CN110760135A - Gas mask and mask composite material and production process thereof - Google Patents

Gas mask and mask composite material and production process thereof Download PDF

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Publication number
CN110760135A
CN110760135A CN201911090178.9A CN201911090178A CN110760135A CN 110760135 A CN110760135 A CN 110760135A CN 201911090178 A CN201911090178 A CN 201911090178A CN 110760135 A CN110760135 A CN 110760135A
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parts
stirring
modified
mixed
bentonite
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韩非
韩彬
肖曙
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Anhui Submersible Electromechanical Technology Co Ltd
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Anhui Submersible Electromechanical 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
    • C08L23/00Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
    • C08L23/26Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers modified by chemical after-treatment
    • C08L23/28Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers modified by chemical after-treatment by reaction with halogens or compounds containing halogen
    • C08L23/283Halogenated homo- or copolymers of iso-olefins
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J3/00Processes of treating or compounding macromolecular substances
    • C08J3/28Treatment by wave energy or particle radiation
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2323/00Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
    • C08J2323/26Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers modified by chemical after-treatment
    • C08J2323/28Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers modified by chemical after-treatment by reaction with halogens or halogen-containing compounds
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2433/00Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers
    • C08J2433/04Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides, or nitriles thereof; Derivatives of such polymers esters
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J2463/00Characterised by the use of epoxy resins; Derivatives of epoxy resins
    • C08J2463/10Epoxy resins modified by unsaturated compounds
    • 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
    • C08K2201/011Nanostructured additives
    • 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
    • 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

Abstract

The invention discloses a gas mask composite material which comprises the following raw materials in parts by weight: 55-65 parts of butyl chloride rubber, 10-20 parts of mixed three-dimensional reticular graphene, 5-10 parts of carbon black, 4-8 parts of dioctyl sebacate, 2-6 parts of an anti-aging agent, 1-3 parts of an accelerant EDC and 15-25 parts of zinc chloride. The bentonite in the modified chlorinated butyl rubber has a layered structure, the surface activity of the modified chlorinated butyl rubber is enhanced by calcining and activating the modified chlorinated butyl rubber, and then the modified chlorinated butyl rubber and a nano modified liquid are stirred together for reaction, the nano modified liquid adopts a coupling agent to modify nano silicon dioxide to enable the nano silicon dioxide to have an organophilic effect, and the coupling agent in the nano modified liquid is used to modify the bentonite, so that the nano silicon dioxide is firstly attached to the layered structure of the bentonite, the nano silicon dioxide has strong activity and high specific surface area, and can be used as a middle point to graft the chlorinated butyl rubber and the organized bentonite.

Description

Gas mask and mask composite material and production process thereof
Technical Field
The invention relates to the technical field of gas mask materials, in particular to a gas mask composite material and a production process thereof.
Background
The gas mask is a personal special labor protection article, is also an individual protective article, is worn on the head to protect the respiratory organs, eyes and face of a person and prevent toxic substances such as poison gas, dust, bacteria, toxic and harmful gas or steam and the like from damaging the personal protective apparatus. The gas mask is widely applied to the fields of petroleum, chemical industry, mines, metallurgy, military, fire fighting, emergency rescue and relief, health and epidemic prevention, scientific and technological environmental protection, mechanical manufacturing and the like, and can play an important role in protecting the personal respiratory system in cities with severe haze and photochemical smog. The gas mask can be divided into a full mask and a half mask from the aspect of modeling, and the full mask is divided into a positive pressure type and a negative pressure type.
The material that current gas mask face guard adopted is gas permeability higher, and the material weatherability is not good simultaneously, leads to the chap easily, and then further influences gas permeability.
The prior Chinese patent literature publication numbers are as follows: CN104341685A discloses a formula of a flame-retardant corrosion-resistant gas mask cover body rubber material, belonging to the technical field of gas mask covers, which comprises the following components in parts by weight: 100 parts of butyl chloride rubber, 8-12 parts of zinc oxide, 0.3-0.5 part of magnesium oxide, 1.5-2.0 parts of accelerator ZDC, 2-3 parts of anti-aging agent, 0.5-2 parts of chlorinated paraffin, 30-40 parts of reinforcing carbon black, 3-6 parts of dioctyl phthalate and 1.2-2 parts of stearic acid, wherein the raw materials adopt butyl chloride rubber as a base material, and the butyl chloride rubber has low weather resistance and gas permeability, but other raw materials in the rubber material are conventional, and the synthesized material performance is obvious, so further improvement treatment is still needed.
Disclosure of Invention
The invention aims to provide a gas mask composite material and a production process thereof, which aim to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme:
a gas mask and mask composite material comprises the following raw materials in parts by weight:
55-65 parts of modified butyl chloride, 10-20 parts of mixed three-dimensional reticular graphene, 5-10 parts of carbon black, 4-8 parts of dioctyl sebacate, 2-6 parts of an anti-aging agent, 1-3 parts of an accelerant EDC and 15-25 parts of zinc chloride.
Preferably, the gas mask and face mask composite material comprises the following raw materials in parts by weight:
60 parts of modified butyl chloride rubber, 15 parts of mixed three-dimensional reticular graphene, 7.5 parts of carbon black, 6 parts of dioctyl sebacate, 4 parts of anti-aging agent, 2 parts of accelerant EDC and 20 parts of zinc chloride.
Preferably, the preparation method of the modified chlorinated butyl rubber comprises the following steps:
step one, activating bentonite: calcining bentonite at 800 ℃ for 1-2h at 600-plus, naturally cooling to room temperature, then sending the bentonite and the nano modified liquid into a magnetic stirrer according to the weight ratio of 1:3, starting the magnetic stirrer, raising the stirring temperature to 75-85 ℃, stirring at the rotation speed of 350-plus 450r/min for 2-5h, after the stirring is finished, centrifuging and drying;
step two, activating bentonite modified butyl chloride: adding the activated bentonite prepared in the step one into the chlorinated butyl rubber according to the weight ratio of 1:5, stirring for 1-2h at the rotating speed of 1100-1500r/min, then adding into a double-screw extruder for extrusion at the extrusion temperature of 145-155 ℃, then cooling to room temperature, and granulating through 200-300 meshes to obtain the modified chlorinated butyl rubber.
Preferably, the preparation method of the nano-modification liquid comprises the steps of adding nano-silica into an ethanol solution according to the weight ratio of 1:9, then adding a silane coupling agent KH560 accounting for 30-40% of the total amount of the nano-silica, stirring at a low rotation speed of 200r/min for 1-2h, and finishing stirring.
Preferably, the preparation method of the hybrid three-dimensional reticular graphene comprises the steps of firstly oxidizing the graphene for 30-40min by using mixed acid of concentrated sulfuric acid and concentrated nitric acid according to the weight ratio of 2:1, then washing for 1-2 times by using dilute hydrochloric acid, then stripping for 20min by using ultrasound, then placing the graphene in a coupling agent for ultrasonic dispersion for 10-20min, wherein the ultrasonic power is 100-200W, then placing the graphene in a protective liquid, stirring for 20-30min at the high rotating speed of 1500r/min for 1000-1500r/min, then stirring for 60-70min at the low speed of 300r/min for 200-70 min, stopping stirring, then standing for 20-30min at the high pressure of 10-20MPa, carrying out ultraviolet light treatment in the standing process, and obtaining the light intensity of 500W/m2And standing and centrifuging to obtain the mixed three-dimensional reticular graphene.
Preferably, the preparation method of the protective liquid comprises the steps of adding vinyl ester resin into the nano silica sol according to the weight ratio of 1:3, then adding a-eucryptite powder and ceramic fibers, stirring for 1-2h at the rotating speed of 200-500r/min, finally adding acrylate emulsion, continuing stirring for 20-30min, and obtaining the protective liquid after the stirring is finished.
Preferably, the carbon black is a mixture of medium super carbon black and high wear-resistant carbon black in a weight ratio of 1: 3; the anti-aging agent is one or a combination of more of an anti-aging agent 264 and an anti-aging agent MB.
The invention also provides a process for producing the gas mask composite material, which comprises the following steps:
weighing raw materials of each component according to requirements;
step two, sequentially adding the modified butyl chloride, the carbon black, the dioctyl sebacate, the anti-aging agent, the accelerant EDC and the zinc chloride into a high-speed stirrer, stirring for 10-20min at the rotating speed of 800-350 r/min, and then continuously stirring for 30-40min at the rotating speed of 250-350r/min to obtain a mixed material A;
step three, mixing the mixed material A for 35-45min at 75-85 ℃ for the first time, then performing primary thin-passing for 3-6 times, then adding the mixed three-dimensional reticular graphene, mixing for the second time at 65-75 ℃ for 45-55min, then performing secondary thin-passing for 5-9 times, and finally discharging to obtain mixed rubber B;
step four, placing the mixed material B into a plasma irradiation box, treating for 10-20min, standing at-2 ℃ for 2h, raising the temperature to 5 ℃ at the speed of 1 ℃/h, and then preserving heat for 20min to obtain a reinforced primer C;
and step five, vulcanizing the reinforced primer C in the step four, wherein the vulcanization temperature is 120-160 ℃, the vulcanization time is 35-45min, the vulcanization pressure is 15-25MPa, and the vulcanization is finished to obtain the gas mask composite material.
Preferably, the irradiation power in the plasma irradiation box is 1000-1500W, and nitrogen atmosphere is adopted for irradiation.
Compared with the prior art, the invention has the following beneficial effects:
the bentonite in the modified chlorinated butyl rubber has a layered structure, the surface activity of the modified chlorinated butyl rubber is enhanced by calcining and activating the modified chlorinated butyl rubber, and then the modified chlorinated butyl rubber is stirred and reacted with the nano modified liquid together, the nano modified liquid adopts the coupling agent to modify the nano silicon dioxide firstly, so that the nano silicon dioxide has the organophilic effect, and then the coupling agent in the nano modified liquid is used to modify the bentonite, so that the nano silicon dioxide is firstly attached to the layered structure of the bentonite, the nano silicon dioxide has strong activity and high specific surface area and can be used as a middle point to graft the chlorinated butyl rubber and the organic bentonite, so that the bentonite is inserted into the chlorinated butyl rubber to a greater extent, the air permeability of the chlorinated butyl rubber is perfected, the integral air permeability of the material is greatly improved, and the mixed three-dimensional reticular graphene can be coated with the chlorinated butyl rubber raw material in a three-dimensional reticular form after, the protective liquid adopted by the mixed three-dimensional reticular graphene is cooperated with the reticular graphene, so that the overall weather resistance and corrosion resistance of the material can be improved, the weather resistance of the material is obviously improved, the vinyl ester resin in the protective liquid is modified epoxy resin, the performance is more excellent, the acrylate emulsion is often used as a cement mortar dispersion, the vinyl ester resin and the acrylate emulsion are dispersed in a nano silica sol medium, the vinyl ester resin and the acrylate emulsion are mutually matched, the raw material of the protective liquid is easier to be mixed with the graphene, the additional performance of the reticular graphene is perfected, the alpha-eucryptite powder and the ceramic fiber are used as fillers, so that the structure of an anticorrosive material in a reticular protective layer is more compact, the prepared material has low air permeability and more excellent weather resistance, and the added carbon black is medium-ultra-carbon black and high-wear-resistance carbon black, so that the wear resistance of, thereby prolonging the service life of the material and having better air permeability effect; the gas mask and face mask composite material is prepared by mixing and vulcanizing twice and performing thin-pass twice in the preparation process, meanwhile, the adaptability of the material body is improved by adopting plasma and temperature change, and finally, the material is vulcanized again, so that the prepared material is improved in weather resistance and is not easy to crack.
Detailed Description
The technical solutions in the embodiments of the present invention are clearly and completely described below with reference to specific embodiments, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1:
the gas mask composite material comprises the following raw materials in parts by weight:
55 parts of modified butyl chloride, 10 parts of mixed three-dimensional reticular graphene, 5 parts of carbon black, 4 parts of dioctyl sebacate, 2 parts of an anti-aging agent, 1 part of an accelerant EDC and 15 parts of zinc chloride.
The preparation method of the modified chlorinated butyl rubber of the embodiment comprises the following steps:
step one, activating bentonite: calcining bentonite at 600 ℃ for 1h, naturally cooling to room temperature, then feeding the bentonite and the nano modified liquid into a magnetic stirrer according to the weight ratio of 1:3, starting the magnetic stirrer, raising the stirring temperature to 75 ℃, stirring at the rotating speed of 350r/min for 2h, after stirring, centrifuging and drying;
step two, activating bentonite modified butyl chloride: and (2) adding the activated bentonite prepared in the step one into chlorinated butyl rubber according to the weight ratio of 1:5, stirring for 1h at the rotating speed of 1100r/min, then adding into a double-screw extruder for extrusion at the extrusion temperature of 145 ℃, cooling to room temperature, and granulating through a 200-mesh sieve to obtain the modified chlorinated butyl rubber.
The preparation method of the nano modified solution of the embodiment includes adding nano silicon dioxide into an ethanol solution according to a weight ratio of 1:9, then adding a silane coupling agent KH560 with a total amount of 30% of the nano silicon dioxide, stirring at a low rotation speed of 100r/min for 1 hour, and finishing stirring.
The preparation method of the hybrid three-dimensional reticular graphene comprises the steps of firstly oxidizing graphene for 30min by using mixed acid of concentrated sulfuric acid and concentrated nitric acid according to a weight ratio of 2:1, then washing for 1 time by using dilute hydrochloric acid, then stripping for 20min by using ultrasound, then placing the graphene in a coupling agent for ultrasonic dispersion for 10min with an ultrasonic power of 100W, then placing the graphene in a protective liquid, stirring for 20min at a high rotating speed of 1000r/min, then stirring for 60min at a low speed of 200r/min, finishing stirring, standing for 20min at a high pressure of 10MPa, and carrying out ultraviolet light treatment in a standing process, wherein the light intensity is 200W/m2And standing and centrifuging to obtain the mixed three-dimensional reticular graphene.
The preparation method of the protective liquid in the embodiment comprises the steps of adding vinyl ester resin into nano silica sol according to the weight ratio of 1:3, then adding a-eucryptite powder and ceramic fibers, stirring for 1 hour at the rotating speed of 200r/min, finally adding acrylate emulsion, continuing stirring for 20 minutes, and obtaining the protective liquid after stirring.
The carbon black of the embodiment is a mixture of medium super carbon black and high wear-resistant carbon black according to the weight ratio of 1: 3; the anti-aging agent is an anti-aging agent 264.
The process for producing the respirator mask composite material of the embodiment comprises the following steps:
weighing raw materials of each component according to requirements;
step two, sequentially adding the modified butyl chloride, the carbon black, the dioctyl sebacate, the anti-aging agent, the accelerant EDC and the zinc chloride into a high-speed stirrer, stirring for 10min at the rotating speed of 800r/min, and then continuously stirring for 30min at the rotating speed of 250r/min to obtain a mixed material A;
step three, mixing the mixed material A for the first time at 75 ℃ for 35min, then performing primary thin pass for 3 times, then adding the mixed three-dimensional reticular graphene, performing secondary mixing at 65 ℃, mixing for 45min, then performing secondary thin pass for 5 times, and finally discharging to obtain mixed rubber B;
step four, placing the mixed material B into a plasma irradiation box, treating for 10min, standing for 2h at-2 ℃, raising the temperature to 5 ℃ at the speed of 1 ℃/h, and then preserving heat for 20min to obtain a reinforced primer C;
and step five, vulcanizing the reinforced primer C in the step four, wherein the vulcanization temperature is 120 ℃, the vulcanization time is 35min, the vulcanization pressure is 15MPa, and the gas mask and mask composite material is obtained after vulcanization.
The irradiation power in the plasma irradiation chamber of this embodiment was 1000W, and nitrogen atmosphere was used for irradiation.
Example 2:
the gas mask composite material comprises the following raw materials in parts by weight:
65 parts of modified butyl chloride rubber, 20 parts of mixed three-dimensional reticular graphene, 10 parts of carbon black, 8 parts of dioctyl sebacate, 6 parts of an anti-aging agent, 3 parts of an accelerant EDC and 25 parts of zinc chloride.
The preparation method of the modified chlorinated butyl rubber of the embodiment comprises the following steps:
step one, activating bentonite: calcining bentonite at 800 ℃ for 2 hours, naturally cooling to room temperature, then feeding the bentonite and the nano modified liquid into a magnetic stirrer according to the weight ratio of 1:3, starting the magnetic stirrer, raising the stirring temperature to 85 ℃, stirring at the rotating speed of 450r/min for 5 hours, after stirring, centrifuging and drying;
step two, activating bentonite modified butyl chloride: and (2) adding the activated bentonite prepared in the step one into chlorinated butyl rubber according to the weight ratio of 1:5, stirring for 2 hours at the rotating speed of 1500r/min, then adding into a double-screw extruder for extrusion at the extrusion temperature of 155 ℃, cooling to room temperature, and granulating through 300 meshes to obtain the modified chlorinated butyl rubber.
The preparation method of the nano modified solution of the embodiment includes adding nano silicon dioxide into an ethanol solution according to a weight ratio of 1:9, then adding a silane coupling agent KH560 with a total amount of 40% of the nano silicon dioxide, stirring at a low rotation speed of 200r/min for 2 hours, and finishing stirring.
The preparation method of the hybrid three-dimensional reticular graphene comprises the steps of firstly oxidizing graphene for 40min by using mixed acid of concentrated sulfuric acid and concentrated nitric acid according to a weight ratio of 2:1, then washing for 2 times by using dilute hydrochloric acid, then stripping for 20min by using ultrasound, then placing the graphene in a coupling agent for ultrasonic dispersion for 20min with an ultrasonic power of 200W, then placing the graphene in a protective liquid, stirring for 30min at a high rotating speed of 1500r/min, then stirring for 70min at a low speed of 300r/min, finishing stirring, standing for 30min at a high pressure of 20MPa, and carrying out ultraviolet light treatment in a standing process, wherein the light intensity is 500W/m2And standing and centrifuging to obtain the mixed three-dimensional reticular graphene.
The preparation method of the protective liquid in the embodiment comprises the steps of adding vinyl ester resin into nano silica sol according to the weight ratio of 1:3, then adding a-eucryptite powder and ceramic fibers, stirring for 2 hours at the rotating speed of 500r/min, finally adding acrylate emulsion, continuing stirring for 30 minutes, and obtaining the protective liquid after stirring.
The carbon black of the embodiment is a mixture of medium super carbon black and high wear-resistant carbon black according to the weight ratio of 1: 3; the anti-aging agent is an anti-aging agent 264.
The process for producing the respirator mask composite material of the embodiment comprises the following steps:
weighing raw materials of each component according to requirements;
step two, sequentially adding the modified butyl chloride, the carbon black, the dioctyl sebacate, the anti-aging agent, the accelerant EDC and the zinc chloride into a high-speed stirrer, stirring for 20min at the rotating speed of 1200r/min, and then continuously stirring for 40min at the rotating speed of 350r/min to obtain a mixed material A;
step three, mixing the mixed material A for the first time at 85 ℃ for 45min, then performing primary thin pass for 6 times, then adding the mixed three-dimensional reticular graphene, performing secondary mixing at 75 ℃ for 55min, then performing secondary thin pass for 9 times, and finally discharging to obtain mixed rubber B;
step four, placing the mixed material B into a plasma irradiation box, treating for 20min, standing for 2h at-2 ℃, raising the temperature to 5 ℃ at the speed of 1 ℃/h, and then preserving heat for 20min to obtain a reinforced primer C;
and step five, vulcanizing the reinforced primer C in the step four, wherein the vulcanization temperature is 160 ℃, the vulcanization time is 45min, the vulcanization pressure is 25MPa, and the gas mask and mask composite material is obtained after vulcanization.
The irradiation power in the plasma irradiation box of this example was 1500W, and nitrogen atmosphere was used for irradiation.
Example 3:
the gas mask composite material comprises the following raw materials in parts by weight:
60 parts of modified butyl chloride rubber, 15 parts of mixed three-dimensional reticular graphene, 7.5 parts of carbon black, 6 parts of dioctyl sebacate, 4 parts of anti-aging agent, 2 parts of accelerant EDC and 20 parts of zinc chloride.
The preparation method of the modified chlorinated butyl rubber of the embodiment comprises the following steps:
step one, activating bentonite: calcining bentonite at 700 ℃ for 1.5h, naturally cooling to room temperature, then feeding the bentonite and the nano modified liquid into a magnetic stirrer according to the weight ratio of 1:3, starting the magnetic stirrer, raising the stirring temperature to 80 ℃, stirring at the rotating speed of 400r/min for 3.5h, centrifuging and drying after the stirring is finished;
step two, activating bentonite modified butyl chloride: and (2) adding the activated bentonite prepared in the step one into chlorinated butyl rubber according to the weight ratio of 1:5, stirring for 1.5h at the rotating speed of 1300r/min, then adding into a double-screw extruder for extrusion at the extrusion temperature of 150 ℃, cooling to room temperature, and granulating through a 250-mesh sieve to obtain the modified chlorinated butyl rubber.
The preparation method of the nano modified solution of the embodiment includes adding nano silicon dioxide into an ethanol solution according to a weight ratio of 1:9, then adding a silane coupling agent KH560 accounting for 35% of the total amount of the nano silicon dioxide, stirring at a low rotation speed of 150r/min for 1.5h, and finishing stirring.
The preparation method of the hybrid three-dimensional reticular graphene comprises the steps of firstly oxidizing the graphene for 35min by using mixed acid of concentrated sulfuric acid and concentrated nitric acid according to a weight ratio of 2:1, then washing for 2 times by using dilute hydrochloric acid, then stripping for 20min by using ultrasound, then placing the graphene in a coupling agent for ultrasonic dispersion for 15min with an ultrasonic power of 150W, then placing the graphene in a protective liquid, stirring for 25min at a high rotating speed of 1300r/min, then stirring for 65min at a low speed of 250/min, finishing stirring, standing for 25min at a high pressure of 15MPa, and carrying out ultraviolet light treatment in a standing process, wherein the light intensity is 350W/m2And standing and centrifuging to obtain the mixed three-dimensional reticular graphene.
The preparation method of the protective liquid in the embodiment comprises the steps of adding vinyl ester resin into nano silica sol according to the weight ratio of 1:3, then adding a-eucryptite powder and ceramic fibers, stirring for 1.5 hours at the rotating speed of 350r/min, finally adding acrylate emulsion, continuing stirring for 25 minutes, and obtaining the protective liquid after stirring.
The carbon black of the embodiment is a mixture of medium super carbon black and high wear-resistant carbon black according to the weight ratio of 1: 3; the anti-aging agent is an anti-aging agent 264.
The process for producing the respirator mask composite material of the embodiment comprises the following steps:
weighing raw materials of each component according to requirements;
step two, sequentially adding the modified butyl chloride, the carbon black, the dioctyl sebacate, the anti-aging agent, the accelerant EDC and the zinc chloride into a high-speed stirrer, stirring for 15min at the rotating speed of 1000r/min, and then continuously stirring for 35min at the rotating speed of 300r/min to obtain a mixed material A;
step three, mixing the mixed material A for the first time at the mixing temperature of 80 ℃ for 40min, then performing primary thin pass for 5 times, then adding the mixed three-dimensional reticular graphene, performing secondary mixing at the mixing temperature of 70 ℃, mixing for 40min, then performing secondary thin pass for 7 times, and finally discharging to obtain mixed rubber B;
step four, placing the mixed material B into a plasma irradiation box, treating for 15min, standing for 2h at-2 ℃, raising the temperature to 5 ℃ at the speed of 1 ℃/h, and then preserving heat for 20min to obtain a reinforced primer C;
and step five, vulcanizing the reinforced primer C in the step four, wherein the vulcanization temperature is 140 ℃, the vulcanization time is 40min, the vulcanization pressure is 20MPa, and the gas mask and mask composite material is obtained after vulcanization.
The irradiation power in the plasma irradiation chamber of this example was 1250W, and nitrogen atmosphere was used for irradiation.
Comparative example 1:
the material and preparation process are basically the same as those of example 3, except that no nano-modification liquid is added in the modification of the chlorinated butyl rubber.
Comparative example 2:
the material and preparation process are basically the same as those of example 3, except that the hybrid three-dimensional network graphene is not added.
Comparative example 3:
the materials and preparation process are basically the same as those of example 3, except that Chinese patent document publication numbers are adopted: CN104341685A raw material and method of example 1.
The materials of examples 1-3 and comparative examples 1-3 were tested under conventional conditions, 2% NaCl for 1h, and UV light for 1h, respectively, and the test results are shown in Table 1
TABLE 1
As can be seen from Table 1, the material of example 3 has a permeability of 0.85cm under conventional conditions3/(m224h.0.5MPa), comparative example 3 was 0.98cm3/(m224h.0.5MPa), and after 2% of sodium chloride is soaked for 1h and ultraviolet illumination is carried out for 1h, the air permeability of the material in the comparative example 3 is obviously poor, but the air permeability of the material is not greatly different, so that the material has good weather resistance and low air permeability.
It will be evident to those skilled in the art that the invention is not limited to the details of the foregoing illustrative embodiments, and that the present invention may be embodied in other specific forms without departing from the spirit or essential attributes thereof. The present embodiments are therefore to be considered in all respects as illustrative and not restrictive, the scope of the invention being indicated by the appended claims rather than by the foregoing description, and all changes which come within the meaning and range of equivalency of the claims are therefore intended to be embraced therein.
Furthermore, it should be understood that although the present description refers to embodiments, not every embodiment may contain only a single embodiment, and such description is for clarity only, and those skilled in the art should integrate the description, and the embodiments may be combined as appropriate to form other embodiments understood by those skilled in the art.

Claims (9)

1. The gas mask and mask composite material is characterized by comprising the following raw materials in parts by weight:
55-65 parts of modified butyl chloride, 10-20 parts of mixed three-dimensional reticular graphene, 5-10 parts of carbon black, 4-8 parts of dioctyl sebacate, 2-6 parts of an anti-aging agent, 1-3 parts of an accelerant EDC and 15-25 parts of zinc chloride.
2. The respirator facepiece composite of claim 1, comprising the following raw materials in parts by weight:
60 parts of modified butyl chloride rubber, 15 parts of mixed three-dimensional reticular graphene, 7.5 parts of carbon black, 6 parts of dioctyl sebacate, 4 parts of anti-aging agent, 2 parts of accelerant EDC and 20 parts of zinc chloride.
3. The respirator mask composite of claim 1, wherein the modified chlorinated butyl rubber is prepared by the following steps:
step one, activating bentonite: calcining bentonite at 800 ℃ for 1-2h at 600-plus, naturally cooling to room temperature, then sending the bentonite and the nano modified liquid into a magnetic stirrer according to the weight ratio of 1:3, starting the magnetic stirrer, raising the stirring temperature to 75-85 ℃, stirring at the rotation speed of 350-plus 450r/min for 2-5h, after the stirring is finished, centrifuging and drying;
step two, activating bentonite modified butyl chloride: adding the activated bentonite prepared in the step one into the chlorinated butyl rubber according to the weight ratio of 1:5, stirring for 1-2h at the rotating speed of 1100-1500r/min, then adding into a double-screw extruder for extrusion at the extrusion temperature of 145-155 ℃, then cooling to room temperature, and granulating through 200-300 meshes to obtain the modified chlorinated butyl rubber.
4. The composite material for the gas mask and the mask as claimed in claim 3, wherein the nano modified solution is prepared by adding nano silica into ethanol solution according to the weight ratio of 1:9, then adding silane coupling agent KH560 accounting for 30-40% of the total amount of the nano silica, and then stirring at a low speed of 100-200r/min for 1-2h, and finishing the stirring.
5. The respirator mask composite material as claimed in claim 1, wherein the preparation method of the hybrid three-dimensional network graphene comprises the steps of oxidizing graphene with a mixed acid of concentrated sulfuric acid and concentrated nitric acid at a weight ratio of 2:1 for 30-40min, washing with dilute hydrochloric acid for 1-2 times, ultrasonically stripping for 20min, ultrasonically dispersing in a coupling agent for 10-20min at an ultrasonic power of 100-Stirring at low speed for 60-70min, standing at 10-20MPa for 20-30min, and ultraviolet irradiation treating at 200W/m2And standing and centrifuging to obtain the mixed three-dimensional reticular graphene.
6. The composite material for the gas mask and the face mask as claimed in claim 5, wherein the protective solution is prepared by adding vinyl ester resin into the nano silica sol according to the weight ratio of 1:3, then adding a-eucryptite powder and ceramic fiber, stirring for 1-2h at the rotation speed of 200-one and 500r/min, finally adding acrylate emulsion, continuing stirring for 20-30min, and obtaining the protective solution after the stirring is finished.
7. The respirator mask composite of claim 1, wherein the carbon black is a mixture of medium ultra carbon black and high abrasion carbon black in a weight ratio of 1: 3; the anti-aging agent is one or a combination of more of an anti-aging agent 264 and an anti-aging agent MB.
8. A process for producing a respirator mask composite according to any one of claims 1 to 7, comprising the steps of:
weighing raw materials of each component according to requirements;
step two, sequentially adding the modified butyl chloride, the carbon black, the dioctyl sebacate, the anti-aging agent, the accelerant EDC and the zinc chloride into a high-speed stirrer, stirring for 10-20min at the rotating speed of 800-350 r/min, and then continuously stirring for 30-40min at the rotating speed of 250-350r/min to obtain a mixed material A;
step three, mixing the mixed material A for 35-45min at 75-85 ℃ for the first time, then performing primary thin-passing for 3-6 times, then adding the mixed three-dimensional reticular graphene, mixing for the second time at 65-75 ℃ for 45-55min, then performing secondary thin-passing for 5-9 times, and finally discharging to obtain mixed rubber B;
step four, placing the mixed material B into a plasma irradiation box, treating for 10-20min, standing at-2 ℃ for 2h, raising the temperature to 5 ℃ at the speed of 1 ℃/h, and then preserving heat for 20min to obtain a reinforced primer C;
and step five, vulcanizing the reinforced primer C in the step four, wherein the vulcanization temperature is 120-160 ℃, the vulcanization time is 35-45min, the vulcanization pressure is 15-25MPa, and the vulcanization is finished to obtain the gas mask composite material.
9. The process for producing a respirator mask composite material as claimed in claim 8, wherein the irradiation power in the plasma irradiation chamber is 1000-1500W, and the irradiation is performed in a nitrogen atmosphere.
CN201911090178.9A 2019-11-08 2019-11-08 Gas mask and mask composite material and production process thereof Pending CN110760135A (en)

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CN111423650A (en) * 2020-05-14 2020-07-17 安徽长远机电股份有限公司 Heat-resistant polyethylene cable material and preparation method thereof
CN113308875A (en) * 2021-06-07 2021-08-27 宜禾股份有限公司 High-acid-alkali-resistance flame-retardant fabric for work clothes
CN114477981A (en) * 2022-02-21 2022-05-13 广东欧文莱陶瓷有限公司 Oil-stain-resistant ceramic sheet and preparation method thereof
CN114685903A (en) * 2022-05-07 2022-07-01 安徽潜隆机电科技有限公司 Rubber for gas mask cover

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Cited By (5)

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Publication number Priority date Publication date Assignee Title
CN111423650A (en) * 2020-05-14 2020-07-17 安徽长远机电股份有限公司 Heat-resistant polyethylene cable material and preparation method thereof
CN113308875A (en) * 2021-06-07 2021-08-27 宜禾股份有限公司 High-acid-alkali-resistance flame-retardant fabric for work clothes
CN114477981A (en) * 2022-02-21 2022-05-13 广东欧文莱陶瓷有限公司 Oil-stain-resistant ceramic sheet and preparation method thereof
CN114477981B (en) * 2022-02-21 2022-10-14 广东欧文莱陶瓷有限公司 Oil-stain-resistant ceramic sheet and preparation method thereof
CN114685903A (en) * 2022-05-07 2022-07-01 安徽潜隆机电科技有限公司 Rubber for gas mask cover

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