- 150000001345 alkine derivatives Chemical class 0.000 claims description 2
- 239000006229 carbon black Substances 0.000 claims description 2
- 239000000758 substrate Substances 0.000 claims description 2
- 230000001629 suppression Effects 0.000 claims 1
- 229920000260 silastic Polymers 0.000 abstract description 7
- 238000002347 injection Methods 0.000 abstract description 6
- 239000007924 injection Substances 0.000 abstract description 6
- 238000004519 manufacturing process Methods 0.000 abstract description 6
- 238000007493 shaping process Methods 0.000 abstract description 6
- 150000002431 hydrogen Chemical class 0.000 description 19
- 230000000052 comparative effect Effects 0.000 description 9
- 238000007789 sealing Methods 0.000 description 7
- 239000003085 diluting agent Substances 0.000 description 5
- 239000002245 particle Substances 0.000 description 5
- VGGSQFUCUMXWEO-UHFFFAOYSA-N Ethene Chemical compound C=C VGGSQFUCUMXWEO-UHFFFAOYSA-N 0.000 description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 4
- 239000004945 silicone rubber Substances 0.000 description 4
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 238000006243 chemical reaction Methods 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 239000003595 mist Substances 0.000 description 3
- 238000007747 plating Methods 0.000 description 3
- 229910052709 silver Inorganic materials 0.000 description 3
- 239000004332 silver Substances 0.000 description 3
- KSLSOBUAIFEGLT-UHFFFAOYSA-N 2-phenylbut-3-yn-2-ol Chemical compound C#CC(O)(C)C1=CC=CC=C1 KSLSOBUAIFEGLT-UHFFFAOYSA-N 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 239000002253 acid Substances 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 125000000484 butyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 230000008021 deposition Effects 0.000 description 2
- 229940008099 dimethicone Drugs 0.000 description 2
- 239000004205 dimethyl polysiloxane Substances 0.000 description 2
- 235000013870 dimethyl polysiloxane Nutrition 0.000 description 2
- 239000000428 dust Substances 0.000 description 2
- 125000001495 ethyl group Chemical group [H]C([H])([H])C([H])([H])* 0.000 description 2
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 2
- 230000003694 hair properties Effects 0.000 description 2
- ZSIAUFGUXNUGDI-UHFFFAOYSA-N hexan-1-ol Chemical compound CCCCCCO ZSIAUFGUXNUGDI-UHFFFAOYSA-N 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 2
- 229910052759 nickel Inorganic materials 0.000 description 2
- 125000005375 organosiloxane group Chemical group 0.000 description 2
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 2
- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- 230000001568 sexual effect Effects 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- 0 C*C(C)N[C@]1*=CC1C(C)C Chemical compound C*C(C)N[C@]1*=CC1C(C)C 0.000 description 1
- 230000002159 abnormal effect Effects 0.000 description 1
- 230000001476 alcoholic effect Effects 0.000 description 1
- HSFWRNGVRCDJHI-UHFFFAOYSA-N alpha-acetylene Natural products C#C HSFWRNGVRCDJHI-UHFFFAOYSA-N 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000006835 compression Effects 0.000 description 1
- 238000007906 compression Methods 0.000 description 1
- 238000000748 compression moulding Methods 0.000 description 1
- 230000003750 conditioning effect Effects 0.000 description 1
- 239000003431 cross linking reagent Substances 0.000 description 1
- 125000001047 cyclobutenyl group Chemical group C1(=CCC1)* 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 125000000118 dimethyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 239000000806 elastomer Substances 0.000 description 1
- 238000001125 extrusion Methods 0.000 description 1
- 239000000945 filler Substances 0.000 description 1
- 238000011049 filling Methods 0.000 description 1
- 239000007789 gas Substances 0.000 description 1
- 239000003292 glue Substances 0.000 description 1
- 238000006459 hydrosilylation reaction Methods 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 1
- 239000003921 oil Substances 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 125000002255 pentenyl group Chemical group C(=CCCC)* 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 229910021420 polycrystalline silicon Inorganic materials 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 229920005573 silicon-containing polymer Polymers 0.000 description 1
- 238000005476 soldering Methods 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
- 125000003944 tolyl group Chemical group 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J183/00—Adhesives based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Adhesives based on derivatives of such polymers
- C09J183/04—Polysiloxanes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L83/00—Compositions of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon only; Compositions of derivatives of such polymers
- C08L83/04—Polysiloxanes
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/12—Polysiloxanes containing silicon bound to hydrogen
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G77/00—Macromolecular compounds obtained by reactions forming a linkage containing silicon with or without sulfur, nitrogen, oxygen or carbon in the main chain of the macromolecule
- C08G77/04—Polysiloxanes
- C08G77/20—Polysiloxanes containing silicon bound to unsaturated aliphatic groups
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/001—Conductive additives
-
- 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
-
- 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
Abstract
It is used for the highly conductive liquid silicon rubber composition of injection moulding the present invention relates to one kind, including following components is constituted:The strong volatile thinner of first organopolysiloxane of 100 mass parts, the second organopolysiloxane of 5~25 mass parts, the white carbon of 15~25 mass parts, the platinum based catalyst of 0.05~0.15 mass parts, the inhibitor of 0.005~0.01 mass parts, the metal based electrically conductive filler of 250~500 mass parts, the dissolving power of 5~50 mass parts, the water of 1~2 mass parts；Advantages of the present invention：Mechanical property is improved by adding white carbon, add the strong volatile thinner of dissolving power to reduce viscosity so that the characteristics of liquid silastic being made has good mobility and higher mechanical property concurrently, available for injection rapid shaping, production efficiency is improved, product cost is reduced；In addition, the present invention also provides a kind of preparation method for the highly conductive liquid silicon rubber composition of injection moulding, including prepared by base rubber, prepared by component A, prepared by B component, composition molding.
Description
Technical field
It is used for highly conductive liquid silicon rubber composition of injection moulding and preparation method thereof the present invention relates to one kind.
Background technology
Recently as the high speed development of electronic technology, various wireless communication system and high-frequency electron device quantity swash
Increase, electromagnetic interference (EMI) caused by electromagnetic wave and electromagnetic compatibility (EMC) problem are increasingly serious, and not only electronic equipment is caused to do
Disturb and damage, but also pollute the environment, endanger human health.It is constantly that more powerful function is integrated in the electronic device at present
Into smaller component, traditional soldering is welded can not meet environment sealing and the requirement of electromagnetic sealing function, therefore in order to
The problems such as solving environment sealing and the electromagnetic sealing in integrated circuit, frequently with composition surface in electronic circuit package shell etc.
Load conductive elastomer (such as conductive rubber) to realize electromagnetic sealing and the shielding of shell, and then effectively suppress electronic equipment production
Raw electromagnetic interference.
After the conventional conductive rubber of die forming or extrusion molding, the processed shape and size into design, then by this
Conductive silicon rubber bar passes through screw and positions or slot installed in the position of electromagnetic sealing is needed, and is close to pressure so that between two parts
Sealing is conductive, meets electromagnetic shielding and seal request.Such as patent CN101050307A, CN101260238A, CN103602072A
Deng using elastomeric compound as base rubber, conductive silicon rubber prepared by metal based electrically conductive filler is added.This kind of conductive high-temperature silicon rubber is usually used
In compression molding, but exist and waste raw material flash and the shortcomings of low production efficiency more, injection rapid shaping can overcome the disadvantages that just
The deficiency of conductive high-temperature silicon rubber.
Molded with traditional conductive high-temperature silicon rubber mould, injection rapid shaping conducting liquid silicon rubber has many good qualities：
It can require to add appropriate raw material according to specified size, generation leftover pieces are few, save product cost；Various complexity can be met
Accurate product demand；Computer controls injection volume, and rapid shaping solidification simplifies production technology, greatly improves production efficiency etc..
Patent US7537712 discloses a kind of conductive silicon rubber composition, including each molecule of (A) 100 parts by weight has
The organopolysiloxane of at least two alkenyls, (B) each molecule has organic poly- silicon of the hydrogen atom of at least two silicon bondings
Oxygen alkane, (C) platinum catalyst, (D) 50-500 part by weight of metal base conductive fillers, and (E) 5-500 parts surfactant contents
No more than spherical silicone rubber particles of percentage by weight 0.3%.Due to adding the number of metal based filler and silicone rubber particles very
Many, though the conductive silicon rubber of soft and low permanent compression set can be formed, its poor fluidity is not suitable for liquid
Injection moulding.Patent CN101624471A announces one kind by adding 100-500 in ethenyl blocking dimethyl silicone polymer
Parts by weight particle size is prepared for conductive silicon rubber for the mode of 10-150um conductive particles, but when metal dust is necessarily being weighed
When measuring part (threshold value) below, conductive path cannot be formed, and electric conductivity is very poor；And the metal dust filled it is too many when, excessive fills out
Filling particle can also be remarkably decreased the mobility of glue, and mechanical property can also decline, and can not meet injection moulding.
The content of the invention
The technical problem to be solved in the present invention is just to provide a kind of for the highly conductive liquid silicon rubber composition of injection moulding
And preparation method thereof, the problem of solving existing conductive silicon rubber composition poor fluidity.
In order to solve the above-mentioned technical problem, the present invention is achieved by the following technical solutions：One kind is used for injection moulding
Highly conductive liquid silicon rubber composition, including following components composition:First organopolysiloxane of 100 mass parts, 5~25 mass
Part the second organopolysiloxane, the white carbon of 15~25 mass parts, the platinum based catalyst of 0.05~0.15 mass parts, 0.005
The inhibitor of~0.01 mass parts, the metal based electrically conductive filler of 250~500 mass parts, the dissolving power of 5~50 mass parts waving by force
Hair property diluent, the water of 1~2 mass parts；
Wherein：Each molecule in first organopolysiloxane at least has two alkenyls；In second machine polysiloxanes
Each molecule have at least two silicon bondings hydrogen atom.
It is preferred that, the first organopolysiloxane is included in molecule chain end, and there is per molecule at least two to be bonded to silicon atom
Vinyl and on molecular side chain do not have vinyl vinyl-terminated silicone fluid, the vinyl-terminated silicone fluid at a temperature of 25 DEG C
Viscosity is 1000~200000mPas；The structural formula of vinyl-terminated silicone fluid is：
Wherein：R is CH3Or C2H5, n is integer, n=200~800.
It is preferred that, the second organopolysiloxane includes the first of at least three Si -- Hs of side chain of 5~20 mass parts
Containing hydrogen silicone oil, Si -- H amount is 1.0 × 10-3Mol/g~1.5 × 10-2Mol/g, the structural formula of the first containing hydrogen silicone oil is：
Wherein：R is CH3Or H, m, n are integer, m=10~50, n=3~6；
And 0~5 mass parts two ends the second containing hydrogen silicone oil comprising Si -- H, Si -- H amount is 1.0
×10-4Mol/g~1.5 × 10-3Mol/g, the structural formula of the second containing hydrogen silicone oil is：
Wherein：N is integer, n=18~270；
The viscosity of the second organopolysiloxane is 1~20000mPas at a temperature of 25 DEG C.
It is preferred that, 1~5mol of offer in the second organopolysiloxane is provided in the first organopolysiloxane per 1mol alkenes
The hydrogen atom of silicon bonding.
It is preferred that, white carbon includes gas-phase silica, and the specific surface area of gas-phase silica is not less than 200m2/ g, gas phase is white
The surface of carbon black, which has, includes hexa methyl silazane in the inorganic agent of hexa methyl silazane, the gas-phase silica of 100 mass parts
Addition is 5~15 mass parts.
It is preferred that, platinum based catalyst includes Karst platinum catalyst, and platinum content is 3000ppm.
It is preferred that, inhibitor include 1- acetylene -1- cyclohexanol, 3- methyl isophthalic acids-butine -3- alcohol, 3,5- dimethyl -1- oneself
The composition or two or more compositions of one or both of alkynes -3- alcohol, 3-Phenyl-1-butyn-3-ol.
It is preferred that, metal based electrically conductive filler includes 5~50um silvered glass powder.
It is preferred that, the strong volatile thinner of dissolving power includes D40~D80 solvent naphthas.
A kind of preparation method for the highly conductive liquid silicon rubber composition of injection moulding, comprises the following steps：
Step one：It is prepared by base rubber：Successively respectively by 50 the first organopolysiloxanes of mass parts, white carbon, hexamethyl silicon nitrogen
Alkane and water are added in kneader, are stirred at room temperature after 1h, are warming up to 150 DEG C and are continued to stir 2h, are eventually adding 50 mass parts
The first organopolysiloxane be diluted, base rubber is obtained after cooling；
Step 2：It is prepared by component A：After base rubber prepared by obtaining step one with metal based electrically conductive filler, dissolving power waving by force
Hair property diluent, platinum based catalyst stir to form component A under planetary mixer vacuum；
Step 3：It is prepared by B component：Base rubber prepared by obtaining step one and the volatilization of metal based electrically conductive filler, dissolving power by force
Property diluent, the second organopolysiloxane, inhibitor stir to form B component under planetary mixer vacuum；
Step 4：Composition molding：B component prepared by component A and step 3 prepared by step 2 is by 1:1 mass ratio
Stir, then poured into after vacuumizing and defoaming in mould, by vulcanizing press vulcanizing treatment, the temperature of vulcanization is 150 DEG C,
Then solidify 300 seconds under 10Mpa, finally in the further curing process of convection oven, the temperature of solidification is 120 DEG C, solidification
Time is 4h.
In summary, advantages of the present invention：1. improving mechanical property by adding white carbon, the volatilization of dissolving power by force is added
Property diluent reduces viscosity so that the liquid silastic being made has good mobility concurrently and the spy of higher mechanical property
Point, available for injection rapid shaping, improves production efficiency, reduces product cost；And the product have specific insulation≤
0.01 Ω cm high conductivity, can be widely used in the electronics such as conductive shell, portable computer and sets as electromagnetic shielding material
It is standby；
2. the addition of metal based electrically conductive filler, can be assigned by solidifying the highly conductive of silicon rubber prepared by the present composition
Property, when metal based electrically conductive filler content is less than 250 mass parts, by the conduction for solidifying the silicon rubber that the present composition is obtained
Sexual orientation is not enough；When metal based electrically conductive filler content is more than 500 mass parts, the viscosity of resulting composition becomes very large, plus
Work is deteriorated, and is not suitable for injection moulding；
3. the addition of the strong volatile thinner of dissolving power, reduces the viscosity of the present composition, improve processability, be beneficial to
Injection moulding, when the strong volatile thinner content of dissolving power is less than 5 mass parts, the viscosity of resulting composition becomes very
Greatly, processability is deteriorated, and is not suitable for injection moulding；When the strong volatile thinner content of dissolving power is more than 50 mass parts,
The viscosity of resulting composition diminishes, and processability improves, but metal based electrically conductive filler is tended to separate with resulting composition, after solidification
Silicone Rubber it is bad；
4. the addition of platinum based catalyst, can promote the hydrosilanes of the first organopolysiloxane and the second organopolysiloxane
Change reaction；
5. the addition of inhibitor, can effectively adjust the curing reaction of the present composition.
Embodiment
One kind is used for the highly conductive liquid silicon rubber composition of injection moulding, including following components is constituted:The of 100 mass parts
One organopolysiloxane, the second organopolysiloxane of 5~25 mass parts, the white carbon of 15~25 mass parts, 0.05~0.15
The platinum based catalyst of mass parts, the inhibitor of 0.005~0.01 mass parts, the metal based electrically conductive filler of 250~500 mass parts, 5
The strong volatile thinner of the dissolving powers of~50 mass parts, the water of 1~2 mass parts, wherein：It is every in first organopolysiloxane
One molecule at least has two alkenyls；Each molecule in second machine polysiloxanes has the hydrogen of at least two silicon bondings former
Son.
First organopolysiloxane is the organopolysiloxane that each molecule at least has two alkenyls, and alkenyl can example
Lift vinyl, pi-allyl, cyclobutenyl and pentenyl, the bonding position of alkenyl, can enumerate molecular chain-end, the side chain of strand or
The side chain of molecular chain-end and strand, the group of the silicon bonding in addition to alkenyl can enumerate methyl, ethyl, propyl group, butyl, the
One organopolysiloxane can also be the mixture of the organosiloxane of two or more above-mentioned different molecular structures, excellent
Being selected in molecule chain end, there is per molecule at least two to be bonded to the vinyl of silicon atom and do not have second on molecular side chain
The vinyl-terminated silicone fluid of alkenyl, the vinyl-terminated silicone fluid has 1000~200000mPas viscosity at 25 DEG C, preferably
5000~50000mPas, more preferably 10000~30000mPas, and the structural formula of vinyl-terminated silicone fluid is
Wherein, R is CH3、C2H5, n is integer, n=200~800.
Second organopolysiloxane is the crosslinking agent of the first organopolysiloxane, each molecule tool of the second organopolysiloxane
There is the hydrogen atom of at least two silicon bondings, the bonding position of the hydrogen atom of silicon bonding can enumerate the side chain of molecular chain-end, strand
Or the side chain of molecular chain-end and strand, in addition in the second organopolysiloxane, the group of the silicon bonding in addition to alkenyl
Methyl, ethyl, propyl group, butyl, phenyl, tolyl can be enumerated, the second organopolysiloxane can be carried more than two or more
And different molecular structures organosiloxane mixture, at 25 DEG C have 1-20000mPas viscosity, preferably 5-
1000mPa·s。
In the present invention, by a kind of first Silicon Containing Hydrogen of the second organopolysiloxane preferably at least three Si -- Hs of side chain
Oil, Si -- H amount is 1.0 × 10-3Mol/g~1.5 × 10-2Mol/g, and the mass parts of the first containing hydrogen silicone oil are 5~20, the
The structural formula of one containing hydrogen silicone oil is：
Wherein, R is CH3Or H, m, n are integer, m=10~50, n=3~6；
And a kind of two ends include the second containing hydrogen silicone oil of a Si -- H, Si -- H amount is 1.0 × 10-4mol/
G~1.5 × 10-3Mol/g, and the mass parts of the second containing hydrogen silicone oil are 0~5, the structural formula of the second containing hydrogen silicone oil is：
Wherein：N is integer, n=18~270；
1~5mol of offer silicon bonding in second organopolysiloxane is provided in the first organopolysiloxane per 1mol alkenes
Hydrogen atom, can guarantee that the solidification of conducting liquid rubber composition.
The specific surface area of white carbon is not less than 200m2/ g, preferably gas-phase silica, and gas-phase silica surface conditioning agent is
Silicon nitrogen silane compound, preferably hexa methyl silazane, it is 5~15 matter relative to the addition of 100 mass parts gas-phase silicas
Measure part.
Platinum based catalyst is used for the hydrosilylation reactions for promoting the first organopolysiloxane and the second organopolysiloxane,
Platinum black, chloroplatinic acid, the alcoholic solution of chloroplatinic acid, platinum alkene complex, preferably Karst platinum catalyst can be enumerated, platinum content is
3000ppm。
Inhibitor is to be used to adjust present composition curing reaction, preferably alkynol compound, including 1- acetylene -1- rings
Hexanol, 3- methyl isophthalic acids-butine -3- alcohol, 3,5- dimethyl -1- hexin -3- alcohol, the one or two of 3-Phenyl-1-butyn-3-ol
Composition or two or more compositions.
Metal based electrically conductive filler is assigned by solidifying silicon rubber high conductivity prepared by the present composition, and Metal Substrate is conductive
Filler includes conductive metal powder or by vapour deposition metal plating or coating micro mist, and metal based electrically conductive filler can be enumerated
Gold, silver, nickel, the metal fine powder of copper；By by vapour deposition, with gold, silver, nickel, the metal plating of copper or it is coated with by glass, has
The micro mist surface of machine resin and analog composition and the micro mist that obtains, the present invention is preferably 5~50um silvered glass powder, because plating
Silver glass powder has relatively low cost and higher electric conductivity, and its relative to 100 part first organopolysiloxane addition 200~
1000 parts, preferably 250~500 parts.When metal based electrically conductive filler is less than above range lower limit, by solidifying the present composition
The conductive sexual orientation of the silicon rubber of acquisition is not enough；When metal based electrically conductive filler content exceedes the above range upper limit, gained combination
The viscosity of thing becomes very large, and processability is deteriorated, and is not suitable for injection moulding.
The strong volatile thinner of dissolving power, the viscosity for reducing the present composition improves processability, beneficial to injection
Shaping, can enumerate normal octane, toluene, solvent naphtha, more preferably D40~D80 solvent naphthas, small toxicity, not interfere with by of the present invention group
The mechanical property and electric conductivity of the silicon rubber of compound solidification, when the strong volatile thinner content of dissolving power is less than 5 mass parts
When, the viscosity of resulting composition becomes very large, and processability is deteriorated, and is not suitable for injection moulding；When the volatilization of dissolving power by force
When property amount of diluent is more than 50 mass parts, the viscosity of resulting composition diminishes, and processability improves, but metal based electrically conductive filler is inclined
Separated in resulting composition, the Silicone Rubber after solidification is bad.
Embodiment one：
A kind of preparation method for the highly conductive liquid silastic of injection moulding, comprises the following steps：
Step one：It is prepared by base rubber：Successively respectively by 50 mass parts 10000mPas vinyl-terminated silicone fluid, 20 mass parts
Specific surface area is 300m2The water of/g gas-phase silica, the hexa methyl silazane of 5 mass parts and 1 mass parts is added to kneader
In, it is stirred at room temperature after 1h, is warming up to 150 DEG C and continues to stir 2h, be eventually adding 50 mass parts 10000mPas end ethene
Base silicone oil is diluted, and base rubber is obtained after cooling；
Step 2：It is prepared by component A：Obtain base rubber and 279.4g silvered glasses powder, 12.27g prepared by 100g steps one
D40 solvent naphthas, 0.27g Karst platinum catalyst stir to form component A under planetary mixer vacuum；
Step 3：It is prepared by B component：Obtain base rubber and 279.4g silvered glasses powder, 12.27g prepared by 100g steps one
D40 solvent naphthas, 3.14g only side chain hydrogeneous containing hydrogen silicone oil (Si -- H amount 8.0 × 10-3Mol/g), 3.59g only two ends are hydrogeneous
Containing hydrogen silicone oil (Si -- H amount 5.0 × 10-4Mol/g), 10 microlitres of 2- methyl -3- butyne-2-alcohols (density 0.86g/cm3),
Stir to form B component under planetary mixer vacuum；
Step 4：Composition molding：B component prepared by component A and step 3 prepared by step 2 is by 1:1 mass ratio
Stir, then poured into after vacuumizing and defoaming in mould, by vulcanizing press vulcanizing treatment, the temperature of vulcanization is 150 DEG C,
Then solidify 300 seconds under 10Mpa, finally in the further curing process of convection oven, the temperature of solidification is 120 DEG C, solidification
Time is 4h.
Embodiment two：
A kind of preparation method for the highly conductive liquid silastic of injection moulding, comprises the following steps：
Step one：It is prepared by base rubber：Successively respectively by 50 mass parts 10000mPas vinyl-terminated silicone fluid, 25 mass parts
Specific surface area is 300m2The water of/g gas-phase silica, the hexa methyl silazane of 6.25 mass parts and 1.25 mass parts is added to
In kneader, it is stirred at room temperature after 1h, is warming up to 150 DEG C and continues to stir 2h, be eventually adding 50 mass parts 10000mPas'
Vinyl-terminated silicone fluid is diluted, and base rubber is obtained after cooling；
Step 2：It is prepared by component A：Obtain base rubber and 279.4g silvered glasses powder, 18.65g prepared by 100g steps one
D40 solvent naphthas, 0.27g Karst platinum catalyst (platinum content is 3000ppm) stir under planetary mixer vacuum
Form component A；
Step 3：It is prepared by B component：Obtain base rubber and 279.4g silvered glasses powder, 12.35g prepared by 100g steps one
D40 solvent naphthas, 2.94g only side chain hydrogeneous containing hydrogen silicone oil (Si -- H amount 8.0 × 10-3Mol/g), 3.36g only two ends are hydrogeneous
Containing hydrogen silicone oil (Si -- H amount 5.0 × 10-4Mol/g), 10 microlitres of 2- methyl -3- butyne-2-alcohols (density 0.86g/cm3),
Stir to form B component under planetary mixer vacuum；
Step 4：Composition molding：B component prepared by component A and step 3 prepared by step 2 is by 1:1 mass ratio
Stir, then poured into after vacuumizing and defoaming in mould, by vulcanizing press vulcanizing treatment, the temperature of vulcanization is 150 DEG C,
Then solidify 300 seconds under 10Mpa, finally in the further curing process of convection oven, the temperature of solidification is 120 DEG C, solidification
Time is 4h.
Comparative example one：
A kind of preparation method for the highly conductive liquid silastic of injection moulding, comprises the following steps：
Step one：It is prepared by base rubber：Successively respectively by 50 mass parts 10000mPas vinyl-terminated silicone fluid, 20 mass parts
Specific surface area is 300m2The water of/g gas-phase silica, the hexa methyl silazane of 5 mass parts and 1 mass parts is added to kneader
In, it is stirred at room temperature after 1h, is warming up to 150 DEG C and continues to stir 2h, be eventually adding 50 mass parts 10000mPas end ethene
Base silicone oil is diluted, and base rubber is obtained after cooling；
Step 2：It is prepared by component A：Obtain base rubber and 191.9g silvered glasses powder, 9.73g D40 prepared by 100g steps one
Solvent naphtha, 0.27g Karst platinum catalyst (platinum content is 3000ppm) stir to be formed under planetary mixer vacuum
Component A；
Step 3：It is prepared by B component：Obtain base rubber and 191.9g silvered glasses powder, 3.27g D40 prepared by 100g steps one
Solvent naphtha, 3.14g only side chain hydrogeneous containing hydrogen silicone oil (Si -- H amount 8.0 × 10-3Mol/g), 3.59g only two ends are hydrogeneous contains
Hydrogen silicone oil (Si -- H amount 5.0 × 10-4Mol/g), 10 microlitres of 2- methyl -3- butyne-2-alcohols (density 0.86g/cm3), it is expert at
Stir to form B component under star mixer vacuum；
Step 4：Composition molding：B component prepared by component A and step 3 prepared by step 2 is by 1:1 mass ratio
Stir, then poured into after vacuumizing and defoaming in mould, by vulcanizing press vulcanizing treatment, the temperature of vulcanization is 150 DEG C,
Then solidify 300 seconds under 10Mpa, finally in the further curing process of convection oven, the temperature of solidification is 120 DEG C, solidification
Time is 4h.
Comparative example two：
A kind of preparation method for the highly conductive liquid silastic of injection moulding, comprises the following steps：
Step one：It is prepared by base rubber：Successively respectively by 50 mass parts 10000mPas vinyl-terminated silicone fluid, 20 mass parts
Specific surface area is 300m2The water of/g gas-phase silica, the hexa methyl silazane of 5 mass parts and 1 mass parts is added to kneader
In, it is stirred at room temperature after 1h, is warming up to 150 DEG C and continues to stir 2h, be eventually adding 50 mass parts 10000mPas end ethene
Base silicone oil is diluted, and base rubber is obtained after cooling；
Step 2：It is prepared by component A：Obtain base rubber and 279.4g silvered glasses powder, 9.73g D40 prepared by 100g steps one
Solvent naphtha, 0.27g Karst platinum catalyst (platinum content is 3000ppm) stir to be formed under planetary mixer vacuum
Component A；
Step 3：It is prepared by B component：Obtain base rubber and 279.4g silvered glasses powder, 3.27g D40 prepared by 100g steps one
Solvent naphtha, 3.14g only side chain hydrogeneous containing hydrogen silicone oil (Si -- H amount 8.0 × 10-3Mol/g), 3.59g only two ends are hydrogeneous contains
Hydrogen silicone oil (Si -- H amount 5.0 × 10-4Mol/g), 10 microlitres of 2- methyl -3- butyne-2-alcohols (density 0.86g/cm3), it is expert at
Stir to form B component under star mixer vacuum；
Step 4：Composition molding：B component prepared by component A and step 3 prepared by step 2 is by 1:1 mass ratio
Stir, then poured into after vacuumizing and defoaming in mould, by vulcanizing press vulcanizing treatment, the temperature of vulcanization is 150 DEG C,
Then solidify 300 seconds under 10Mpa, finally in the further curing process of convection oven, the temperature of solidification is 120 DEG C, solidification
Time is 4h.
Comparative example three：
A kind of preparation method for the highly conductive liquid silastic of injection moulding, comprises the following steps：
Step one：It is prepared by base rubber：Successively respectively by 50 mass parts 10000mPas vinyl-terminated silicone fluid, 20 mass parts
Specific surface area is 300m2The water of/g gas-phase silica, the hexa methyl silazane of 5 mass parts and 1 mass parts is added to kneader
In, it is stirred at room temperature after 1h, is warming up to 150 DEG C and continues to stir 2h, be eventually adding 50 mass parts 10000mPas end ethene
Base silicone oil is diluted, and base rubber is obtained after cooling；
Step 2：It is prepared by component A：The base rubber and 279.4g silvered glasses powder, 12.27g for obtaining the preparation of 100g steps one are glued
Degree 20cP dimethicone, 0.27g Karst platinum catalyst stirs to form component A under planetary mixer vacuum；
Step 3：It is prepared by B component：The base rubber and 279.4g silvered glasses powder, 12.27g for obtaining the preparation of 100g steps one are glued
Spend hydrogeneous containing hydrogen silicone oil (the Si -- H amount 8.0 × 10 of 20cP dimethicone, 3.14g only side chains-3Mol/g), 3.59g is only
Two ends hydrogeneous containing hydrogen silicone oil (Si -- H amount 5.0 × 10-4Mol/g), 10 microlitres of 2- methyl -3- butyne-2-alcohol (density
0.86g/cm3), stir to form B component under planetary mixer vacuum；
Step 4：Composition molding：B component prepared by component A and step 3 prepared by step 2 is by 1:1 mass ratio
Stir, then poured into after vacuumizing and defoaming in mould, by vulcanizing press vulcanizing treatment, the temperature of vulcanization is 150 DEG C,
Then solidify 300 seconds under 10Mpa, finally in the further curing process of convection oven, the temperature of solidification is 120 DEG C, solidification
Time is 4h.
Comparative example four：
Conductive silicon rubber composition is prepared in the same manner as example 1, except that dissolving power in embodiment 1
Strong volatile thinner selects D40 solvent naphthas, and the strong volatile thinner of dissolving power is not added with comparative example 4, can be with
Substantially find in the case of the volatile thinner strong without dissolving power, because viscosity is increased very big, stirring is abnormal tired
Difficulty, therefore uniform composition can not be prepared.
Respectively to embodiment one, embodiment two, comparative example one, comparative example two, comparative example three, the forming composition of comparative example four
Tested, testing standard is that viscosity refers to obtain data at 25 DEG C, is tested using Brookfield rotation viscometers；It is based on
GB 2411 is tested tensile strength, elongation at break, is based on to tearing strength, GB/T 528 to hardness, GB/T 529
MIL-DTL-83528C is tested specific insulation, and test result is as shown in Table 1：
Table one
In addition to above preferred embodiment, the present invention also has other embodiments, and those skilled in the art can be according to this
Invention is variously modified and deformed, and without departing from the spirit of the present invention, all should belong to appended claims of the present invention and determine
The scope of justice.
Claims (10)
1. one kind is used for the highly conductive liquid silicon rubber composition of injection moulding, it is characterised in that：Including following components composition:100
First organopolysiloxane of mass parts, the second organopolysiloxane of 5~25 mass parts, the white carbon of 15~25 mass parts,
The platinum based catalyst of 0.05~0.15 mass parts, the inhibitor of 0.005~0.01 mass parts, the Metal Substrate of 250~500 mass parts
The strong volatile thinner of dissolving power, the water of 1~2 mass parts of conductive filler, 5~50 mass parts；
Wherein：Each molecule in first organopolysiloxane at least has two alkenyls；It is every in second machine polysiloxanes
One molecule has the hydrogen atom of at least two silicon bondings.
2. it is according to claim 1 a kind of for the highly conductive liquid silicon rubber composition of injection moulding, it is characterised in that：The
One organopolysiloxane is included in molecule chain end, and there is per molecule at least two to be bonded to the vinyl of silicon atom and divide
On sub- side chain do not have vinyl vinyl-terminated silicone fluid, at a temperature of 25 DEG C the viscosity of vinyl-terminated silicone fluid be 1000~
200000mPa·s；The structural formula of vinyl-terminated silicone fluid is：
Wherein：R is CH3Or C2H5, n is integer, n=200~800.
3. it is according to claim 1 a kind of for the highly conductive liquid silicon rubber composition of injection moulding, it is characterised in that：The
Diorganopolysiloxanecompositions include first containing hydrogen silicone oil of at least three Si -- Hs of side chain of 5~20 mass parts, Si -- H
Measure as 1.0 × 10-3Mol/g~1.5 × 10-2Mol/g, the structural formula of the first containing hydrogen silicone oil is：
Wherein：R is CH3Or H, m, n are integer, m=10~50, n=3~6；
And 0~5 mass parts two ends the second containing hydrogen silicone oil comprising Si -- H, Si -- H amount is 1.0 × 10- 4Mol/g~1.5 × 10-3Mol/g, the structural formula of the second containing hydrogen silicone oil is：
Wherein：N is integer, n=18~270；
The viscosity of the second organopolysiloxane is 1~20000mPas at a temperature of 25 DEG C.
4. it is according to claim 1 a kind of for the highly conductive liquid silicon rubber composition of injection moulding, it is characterised in that：The
The hydrogen atom of 1~5mol of offer silicon bonding in second organopolysiloxane is provided in one organopolysiloxane per 1mol alkenes.
5. it is according to claim 1 a kind of for the highly conductive liquid silicon rubber composition of injection moulding, it is characterised in that：In vain
Carbon black includes gas-phase silica, and the specific surface area of gas-phase silica is not less than 200m2/ g, the surface of gas-phase silica, which has, to be included
The addition of hexa methyl silazane is 5~15 mass in the inorganic agent of hexa methyl silazane, the gas-phase silica of 100 mass parts
Part.
6. it is according to claim 1 a kind of for the highly conductive liquid silicon rubber composition of injection moulding, it is characterised in that：Platinum
Base catalyst includes Karst platinum catalyst, and platinum content is 3000ppm.
7. it is according to claim 1 a kind of for the highly conductive liquid silicon rubber composition of injection moulding, it is characterised in that：Suppression
Preparation includes 1- acetylene -1- cyclohexanol, 3- methyl isophthalic acids-butine -3- alcohol, 3,5- dimethyl -1- hexin -3- alcohol, 3- phenyl -1- fourths
The composition or two or more compositions of one or both of alkynes -3- alcohol.
8. it is according to claim 1 a kind of for the highly conductive liquid silicon rubber composition of injection moulding, it is characterised in that：Gold
Belonging to base conductive filler includes 5~50um silvered glass powder.
9. it is according to claim 1 a kind of for the highly conductive liquid silicon rubber composition of injection moulding, it is characterised in that：It is molten
Solving the strong volatile thinner of power includes D40~D80 solvent naphthas.
10. a kind of preparation method for the highly conductive liquid silicon rubber composition of injection moulding, it is characterised in that：
Comprise the following steps：
Step one：It is prepared by base rubber：Successively respectively by 50 the first organopolysiloxanes of mass parts, white carbon, hexa methyl silazane and
Water is added in kneader, is stirred at room temperature after 1h, is warming up to 150 DEG C and is continued to stir 2h, is eventually adding the of 50 mass parts
One organopolysiloxane is diluted, and base rubber is obtained after cooling；
Step 2：It is prepared by component A：The volatility that the base rubber of the preparation of obtaining step one is strong with metal based electrically conductive filler, dissolving power is dilute
Agent, platinum based catalyst is released to stir to form component A under planetary mixer vacuum；
Step 3：It is prepared by B component：The volatility that the base rubber of the preparation of obtaining step one is strong with metal based electrically conductive filler, dissolving power is dilute
Agent, the second organopolysiloxane, inhibitor is released to stir to form B component under planetary mixer vacuum；
Step 4：Composition molding：B component prepared by component A and step 3 prepared by step 2 is by 1:1 mass ratio stirring
Uniformly, then poured into after vacuumizing and defoaming in mould, by vulcanizing press vulcanizing treatment, the temperature of vulcanization is 150 DEG C, then
Solidify 300 seconds under 10Mpa, finally in the further curing process of convection oven, the temperature of solidification is 120 DEG C, the time of solidification
For 4h.
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Application publication date: 20170922 |