CN107043540A - A kind of sizing of transparent silica gel terminal sleeve and preparation method thereof - Google Patents

A kind of sizing of transparent silica gel terminal sleeve and preparation method thereof Download PDF

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Publication number
CN107043540A
CN107043540A CN201710038222.6A CN201710038222A CN107043540A CN 107043540 A CN107043540 A CN 107043540A CN 201710038222 A CN201710038222 A CN 201710038222A CN 107043540 A CN107043540 A CN 107043540A
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Prior art keywords
sizing
silica gel
terminal sleeve
parts
transparent silica
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CN201710038222.6A
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王中立
王西弱
谢金刚
王文本
王西宇
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Anhui Xingxin Chemical Science & Technology Co Ltd
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Anhui Xingxin Chemical Science & Technology Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L83/00Compositions 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
    • C08L83/04Polysiloxanes
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/002Physical properties
    • C08K2201/006Additives being defined by their surface area
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/014Additives containing two or more different additives of the same subgroup in C08K
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/10Transparent films; Clear coatings; Transparent materials
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2203/00Applications
    • C08L2203/20Applications use in electrical or conductive gadgets
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/02Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/02Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
    • C08L2205/025Polymer 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
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/03Polymer mixtures characterised by other features containing three or more polymers in a blend

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  • Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Processing And Handling Of Plastics And Other Materials For Molding In General (AREA)

Abstract

The invention discloses a kind of sizing of transparent silica gel terminal sleeve, it is characterised in that:It is by 98 100 parts of Polymethyl methacrylates, 10 60 parts of reinforced fillings, 1 60 parts of polymethyl hydrogen siloxanes, 0.1 1 parts of defoamers, 0.001 0.1 parts of platinum catalysts, 0.001 1 parts of inhibitor, 1 10 parts of antistructurizing agents be well mixed by weight after be made using dip forming technology, the silica gel terminal sleeve prepared by transparent silica gel terminal sleeve sizing for providing of the present invention and preparation method thereof has the advantages that mechanical strength is good, weatherability is excellent, insulation, transparent.

Description

A kind of sizing of transparent silica gel terminal sleeve and preparation method thereof
Technical field
The invention belongs to polymeric material field, and in particular to the formula and moulding process of a kind of gel protective sleeve, especially It is a kind of impregnation forming method of silica gel terminal sleeve.
Background technology
Terminal sleeve is to apply the electrical equipment for being connected protection with connector in electrical equipment, automobile, communication device wirning harness, electric wire Beam is held and positioned by terminal sleeve, it is to avoid wirning harness, which contacts with each other, causes short circuit, improves the security of electrical equipment. Terminal sleeve as wire harness and connector connecting element, in addition to insulating properties, will also have good mechanical performance, Heat resistance and weather resistance.Terminal sleeve material general at present is mainly PVC and silicon rubber, with the resistance to height to terminal sleeve The requirement of each side such as warm nature energy, insulating properties, solvent resistance is more and more stricter, and PVC terminal sleeves will be gradually by silica gel terminal Set substitution.Silica gel terminal sleeve species is various, and size heterogeneity is larger, and using molding or injection molding technique, not only the production cycle is long, Die cost is high, and the terminal sleeve prepared is opaque, is unfavorable for being reliably connected for wire harness and connector, reduces electronic equipment Security.Therefore, using short molding cycle, mold design exploitation is flexible, with low cost, it is adaptable to serialization, scale metaplasia The dip forming technology of production simultaneously has importance for preparing transparent silica gel terminal sleeve.
Chinese patent(Application number 201010184005.6)A kind of anti-static silicon rubber sleeve and preparation method thereof is disclosed, with Silicon rubber, white carbon, conductive filler, hydroxy silicon oil, containing hydrogen silicone oil, vulcanizing agent are raw material, pass through mixing silicon rubber, conducting resinl system Antistatic silicone rubber sleeve pipe is made in compression molding after the mixing of standby plus sulphur, extrusion vulcanization.The invention is provided suitable for daily The antistatic sleeve pipe of life, is not suitable for electrical equipment protection.
United States Patent (USP) US3872515A discloses a kind of dip forming technology of medical rubber glove, will scribble polytetrafluoroethyl-ne The ceramic glove mould immersion sizing content of alkene is moulded in liquid for the leaching of 12 ~ 14% trichloroethanes, adds catalyst, filler Deng raw material, die lifting speed and dip time, the length of dip time and the number of times control of dipping are controlled by automatic hydraulic The thickness of gloves.Drying makes trichloroethanes volatilize in atmosphere after dipping, then sticks trade mark, mould is immersed into Dry-powder Lubricant The middle outer surface for forming gloves, rubber gloves is made after vulcanizing about one hour in 270 ℉ curing cage.The leaching that the invention is provided Stain technique cure time is long, needs solvent volatilization to be molded after dipping, complex technical process, and trichloroethanes is poisonous, easily Cause environmental pollution.
The content of the invention
It is an object of the invention to provide a kind of formula of transparent silica gel terminal sleeve and preparation method thereof, to overcome existing product Technological deficiency;
A kind of sizing of transparent silica gel terminal sleeve, it is by 98-100 parts of Polymethyl methacrylates, 10-60 parts of reinforcement Filler, 1-60 part polymethyl hydrogen siloxane, 0.1-1 parts of defoamers, 0.001-0.1 parts of platinum catalysts, 0.001-1 parts of suppression Agent, 1-10 parts of antistructurizing agents are made after being well mixed by weight using dip forming technology.
A kind of preparation method of the sizing of transparent silica gel terminal sleeve, comprises the following steps:
(1)The Polymethyl methacrylate, reinforced filling, defoamer of above-mentioned parts by weight are added in vacuum kneader, heating Mixed 2-4 hours to 150-180 DEG C, be cooled to room temperature;
(2)Material after cooling is added in planetary mixer, add the polymethyl hydrogen siloxanes of above-mentioned parts by weight, inhibitor, Antistructurizing agent, is stirred 1-2 hours, and the platinum catalyst for adding above-mentioned parts by weight is stirred 27-30 minutes, is well mixed;
(3)After well mixed, de-bubbled is vacuumized, material is extruded with swager, filtered, dipping sizing material is made.
A kind of sizing of transparent silica gel terminal sleeve, described Polymethyl methacrylate machine can be average molecular On the relatively low alkene based polysiloxane of amount or chain or the end of the chain at least has the height of two bonded vinyl of silicon The dimethyl silicone polymer of polymerization or the alkene based polysiloxane of low polymerization degree with chain or the end of the chain at least has two The mixture of the dimethyl silicone polymer of the high polymeric of the individual bonded vinyl of silicon;Oligomeric or high polymeric siloxanes structure Can be linear, ring-type or the structure or similar branch of collateralization or netted structure;Preferred viscosities are in 5000- 50000mPa.s linear Polymethyl methacrylate.
A kind of sizing of transparent silica gel terminal sleeve, described polymethyl hydrogen siloxane is to contain two or two in molecule Bonded hydrogen atom on the silicon atoms more than individual, polymethyl hydrogen siloxane of the preferred viscosity ranges in 1-500mPa.s
A kind of sizing of transparent silica gel terminal sleeve, described platinum catalyst is the aqueous isopropanol of chloroplatinic acid, adjacent benzene two Formic acid diethylester co-ordination complex, platinum tetrahydrofuran complex one of which or several mixtures, wherein platinum content exist 1000-5000ppm。
A kind of sizing of transparent silica gel terminal sleeve, described reinforced filling is specific surface area in 100-300m2/ g's Fume colloidal silica, precipitated silica, surface treatment hydrophobic gas-phase silica, surface treatment hydrophobic precipitated silica or MQ silicones one of which or several mixtures;
A kind of sizing of transparent silica gel terminal sleeve, described antistructurizing agent is hydroxy silicon oil, polyether modified silicon oil, gathered One or more of mixtures in ester modified silicone oil or HMDS;
A kind of sizing of transparent silica gel terminal sleeve, described inhibitor is alkynol compound, many vinyl polysiloxanes, acyl Amines or maleic acid ester type compound one of which or several mixtures.
A kind of sizing of transparent silica gel terminal sleeve, the preparation of the transparent silica gel terminal sleeve is prepared with the sizing Method, comprises the following steps:
(1)Mould is put into heating furnace and is preheating to 70-300 DEG C, above-mentioned sizing is immersed, makes sizing in mould table Face is adhered to, and mould decrease speed is 100-200mm/min, soaks material time 10-50s;
(2)The mould for being attached with sizing is taken out from leaching material pond, the rate of climb is 100-300 mm/min, in 200- After being toasted 20-90 seconds at 400 DEG C, make sizing complete cure;
(3)It will be cooled down 5-20 seconds in the terminal sleeve insertion cooling water of mould and complete cure, with air gun by terminal sleeve stripping, i.e., It can obtain transparent silica gel terminal sleeve.
Invention advantage:
Silica gel terminal sleeve prepared by transparent silica gel terminal sleeve sizing that the present invention is provided and preparation method thereof has mechanics Intensity is good, weatherability is excellent, insulation, it is transparent the advantages of, baroque terminal sleeve device is especially suitable for using dip forming technology Part, with short molding cycle, mold design exploitation is flexible, the low advantage of die cost, it is adaptable to serialization, large-scale production.
Embodiment
Embodiment 1:
100 parts of Polymethyl methacrylates are added in vacuum kneader(Viscosity is 30000mPa.s at 25 DEG C), 20 parts are dredged Water fume colloidal silica(Specific surface area 200m2/g), 1 part of fluorine silicon defoaming agent, 180 DEG C mix 2 hours when vacuumizing, cooling To room temperature.Material after cooling is added in planetary mixer, 30 parts of polymethyl hydrogen siloxanes are added(Viscosity is at 25 DEG C 200mPa.s), 0.01 part of inhibitor, 10 parts of HMDSs stir 1 hour, add the stirring of 10ppm platinum catalysts 30 minutes, after being well mixed, de-bubbled is vacuumized with planet machine, material is extruded with swager, filtered, dipping sizing material is made.
Mould is put into heating furnace and is preheating to 150 DEG C, immersion dipping sizing material, mould decrease speed is 100mm/min, leaching Material time 20s;The mould for being attached with silica gel is taken out from leaching material pond, the rate of climb is 160 mm/min, is toasted at 350 DEG C 45 seconds, make silica gel complete cure;It will be cooled down 10 seconds in the terminal sleeve insertion cooling water of mould and complete cure, with air gun by terminal Stripping is covered, transparent silica gel terminal sleeve is made.
Embodiment 2:
100 parts of Polymethyl methacrylates are added in vacuum kneader(Viscosity is 20000mPa.s at 25 DEG C), 45 parts are not The fume colloidal silica of processing(Specific surface area 180m2/g), 0.5 part of fluorine silicon defoaming agent, 150 DEG C when vacuumizing to mix 4 small When, it is cooled to room temperature.Material after cooling is added in planetary mixer, 45 parts of polymethyl hydrogen siloxanes are added(Glued at 25 DEG C Spend for 100mPa.s), 0.02 part of inhibitor, 2 parts of polyether modified silicon oils stir 1 hour, add the stirring of 8ppm platinum catalysts 30 minutes, after being well mixed, de-bubbled is vacuumized with planet machine, material is extruded with swager, filtered, dipping sizing material is made.
Mould is put into heating furnace and is preheating to 200 DEG C, immersion dipping sizing material, mould decrease speed is 120mm/min, leaching Material time 25s;The mould for being attached with silica gel is taken out from leaching material pond, the rate of climb is 200 mm/min, is toasted at 300 DEG C 40 seconds, make silica gel complete cure;It will be cooled down 15 seconds in the terminal sleeve insertion cooling water of mould and complete cure, with air gun by terminal Stripping is covered, transparent silica gel terminal sleeve is made.
Embodiment 3:
100 parts of Polymethyl methacrylates are added in vacuum kneader(Viscosity is 5000mPa.s at 25 DEG C), 60 parts hydrophobic Precipitated silica(Specific surface area 300m2/g), 0.1 part of fluorine silicon defoaming agent, 170 DEG C mix 2 hours when vacuumizing, cooling To room temperature.Material after cooling is added in planetary mixer, 60 parts of polymethyl hydrogen siloxanes are added(Viscosity is at 25 DEG C 50mPa.s), 0.05 part of inhibitor, 1 part of hydroxy silicon oil stir 1 hour, add 8ppm platinum catalysts and stir 30 minutes, mix After closing uniformly, de-bubbled is vacuumized with planet machine, material is extruded with swager, filtered, dipping sizing material is made.
Mould is put into heating furnace and is preheating to 300 DEG C, immersion dipping sizing material, mould decrease speed is 200mm/min, leaching Material time 50s;The mould for being attached with silica gel is taken out from leaching material pond, the rate of climb is 300 mm/min, is toasted at 400 DEG C 20 seconds, make silica gel complete cure;It will be cooled down 12 seconds in the terminal sleeve insertion cooling water of mould and complete cure, with air gun by terminal Stripping is covered, transparent silica gel terminal sleeve is made.
Embodiment 4:
100 parts of Polymethyl methacrylates are added in vacuum kneader(Viscosity is 50000mPa.s at 25 DEG C), 20 parts are dredged Water sedimentation method white carbon(Specific surface area 200m2/g), 25 parts of MQ silicones, 0.6 part of fluorine silicon defoaming agent, 150 DEG C when vacuumizing Mixing 4 hours, is cooled to room temperature.Material after cooling is added in planetary mixer, 10 parts of polymethyl hydrogen siloxanes are added(25 Viscosity is 50mPa.s at DEG C), 0.02 part of inhibitor, 1 part of HMDS, stir 1 hour, add 10ppm platinums and urge Agent is stirred 30 minutes, after being well mixed, is vacuumized de-bubbled with planet machine, is extruded material with swager, is filtered, and leaching is made Stain sizing material.
Mould is put into heating furnace and is preheating to 70 DEG C, immersion dipping sizing material, mould decrease speed is 100mm/min, leaching Material time 90s;The mould for being attached with silica gel is taken out from leaching material pond, the rate of climb is 100 mm/min, is toasted at 200 DEG C 90 seconds, make silica gel complete cure;It will be cooled down 20 seconds in the terminal sleeve insertion cooling water of mould and complete cure, with air gun by terminal Stripping is covered, transparent silica gel terminal sleeve is made.
Embodiment 5:
100 parts of Polymethyl methacrylates are added in vacuum kneader(Viscosity is 10000mPa.s at 25 DEG C), 40 parts are not Precipitated silica through processing(Specific surface area 180m2/g), 1 part of fluorine silicon defoaming agent, 180 DEG C when vacuumizing to mix 2 small When, it is cooled to room temperature.Material after cooling is added in planetary mixer, 10 parts of polymethyl hydrogen siloxanes are added(Glued at 25 DEG C Spend for 50mPa.s), 0.02 part of inhibitor, 1 part of HMDS, stir 1 hour, add 10ppm platinum catalysts and stir Mix 30 minutes, after being well mixed, vacuumize de-bubbled with planet machine, extruded material with swager, filter, dipping glue is made Material.
Mould is put into heating furnace and is preheating to 240 DEG C, immersion dipping sizing material, mould decrease speed is 150mm/min, leaching Material time 90s;The mould for being attached with silica gel is taken out from leaching material pond, the rate of climb is 250 mm/min, is toasted at 350 DEG C 25 seconds, make silica gel complete cure;It will be cooled down 20 seconds in the terminal sleeve insertion cooling water of mould and complete cure, with air gun by terminal Stripping is covered, transparent silica gel terminal sleeve is made.

Claims (9)

1. a kind of sizing of transparent silica gel terminal sleeve, it is characterised in that:It is by 98-100 parts of poly- methyl ethylene silica Alkane, 10-60 part reinforced filling, 1-60 parts of polymethyl hydrogen siloxanes, 0.1-1 parts of defoamers, 0.001-0.1 parts of platinum catalysts, 0.001-1 parts of inhibitor, 1-10 parts of antistructurizing agents are made after being well mixed by weight using dip forming technology.
2. a kind of preparation method of the sizing of transparent silica gel terminal sleeve as claimed in claim 1, comprises the following steps:
(1)The Polymethyl methacrylate, reinforced filling, defoamer of above-mentioned parts by weight are added in vacuum kneader, heating Mixed 2-4 hours to 150-180 DEG C, be cooled to room temperature;
(2)Material after cooling is added in planetary mixer, add the polymethyl hydrogen siloxanes of above-mentioned parts by weight, inhibitor, Antistructurizing agent, is stirred 1-2 hours, and the platinum catalyst for adding above-mentioned parts by weight is stirred 27-30 minutes, is well mixed;
(3)After well mixed, de-bubbled is vacuumized, material is extruded with swager, filtered, dipping sizing material is made.
3. a kind of sizing of transparent silica gel terminal sleeve according to claim 1, it is characterised in that described poly- methyl Vinylsiloxane machine can be on the relatively low alkene based polysiloxane of relative molecular weight or chain or the end of the chain extremely There is the poly- silicon of the alkylene of dimethyl silicone polymer or low polymerization degree of the high polymeric of two bonded vinyl of silicon less On oxygen alkane and chain or the end of the chain at least has the mixture of the dimethyl silicone polymer of the high polymeric of two bonded vinyl of silicon; Oligomeric or high polymeric siloxanes structure can be linear, ring-type or collateralization structure or similar branch or Netted structure;Linear Polymethyl methacrylate of the preferred viscosities in 5000-50000mPa.s.
4. a kind of sizing of transparent silica gel terminal sleeve according to claim 1, it is characterised in that described poly- methyl Hydrogen siloxane is that preferred viscosity ranges are in 1- containing two or more bonded hydrogen atoms on the silicon atoms in molecule 500mPa.s polymethyl hydrogen siloxane.
5. the sizing of a kind of transparent silica gel terminal sleeve according to claim 1, it is characterised in that described platinum is urged Agent is the aqueous isopropanol of chloroplatinic acid, diethyl phthalate co-ordination complex, platinum tetrahydrofuran complex one of which Or several mixtures, wherein platinum content is in 1000-5000ppm.
6. the sizing of a kind of transparent silica gel terminal sleeve according to claim 1, it is characterised in that described reinforcement is filled out Material is specific surface area in 100-300m2/ g fume colloidal silica, precipitated silica, the hydrophobic gas phase hard charcoal of surface treatment Black, surface treatment hydrophobic precipitated silica or MQ silicones one of which or several mixtures.
7. a kind of sizing of transparent silica gel terminal sleeve according to claim 1, it is characterised in that described structuring Controlling agent is one or more of mixed in hydroxy silicon oil, polyether modified silicon oil, polyester modification silicone oil or HMDS Compound.
8. a kind of sizing of transparent silica gel terminal sleeve according to claim 1, it is characterised in that described inhibitor It is alkynol compound, many vinyl polysiloxanes, amide compound or maleic acid ester type compound one of which or several mixed Compound.
9. the sizing of a kind of transparent silica gel terminal sleeve according to claim 1, it is characterised in that use the sizing The preparation method of the transparent silica gel terminal sleeve is prepared, is comprised the following steps:
(1)Mould is put into heating furnace and is preheating to 70-300 DEG C, above-mentioned sizing is immersed, makes sizing in mould table Face is adhered to, and mould decrease speed is 100-200mm/min, soaks material time 10-50s;
(2)The mould for being attached with sizing is taken out from leaching material pond, the rate of climb is 100-300 mm/min, in 200- After being toasted 20-90 seconds at 400 DEG C, make sizing complete cure;
(3)It will be cooled down 5-20 seconds in the terminal sleeve insertion cooling water of mould and complete cure, with air gun by terminal sleeve stripping, i.e., It can obtain transparent silica gel terminal sleeve.
CN201710038222.6A 2017-01-19 2017-01-19 A kind of sizing of transparent silica gel terminal sleeve and preparation method thereof Pending CN107043540A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112852170A (en) * 2021-01-15 2021-05-28 北京中石伟业科技股份有限公司 Preparation process of single-component silicone rubber capable of being stored at room temperature for long time

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102924926A (en) * 2012-11-01 2013-02-13 深圳市森日有机硅材料有限公司 Liquid silicone rubber composition and preparation method thereof
CN104917009A (en) * 2014-03-14 2015-09-16 吴俊宏 Splicing-type waterproof cable structure and power supply module and waterproof terminal sleeve assembly

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102924926A (en) * 2012-11-01 2013-02-13 深圳市森日有机硅材料有限公司 Liquid silicone rubber composition and preparation method thereof
CN104917009A (en) * 2014-03-14 2015-09-16 吴俊宏 Splicing-type waterproof cable structure and power supply module and waterproof terminal sleeve assembly

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112852170A (en) * 2021-01-15 2021-05-28 北京中石伟业科技股份有限公司 Preparation process of single-component silicone rubber capable of being stored at room temperature for long time

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