CN117467280A - Method for preventing conductive shielding silica gel from aging - Google Patents

Method for preventing conductive shielding silica gel from aging Download PDF

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Publication number
CN117467280A
CN117467280A CN202311514238.1A CN202311514238A CN117467280A CN 117467280 A CN117467280 A CN 117467280A CN 202311514238 A CN202311514238 A CN 202311514238A CN 117467280 A CN117467280 A CN 117467280A
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conductive shielding
solution
silica gel
aging
prepared
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CN202311514238.1A
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Inventor
徐江山
王万俊
颜智宏
杨述霞
方刚
黄正元
赵栋财
张秀英
马鑫
宋谋通
冯泽树
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Jinchuan Group Nickel Cobalt Co ltd
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Jinchuan Group Co Ltd
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Priority to CN202311514238.1A priority Critical patent/CN117467280A/en
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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
    • HELECTRICITY
    • H05ELECTRIC TECHNIQUES NOT OTHERWISE PROVIDED FOR
    • H05KPRINTED CIRCUITS; CASINGS OR CONSTRUCTIONAL DETAILS OF ELECTRIC APPARATUS; MANUFACTURE OF ASSEMBLAGES OF ELECTRICAL COMPONENTS
    • H05K9/00Screening of apparatus or components against electric or magnetic fields
    • H05K9/0073Shielding materials
    • H05K9/0081Electromagnetic shielding materials, e.g. EMI, RFI shielding
    • 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
    • C08K3/00Use of inorganic substances as compounding ingredients
    • C08K3/02Elements
    • C08K3/08Metals
    • C08K2003/0862Nickel
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2201/00Properties
    • C08L2201/08Stabilised against heat, light or radiation or oxydation

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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)
  • Physics & Mathematics (AREA)
  • Electromagnetism (AREA)
  • Engineering & Computer Science (AREA)
  • Microelectronics & Electronic Packaging (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

The invention provides a method for preventing aging of conductive shielding silica gel, belongs to the technical field of powder metallurgy manufacturing, and solves the problem of aging of conductive shielding silica gel, and the method comprises the following steps: preparing monomer solution A and monomer solution B respectively; mixing the solution A and the solution B, filling the mixture into a glass bottle for sealing and preserving, and standing the mixture to obtain colorless transparent liquid to obtain an anti-aging additive for later use; uniformly spraying the prepared anti-aging additive on the surface of the conductive shielding filling material, and drying; and uniformly adding the silica gel, the vulcanizing agent and the curing agent into a rubber mixing machine for repeated extrusion, weighing the dried conductive shielding filler, adding the conductive shielding filler into the rubber mixing machine, uniformly mixing and extruding, taking out the refined silica gel, placing the silica gel into a grinding tool, and curing and forming to obtain the conductive shielding silica gel. The conductive shielding silica gel anti-aging additive prepared by the invention can ensure that the conductive shielding filler has good wettability with silica gel and is firmly bonded, and avoid the conductive filler from falling off due to overlong time or aging of the silica gel at high temperature.

Description

Method for preventing conductive shielding silica gel from aging
Technical Field
The invention belongs to the technical field of powder metallurgy manufacturing, and particularly relates to a method for preventing conductive shielding silica gel from aging.
Background
The conductive shielding silica gel is prepared by uniformly distributing conductive shielding fillers such as nickel-coated copper powder, nickel-coated graphite powder, nickel-coated aluminum powder and the like in the silica gel, and the conductive shielding fillers are mutually contacted and communicated through conductive particles to achieve good conductive performance, and the conductive shielding silica gel has application in military and commercial industries and has the main functions of sealing and electromagnetic shielding. The cable has moderate hardness, high conductivity, good electromagnetic sealing and water vapor sealing capability, is mainly black paste, can improve the electric field distribution of an insulating shielding layer, reduce the damage of insulation and ensure the service life of the cable. The product can be molded or extruded, and can be selected from sheet-like or other punching shapes, the shielding performance is as high as 120dB (10 GHz), and good conductivity (suppression frequency is as high as 40 GHz) can be provided under certain pressure.
The better the dispersibility of the conductive particles in the matrix and the better the combination degree of the matrix and the filler, the better the conductive performance of the composite material, and how to enable the matrix resin and the conductive particles to be well glued together, so that the conductive shielding filler and the silica gel keep good wettability, and the conductive shielding silica gel is important to prevent aging.
Disclosure of Invention
The invention aims to provide a method for preventing aging of conductive shielding silica gel, which aims to solve the problem of aging of the conductive shielding silica gel.
The technical scheme of the invention is as follows: a method of preventing aging of conductive shielding silicone, comprising the steps of:
step one: the monomer solution A and the monomer solution B are respectively prepared, and the preparation method of the monomer solution A is as follows: the solution A is prepared by dissolving five solvents of ethanol, glycol, acetone, methanol and polyethanol in one of four solutes of a silane coupling agent, hydroxycellulose, dimethyl silicone oil and paraffin; the preparation method of the solution B comprises the following steps: the preparation method comprises the steps of preparing an ethyl alcohol solution by dissolving one of five solvents selected from ethanol, ethylene glycol, acetone, methanol and polyethanol in one of four solutes selected from silane coupling agent, hydroxycellulose, dimethyl silicone oil and paraffin, wherein the solutes selected from the ethyl alcohol solution, the ethylene glycol solution and the methyl alcohol solution are different in solute and solvent, and respectively filling the prepared ethyl alcohol solution and methyl alcohol solution into a stainless steel container for sealing and preserving;
step two: mixing the solution A and the solution B, filling the mixture into a glass bottle for sealing and preserving, and standing the mixture to obtain colorless transparent liquid to obtain an anti-aging additive for later use;
step three: uniformly spraying the prepared anti-aging additive on the surface of the conductive shielding filling material, and drying;
step four: and (3) uniformly adding the silica gel, the vulcanizing agent and the curing agent into a rubber mixing machine for repeated extrusion, weighing the conductive shielding filler dried in the third step, adding the conductive shielding filler into the rubber mixing machine, mixing and extruding uniformly, taking out the refined silica gel, placing the silica gel into a grinding tool, and curing and forming to obtain the conductive shielding silica gel.
Further, in the first step, the concentration of the solution A is 10-15g/L, and the concentration of the solution B is 0.5-1.5g/L.
Further, in the second step, the solution A and the solution B are mixed according to the proportion of 1:2; the standing time is 1-3 hours.
Further, in the third step, 3-6mL of anti-aging additive is sprayed according to the proportion of each 100g of conductive shielding filler, and the conductive shielding filler is dried at 80+/-5 ℃.
Further, in the third step, the conductive shielding filler is nickel-coated graphite powder or nickel-coated copper powder or nickel-coated aluminum powder.
In the fourth step, the components added into the rubber mixing machine are prepared according to the following parts by weight: 58-62 parts of silica gel, 1-3 parts of vulcanizing agent, 1-3 parts of curing agent and 8-12 minutes of extrusion time.
Further, in the fourth step, 98-102 parts of selected conductive shielding filler is added after all the component substances are added into a rubber mixing machine and extruded uniformly, and the mixing extrusion time is 18-22 minutes again.
Further, in the fourth step, the curing temperature is 165-175 ℃, the curing pressure is 8-12MPa, and the curing time is 8-12 minutes.
The beneficial effects of the invention are as follows:
1. according to the solubility of the selected solvent, four solutes of a silane coupling agent, hydroxy cellulose, dimethyl silicone oil and paraffin are correspondingly selected, so that on one hand, the selected solutes can be ensured to be dissolved in five solvents, and the solvent and the solute have good dissolving effect; on the other hand, different solutes have different hydrophilicities and adsorptivity, so that two different solutions are required to be prepared in order to ensure that organic and inorganic substances can be well connected together and that good wettability can be ensured.
2. Ethanol, glycol, acetone, methanol and polyethanol are selected as the most common organic solvents, the materials are easy to obtain, the preparation cost is low, and the five solvents are liquid at normal temperature, have the characteristics of low toxicity and easy volatilization, can have good compatibility with a plurality of organic components, have good lubricity, moisture retention, dispersibility and adhesiveness, and are generally used as solvents in industry.
3. After the two solutions are prepared, the two solutions are mixed and kept stand, so that the prepared anti-aging agent has good affinity with silica gel and conductive shielding materials, the conductive shielding filler sprayed with the anti-aging additive has good wettability with the silica gel, and the conductive shielding filler is firmly bonded, and can obviously reduce the resistance of the conductive shielding silica gel.
4. The prepared anti-aging additive is added in the process of preparing the conductive shielding silica gel filler, so that the wettability of the conductive shielding filler and the silica gel can be effectively enhanced, the resistance change of the conductive silica gel is ensured to be less than 5% under the temperature condition of-40-200 ℃, and the change rate of the resistance of the conductive silica gel at normal temperature for 180 days is ensured to be less than 2.5%; the anti-aging additive can volatilize in the rubber mixing process, can not introduce other impurities, can prevent oxidation, has good wettability with silica gel when being sprayed with the conductive shielding filler of the anti-aging additive, is firmly bonded, and can obviously reduce the resistance of the conductive shielding silica gel.
The conductive shielding silica gel anti-aging additive prepared by the invention can ensure that the conductive shielding filler has good wettability with silica gel and is firmly bonded, and avoid the conductive filler from falling off due to overlong time or aging of the silica gel at high temperature.
Detailed Description
The present invention will be described in further detail with reference to examples.
Example 1,
Step one: preparing a first monomer solution and a second monomer solution respectively, wherein the first solution is prepared by dissolving ethanol in a silane coupling agent, and the concentration of the first solution is 10g/L; the solution B is prepared by dissolving ethanol in hydroxy cellulose, the concentration of the solution B is 0.5g/L, and the solution A and the solution B are respectively filled into a stainless steel container for sealing and preserving for later use after being prepared;
step two: mixing the solution A and the solution B according to the proportion of 1:2, filling the mixture into a glass bottle for sealing and preserving, standing for 1 hour, and changing the mixed solution into colorless transparent liquid to obtain an anti-aging additive for later use;
step three: uniformly spraying 3mL of the prepared anti-aging additive according to the proportion of spraying 3mL of the anti-aging additive on each 100g of nickel-coated graphite powder, and drying at 75 ℃ after spraying;
step four: and (3) uniformly adding 58g of silica gel, 1g of vulcanizing agent and 1g of curing agent into a rubber mixing machine, repeatedly extruding for 8 minutes, weighing 98g of dried nickel-coated graphite powder, adding into the rubber mixing machine, mixing and extruding for 18 minutes, uniformly mixing and extruding, taking out the refined silica gel, placing into a grinding tool, curing for 8 minutes at 165 ℃ and 8MPa, and curing and forming to obtain the conductive shielding silica gel.
EXAMPLE 2,
Step one: preparing a first monomer solution and a second monomer solution respectively, wherein the first solution is prepared by dissolving ethylene glycol in hydroxy cellulose, and the concentration of the first solution is 11g/L; the solution B is prepared by dissolving ethanol in dimethyl silicone oil, the concentration of the solution B is 0.7g/L, and the solution A and the solution B are respectively filled into a stainless steel container for sealing and preserving for later use after being prepared;
step two: mixing the solution A and the solution B according to the proportion of 1:2, filling the mixture into a glass bottle for sealing and preserving, standing for 1 hour, and changing the mixed solution into colorless transparent liquid to obtain an anti-aging additive for later use;
step three: uniformly spraying the prepared anti-aging additive according to the proportion of spraying 4mL of the anti-aging additive on each 100g of nickel-coated copper powder, and drying at 80 ℃ after spraying;
step four: uniformly adding 59g of silica gel, 1g of vulcanizing agent and 1g of curing agent into a rubber mixing machine, repeatedly extruding for 9 minutes, weighing 100g of dried nickel-coated copper powder, adding into the rubber mixing machine, mixing and extruding for 19 minutes, uniformly mixing and extruding, taking out the refined silica gel, placing into a grinding tool, curing for 9 minutes at 167 ℃ under the pressure of 9MPa, and curing to obtain the conductive shielding silica gel.
EXAMPLE 3,
Step one: preparing a first monomer solution and a second monomer solution respectively, wherein the first solution is prepared by dissolving acetone in dimethyl silicone oil, and the concentration of the first solution is 12g/L; the solution B is prepared by dissolving glycol in a silane coupling agent, the concentration of the solution B is 0.9g/L, and the solution A and the solution B are respectively filled into a stainless steel container for sealing and preserving for later use after being prepared;
step two: mixing the solution A and the solution B according to the proportion of 1:2, filling the mixture into a glass bottle for sealing and preserving, standing for 2 hours, and changing the mixed solution into colorless transparent liquid to obtain the anti-aging additive for later use;
step three: uniformly spraying the prepared anti-aging additive according to the proportion of spraying 4mL of the anti-aging additive on every 100g of nickel-coated graphite powder, and drying at 80 ℃ after spraying;
step four: and (3) uniformly adding 60g of silica gel, 2g of vulcanizing agent and 2g of curing agent into a rubber mixing machine, repeatedly extruding for 10 minutes, weighing 100g of dried nickel-coated graphite powder, adding into the rubber mixing machine, mixing and extruding for 20 minutes, uniformly mixing and extruding, taking out the refined silica gel, placing into a grinding tool, curing for 10 minutes at 170 ℃ under the pressure of 10MPa, and curing and forming to obtain the conductive shielding silica gel.
EXAMPLE 4,
Step one: preparing a first monomer solution and a second monomer solution respectively, wherein the first solution is prepared by dissolving methanol in paraffin, and the concentration of the first solution is 13g/L; the solution B is prepared by dissolving acetone in dimethyl silicone oil, the concentration of the solution B is 1.3g/L, and the solution A and the solution B are respectively filled into a stainless steel container for sealing and preserving for later use after being prepared;
step two: mixing the solution A and the solution B according to the proportion of 1:2, filling the mixture into a glass bottle for sealing and preserving, standing for 2 hours, and changing the mixed solution into colorless transparent liquid to obtain the anti-aging additive for later use;
step three: uniformly spraying 5mL of the prepared anti-aging additive according to the proportion of spraying 5mL of the anti-aging additive on each 100g of nickel-coated aluminum powder, and drying at 85 ℃ after spraying;
step four: and (3) uniformly adding 60g of silica gel, 3g of vulcanizing agent and 3g of curing agent into a rubber mixing machine, repeatedly extruding for 10 minutes, weighing 100g of dried nickel-coated aluminum powder, adding into the rubber mixing machine, mixing and extruding for 20 minutes, uniformly mixing and extruding, taking out the refined silica gel, placing into a grinding tool, curing for 10 minutes at 172 ℃ under the pressure of 10MPa, and curing and forming to obtain the conductive shielding silica gel.
EXAMPLE 5,
Step one: preparing a first monomer solution and a second monomer solution respectively, wherein the first solution is prepared by dissolving polyethylene alcohol in paraffin, and the concentration of the first solution is 15g/L; the solution B is prepared by dissolving ethanol in hydroxy cellulose, the concentration of the solution B is 1.5g/L, and the solution A and the solution B are respectively filled into a stainless steel container for sealing and preserving for later use after being prepared;
step two: mixing the solution A and the solution B according to the proportion of 1:2, filling the mixture into a glass bottle for sealing and preserving, standing for 3 hours, and changing the mixed solution into colorless transparent liquid to obtain the anti-aging additive for later use;
step three: uniformly spraying 6mL of the prepared anti-aging additive according to the proportion of spraying 6mL of the anti-aging additive on each 100g of nickel-coated aluminum powder, and drying at 85 ℃ after spraying;
step four: and uniformly adding 62g of silica gel, 3g of vulcanizing agent and 3g of curing agent into a rubber mixing machine, repeatedly extruding for 12 minutes, weighing 102g of dried nickel-coated aluminum powder, adding into the rubber mixing machine, mixing and extruding for 22 minutes, uniformly mixing and extruding, taking out the refined silica gel, placing into a grinding tool, curing for 12 minutes at 175 ℃ under the pressure of 12MPa, and curing and forming to obtain the conductive shielding silica gel.
As can be seen from the comparison of the data in Table 1, the anti-aging additive prepared by the method is added in the process of preparing the conductive shielding silica gel filler, so that the wettability of the conductive shielding filler and the silica gel can be effectively enhanced, the resistance change of the conductive silica gel is ensured to be less than 5% under the temperature condition of-40-200 ℃, the change rate of the resistance of the conductive shielding silica gel at normal temperature for 180 days is less than 2.5%, and the conductive shielding silica gel anti-aging additive prepared by the method can ensure that the wettability of the conductive shielding filler and the silica gel is good, the adhesion is firm, and the conductive filler is prevented from falling off due to overlong time or aging of the silica gel at high temperature.

Claims (8)

1. A method for preventing aging of conductive shielding silicone, comprising the steps of: the method comprises the following steps:
step one: the monomer solution A and the monomer solution B are respectively prepared, and the preparation method of the monomer solution A is as follows: the solution A is prepared by dissolving five solvents of ethanol, glycol, acetone, methanol and polyethanol in one of four solutes of a silane coupling agent, hydroxycellulose, dimethyl silicone oil and paraffin; the preparation method of the solution B comprises the following steps: the preparation method comprises the steps of preparing an ethyl alcohol solution by dissolving one of five solvents selected from ethanol, ethylene glycol, acetone, methanol and polyethanol in one of four solutes selected from silane coupling agent, hydroxycellulose, dimethyl silicone oil and paraffin, wherein the solutes selected from the ethyl alcohol solution, the ethylene glycol solution and the methyl alcohol solution are different in solute and solvent, and respectively filling the prepared ethyl alcohol solution and methyl alcohol solution into a stainless steel container for sealing and preserving;
step two: mixing the solution A and the solution B, filling the mixture into a glass bottle for sealing and preserving, and standing the mixture to obtain colorless transparent liquid to obtain an anti-aging additive for later use;
step three: uniformly spraying the prepared anti-aging additive on the surface of the conductive shielding filling material, and drying;
step four: and (3) uniformly adding the silica gel, the vulcanizing agent and the curing agent into a rubber mixing machine for repeated extrusion, weighing the conductive shielding filler dried in the third step, adding the conductive shielding filler into the rubber mixing machine, mixing and extruding uniformly, taking out the refined silica gel, placing the silica gel into a grinding tool, and curing and forming to obtain the conductive shielding silica gel.
2. A method for preventing aging of a conductive shielding silicone as set forth in claim 1, wherein: in the first step, the concentration of the solution A is 10-15g/L, and the concentration of the solution B is 0.5-1.5g/L.
3. A method for preventing aging of a conductive shielding silicone as set forth in claim 1, wherein: in the second step, the solution A and the solution B are mixed according to the proportion of 1:2; the standing time is 1-3 hours.
4. A method for preventing aging of a conductive shielding silicone as set forth in claim 1, wherein: in the third step, 3-6mL of anti-aging additive is sprayed according to the proportion of each 100g of conductive shielding filler, and the conductive shielding filler is dried at 80+/-5 ℃.
5. A method for preventing aging of a conductive shielding silicone as set forth in claim 1, wherein: in the third step, the conductive shielding filler is nickel-coated graphite powder or nickel-coated copper powder or nickel-coated aluminum powder.
6. A method for preventing aging of a conductive shielding silicone as set forth in claim 1, wherein: in the fourth step, the components added into the rubber mixing machine are prepared according to the following parts by weight: 58-62 parts of silica gel, 1-3 parts of vulcanizing agent, 1-3 parts of curing agent and 8-12 minutes of extrusion time.
7. A method for preventing aging of a conductive shielding silicone as set forth in claim 1, wherein: in the fourth step, 98-102 parts of selected conductive shielding filler is added after all the component substances are added into a rubber mixing machine and extruded uniformly, and the secondary mixing extrusion time is 18-22 minutes.
8. A method for preventing aging of a conductive shielding silicone as set forth in claim 1, wherein: in the fourth step, the curing temperature is 165-175 ℃, the curing pressure is 8-12MPa, and the curing time is 8-12 minutes.
CN202311514238.1A 2023-11-14 2023-11-14 Method for preventing conductive shielding silica gel from aging Pending CN117467280A (en)

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