CN112625625B - Preparation method of low-temperature adhesive for low-temperature pump activated carbon adsorption material - Google Patents
Preparation method of low-temperature adhesive for low-temperature pump activated carbon adsorption material Download PDFInfo
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- CN112625625B CN112625625B CN202011428934.7A CN202011428934A CN112625625B CN 112625625 B CN112625625 B CN 112625625B CN 202011428934 A CN202011428934 A CN 202011428934A CN 112625625 B CN112625625 B CN 112625625B
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 85
- 239000000463 material Substances 0.000 title claims abstract description 23
- 238000001179 sorption measurement Methods 0.000 title claims abstract description 18
- 239000000853 adhesive Substances 0.000 title claims abstract description 17
- 230000001070 adhesive effect Effects 0.000 title claims abstract description 17
- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims description 62
- 239000000843 powder Substances 0.000 claims description 60
- 229920002493 poly(chlorotrifluoroethylene) Polymers 0.000 claims description 56
- 239000005023 polychlorotrifluoroethylene (PCTFE) polymer Substances 0.000 claims description 56
- -1 polychlorotrifluoroethylene Polymers 0.000 claims description 55
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 53
- 239000000243 solution Substances 0.000 claims description 44
- 239000000203 mixture Substances 0.000 claims description 40
- 238000003756 stirring Methods 0.000 claims description 36
- NIXOWILDQLNWCW-UHFFFAOYSA-N 2-Propenoic acid Natural products OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 32
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 claims description 28
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 24
- 238000003825 pressing Methods 0.000 claims description 24
- 239000008367 deionised water Substances 0.000 claims description 20
- 229910021641 deionized water Inorganic materials 0.000 claims description 20
- 229910021389 graphene Inorganic materials 0.000 claims description 20
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 18
- 239000007789 gas Substances 0.000 claims description 18
- 239000012745 toughening agent Substances 0.000 claims description 18
- 239000011812 mixed powder Substances 0.000 claims description 16
- 239000000725 suspension Substances 0.000 claims description 16
- LPXPTNMVRIOKMN-UHFFFAOYSA-M sodium nitrite Chemical compound [Na+].[O-]N=O LPXPTNMVRIOKMN-UHFFFAOYSA-M 0.000 claims description 14
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 12
- 239000012153 distilled water Substances 0.000 claims description 12
- 238000005406 washing Methods 0.000 claims description 12
- 238000001816 cooling Methods 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 11
- 238000000034 method Methods 0.000 claims description 11
- HVBSAKJJOYLTQU-UHFFFAOYSA-N 4-aminobenzenesulfonic acid Chemical compound NC1=CC=C(S(O)(=O)=O)C=C1 HVBSAKJJOYLTQU-UHFFFAOYSA-N 0.000 claims description 9
- 229910052757 nitrogen Inorganic materials 0.000 claims description 9
- 229950000244 sulfanilic acid Drugs 0.000 claims description 9
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- 239000007864 aqueous solution Substances 0.000 claims description 8
- 239000002131 composite material Substances 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- 239000005457 ice water Substances 0.000 claims description 8
- 238000002156 mixing Methods 0.000 claims description 8
- 230000007935 neutral effect Effects 0.000 claims description 8
- 238000009832 plasma treatment Methods 0.000 claims description 8
- 239000012286 potassium permanganate Substances 0.000 claims description 8
- VWDWKYIASSYTQR-UHFFFAOYSA-N sodium nitrate Chemical compound [Na+].[O-][N+]([O-])=O VWDWKYIASSYTQR-UHFFFAOYSA-N 0.000 claims description 8
- 238000009210 therapy by ultrasound Methods 0.000 claims description 8
- 239000011259 mixed solution Substances 0.000 claims description 7
- 235000010288 sodium nitrite Nutrition 0.000 claims description 7
- MYMOFIZGZYHOMD-UHFFFAOYSA-N Dioxygen Chemical compound O=O MYMOFIZGZYHOMD-UHFFFAOYSA-N 0.000 claims description 6
- 238000005086 pumping Methods 0.000 claims description 6
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 4
- 238000010306 acid treatment Methods 0.000 claims description 4
- 239000012295 chemical reaction liquid Substances 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 4
- 238000010790 dilution Methods 0.000 claims description 4
- 239000012895 dilution Substances 0.000 claims description 4
- 229910001882 dioxygen Inorganic materials 0.000 claims description 4
- 239000003517 fume Substances 0.000 claims description 4
- 239000011521 glass Substances 0.000 claims description 4
- 239000003292 glue Substances 0.000 claims description 4
- 239000000178 monomer Substances 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 4
- 238000004321 preservation Methods 0.000 claims description 4
- 239000000047 product Substances 0.000 claims description 4
- 230000001681 protective effect Effects 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- 238000000926 separation method Methods 0.000 claims description 4
- 229910000033 sodium borohydride Inorganic materials 0.000 claims description 4
- 239000012279 sodium borohydride Substances 0.000 claims description 4
- 235000010344 sodium nitrate Nutrition 0.000 claims description 4
- 239000004317 sodium nitrate Substances 0.000 claims description 4
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 claims description 4
- 235000019345 sodium thiosulphate Nutrition 0.000 claims description 4
- 239000007787 solid Substances 0.000 claims description 4
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims description 4
- 239000006228 supernatant Substances 0.000 claims description 4
- 238000009966 trimming Methods 0.000 claims description 4
- 238000001291 vacuum drying Methods 0.000 claims description 4
- 238000005303 weighing Methods 0.000 claims description 4
- 229920001780 ECTFE Polymers 0.000 claims description 3
- 229920001577 copolymer Polymers 0.000 claims description 3
- 238000004090 dissolution Methods 0.000 claims description 3
- 230000008569 process Effects 0.000 claims description 2
- 230000006378 damage Effects 0.000 description 16
- 230000000052 comparative effect Effects 0.000 description 9
- 239000007788 liquid Substances 0.000 description 5
- 239000003463 adsorbent Substances 0.000 description 4
- 229920001875 Ebonite Polymers 0.000 description 3
- 230000008859 change Effects 0.000 description 3
- 238000007731 hot pressing Methods 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000002184 metal Substances 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 2
- 238000009835 boiling Methods 0.000 description 2
- 238000007654 immersion Methods 0.000 description 2
- 239000003949 liquefied natural gas Substances 0.000 description 2
- 239000003921 oil Substances 0.000 description 2
- 239000007800 oxidant agent Substances 0.000 description 2
- 230000035699 permeability Effects 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 229920003023 plastic Polymers 0.000 description 2
- 229920000642 polymer Polymers 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 229910001369 Brass Inorganic materials 0.000 description 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 229910000831 Steel Inorganic materials 0.000 description 1
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- 230000032683 aging Effects 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 125000003118 aryl group Chemical group 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000010951 brass Substances 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 238000010622 cold drawing Methods 0.000 description 1
- 238000009833 condensation Methods 0.000 description 1
- 230000005494 condensation Effects 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000009792 diffusion process Methods 0.000 description 1
- 239000011363 dried mixture Substances 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 229920003247 engineering thermoplastic Polymers 0.000 description 1
- 150000002148 esters Chemical class 0.000 description 1
- 239000000499 gel Substances 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- 239000001307 helium Substances 0.000 description 1
- 229910052734 helium Inorganic materials 0.000 description 1
- SWQJXJOGLNCZEY-UHFFFAOYSA-N helium atom Chemical compound [He] SWQJXJOGLNCZEY-UHFFFAOYSA-N 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000003507 refrigerant Substances 0.000 description 1
- 229920005989 resin Polymers 0.000 description 1
- 239000011347 resin Substances 0.000 description 1
- 239000003566 sealing material Substances 0.000 description 1
- 229920002379 silicone rubber Polymers 0.000 description 1
- 238000002791 soaking Methods 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 229920002725 thermoplastic elastomer Polymers 0.000 description 1
- 239000004636 vulcanized rubber Substances 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J151/00—Adhesives based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Adhesives based on derivatives of such polymers
- C09J151/003—Adhesives based on graft polymers in which the grafted component is obtained by reactions only involving carbon-to-carbon unsaturated bonds; Adhesives based on derivatives of such polymers grafted on to macromolecular compounds obtained by reactions only involving unsaturated carbon-to-carbon bonds
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
- C09J11/00—Features of adhesives not provided for in group C09J9/00, e.g. additives
- C09J11/02—Non-macromolecular additives
- C09J11/04—Non-macromolecular additives inorganic
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Carbon And Carbon Compounds (AREA)
Abstract
The invention belongs to the technical field of cryogenic pumps, and particularly relates to a preparation method of a low-temperature adhesive for a cryogenic pump activated carbon adsorption material.
Description
Technical Field
The invention belongs to the technical field of cryopumps, and particularly relates to a preparation method of low-temperature glue for a cryopump active carbon adsorption material.
Background
The cryopump is a vacuum pump that condenses and physically adsorbs gases using a low temperature surface song. Also known as condensate pumps and cryosorption pumps. At present, cryogenic pumping is increasingly used. The pumping with the cryopump is based on condensation of gases on cryogenic surfaces that are cooled to very low temperatures. Cryopumps differ from cold traps in the use of different refrigerants. The surface to be cooled to the liquid nitrogen (the boiling point of the liquid nitrogen is minus 196 ℃ C. at the standard pressure, and hydrogen or helium, which has the boiling points of minus 253 ℃ C. and minus 269 ℃ C. at the standard pressure, respectively.) the surface cooled to the liquid nitrogen temperature enables the gas (including most of the decomposition products of the oil diffusion pump) to condense extremely easily, can be regarded as a cryopump that needs to be assisted in its evacuation by an adsorbent material, and the adhesion of the adsorbent material to the panel is achieved by an adhesive, but the existing adhesive has poor low-temperature resistance and low adhesion strength, and activated carbon is one of the temperature adsorbent materials of the cryopump that is currently most widely used, and further, the cryopump has a characteristic that the vapor partial pressure strongly depends on the temperature. The temperature of the cooling surface is increased, the ultimate vacuum degree is deteriorated, the durability, the bonding performance and the low temperature resistance of the adhesive have great influence on the use performance and the service life of the panel and the low-temperature pump, and the technical personnel in the field need to develop a preparation method of the low-temperature adhesive for the activated carbon adsorption material of the low-temperature pump.
Aiming at the problems, the invention aims to provide a preparation method of a low-temperature adhesive for a low-temperature pump activated carbon adsorption material.
The invention is realized by the following technical scheme:
a preparation method of low-temperature glue for a low-temperature pump activated carbon adsorption material comprises the following steps: (1) mixing 3-5 parts by weight of natural flake graphite powder, 2-2.5 parts by weight of sodium nitrate and 100-115 parts by weight of 98% concentrated sulfuric acid, placing the mixture into a reaction kettle, stirring the mixture in an ice-water bath at the temperature of-1-2 ℃ to fully mix the mixture, weighing 14-15 parts by weight of potassium permanganate fine powder, slowly adding the potassium permanganate fine powder into the mixed solution for 0.5-1 hour, raising the temperature of the water bath to 10-15 ℃, continuously stirring the mixture for 1-2 hours, raising the temperature of the water bath to 20-35 ℃, continuously stirring the mixture for 20-30 minutes after the temperature is raised to the temperature, continuously and slowly adding 200-230 parts by weight of distilled water into the mixture by using a constant-pressure funnel, adding the distilled water bath for 30-60 minutes, raising the temperature of the water bath to 95-98 ℃, continuously reacting the reaction liquid for 10-15 minutes after the reaction is finished, adding 12-15 parts by weight of 30% hydrogen peroxide into the reaction kettle, uniformly stirring the mixture to make the solution turn into bright yellow, continuously stirring for 8-10 min, adding 130-140 parts of distilled water for dilution, standing for 1-2 h, removing supernatant, washing with deionized water for three times, dissolving in deionized water until the pH value is 7.0-7.2, pouring the obtained product, namely graphene oxide hydrosol, into a watch glass, stirring flatly, vacuumizing and drying at 60 ℃ in a vacuum drying oven, taking out after drying completely to obtain solid graphene oxide, preparing 8-10 parts of graphene oxide solution with the concentration of 1mg/mL, adjusting the pH value to 9-10 with 5% by mass of anhydrous sodium carbonate solution, carrying out ultrasonic treatment, adding 15-20 parts of 0.2mol/L sodium borohydride solution, washing with water to be neutral after reaction to obtain partially reduced graphene oxide solution, adding 1.9-2.1 parts of 4-aminobenzenesulfonic acid in parts by weight into 8-10 parts of 5% NaOH solution for dissolution, dissolving 0.6-0.8 part of sodium nitrite in 5-6 parts of deionized water, adding the sodium nitrite into a mixed solution of 4-aminobenzenesulfonic acid and NaOH, adding 2.8-3.1 parts of concentrated hydrochloric acid with the mass fraction of 36% and 8-10 parts of deionized water into the reaction solution under the condition of ice-water bath at the temperature of-1-2 ℃, reacting for 10-20 min, adding the reaction solution into a partially reduced graphene oxide solution for reaction at the temperature of 20-25 ℃, adding 4-5 parts of sodium hyposulfite into the reaction system after carrying out ultrasonic treatment on the reaction solution for 8-10 min, carrying out small stirring reaction at the temperature of 90-95 ℃ for 15-20 min, and washing to be neutral to obtain sulfonated graphene; (2) plasma-induced graft acrylic acid treatment of polychlorotrifluoroethylene powder: performing plasma treatment on polychlorotrifluoroethylene powder by adopting a ZYHD-1A plasma treatment instrument, placing the pretreated polychlorotrifluoroethylene powder in a reaction chamber between two electrodes in the reaction chamber, connecting one end of the reaction chamber with a vacuum pump, connecting the other end of the reaction chamber with an air inlet system, closing a reaction chamber cover plate and all vacuum valves, pressing a switch of a thermocouple vacuum gauge, measuring the vacuum degree, simultaneously observing a pointer of the vacuum gauge, pumping the vacuum degree to 0.8-1 Pa, slowly screwing off an adjusting valve on a rotor flow meter, adjusting the oxygen gas inlet amount of working gas, starting a high-frequency power supply when the air pressure in the reaction chamber is stabilized to 25-28 Pa, treating for 400-600 s under the power of 65W, closing a radio-frequency power supply firstly after the treatment is finished, then closing an air inlet gas circuit and the vacuum pump, taking out the polychlorotrifluoroethylene powder and placing the polychlorotrifluoroethylene powder in the air for 15-30 min; adding the plasma-treated polychlorotrifluoroethylene powder into an acrylic acid aqueous solution with the mass fraction of 8-10% in a fume hood, wherein the mass ratio of the polychlorotrifluoroethylene powder to the acrylic acid aqueous solution is (4-5.5): 100, introducing nitrogen as protective gas, and magnetically stirring at 65-70 ℃ to obtain a suspension; stirring and reacting for 24-30 h, then carrying out centrifugal separation on the suspension, wherein the rotating speed of a centrifugal machine is 3500-4000 r/min, the centrifugal time is 8-10 min, repeatedly cleaning the suspension by using deionized water to remove acrylic monomers on the surface of the polychlorotrifluoroethylene powder, and then placing the suspension in an oven to dry for 12h at 65-70 ℃ to obtain the polychlorotrifluoroethylene powder subjected to acrylic acid grafting treatment; (3) sulfonated graphene prepared in the step (1), acrylic acid grafted polychlorotrifluoroethylene powder prepared in the step (2) and a toughening agent; the dosage of the raw materials has the following mass proportion relation: sulfonated graphene, acrylic acid grafted polychlorotrifluoroethylene powder and a toughening agent are 15-20: 80-95: 20-40; uniformly mixing the sulfonated graphene prepared in the step (1), a toughening agent and acrylic acid grafted polychlorotrifluoroethylene powder, and pouring the mixture into a mould pressing die at 170-190 ℃ for pressing and forming, wherein the pressing pressure is 30-45 Mpa, and the pressing time is 10-20 min; and after the mixed powder is pressed, taking the mixed powder out of a cold mould pressing die, trimming and removing burrs of the mixed powder to enable the mixed powder to be smooth and flat to obtain a sulfonated graphene-polytrifluorochloroethylene composite material sheet, placing the sulfonated graphene-polytrifluorochloroethylene composite material sheet in a low-temperature lining plate to carry out heat treatment in a temperature-controlled electric furnace, raising the temperature of the electric furnace from room temperature to 225 ℃ at the heating rate of 5 ℃/min, carrying out heat preservation for 30min at 225 ℃, then cooling the temperature of the electric furnace from 225 ℃ to 200 ℃, carrying out the cooling process for 2-3 min, carrying out heat preservation for 20-35 min at 200 ℃, finally turning off a power supply of the electric furnace, naturally cooling the temperature of the electric furnace from 200 ℃ to room temperature, and taking out the heat-treated sheet after the electric furnace is naturally cooled to the room temperature to obtain the low-temperature adhesive for the low-temperature pump activated carbon adsorption material.
Further, the toughening agent is one of vinylidene fluoride-chlorotrifluoroethylene copolymer and chlorotrifluoroethylene-ethylene copolymer.
Further, the polychlorotrifluoroethylene is powder with an average particle size of 300-500 μm.
The invention has the beneficial effects that:
the preparation method of the low-temperature adhesive for the low-temperature pump activated carbon adsorption material disclosed by the invention is prepared from polychlorotrifluoroethylene, sulfonated graphene and a toughening agent, and has the advantages of good cold flow resistance, wear resistance, dimensional stability, good processability and good adhesion with metal. The PCTFE has particularly outstanding low temperature resistance, does not crack or creep in liquid nitrogen, liquid oxygen and liquefied natural gas, can be used at a temperature close to zero (-273 ℃), and can resist almost all chemical substances and oxidants under certain conditions. The PCTFE has the lowest water vapor permeability, can not permeate any gas, is a good barrier polymer, has excellent optical performance and good weather resistance, can be uniformly coated on the surface of a metal low-temperature bottom plate such as steel, brass, aluminum, zinc and the like, is suitable for being used as a low-temperature adsorption material such as activated carbon and the like to adhere and not absorb water, and can resist various acids, alkalis, oils and organic solvents. It has the advantages of non-combustibility, good mechanical, electrical insulation, aging resistance, irradiation resistance, good dimensional stability, good adhesion with metal, and welding.
Compared with the prior art, the invention has the following advantages:
the low-temperature adhesive for the low-temperature pump activated carbon adsorption material disclosed by the invention can bear extreme conditions, can tolerate extreme temperature and temperature change thereof, does not crack or creep in liquid nitrogen, liquid oxygen and liquefied natural gas, has good mechanical property and chemical property within a long-term use temperature range of-240-125 ℃, so that the low-temperature adhesive becomes an excellent engineering thermoplastic plastic, can tolerate almost all chemical substances and oxidants, slightly swells in a halogen-containing ether, ester and aromatic solution, has the lowest water-vapor permeability in all plastics, is impermeable to any gas, is not combusted, is a good barrier polymer, and does not influence low-temperature gas adsorption.
Detailed Description
The invention is illustrated by the following specific examples, which are not intended to be limiting.
Example 1
(1) Mixing 5 parts by weight of natural flake graphite powder, 2.5 parts by weight of sodium nitrate and 115 parts by weight of 98% concentrated sulfuric acid, placing the mixture in a reaction kettle, stirring the mixture in an ice-water bath at the temperature of 2 ℃ to fully mix the mixture, weighing 15 parts by weight of potassium permanganate fine powder, slowly adding the potassium permanganate fine powder into the mixed solution for 1 hour, raising the temperature of the water bath to 15 ℃, continuously stirring the mixture for 2 hours, raising the temperature of a water bath kettle to 35 ℃, continuously stirring the mixture for 30 minutes when the temperature is raised to the temperature, continuously and slowly adding 230 parts by weight of distilled water by using a constant-pressure funnel, adding the distilled water for 60 minutes, raising the temperature of the water bath kettle to 98 ℃, continuously reacting the reaction liquid for 15 minutes, after the reaction is finished, adding 15 parts by weight of 30% hydrogen peroxide into the reaction kettle, uniformly stirring the hydrogen peroxide to change the solution into bright yellow, continuously stirring the solution for 10 minutes, adding 140 parts by weight of distilled water for dilution, standing the solution for 2 hours, removing supernatant, washing the mixture by using deionized water for three times, then dissolving the graphene oxide into deionized water until the pH value is 7.2, pouring the hydrosol into a watch glass, stirring the mixture evenly, vacuumizing and drying the mixture in a vacuum drying oven at 60 ℃, taking the dried mixture out after complete drying to prepare solid graphene oxide, preparing 10 parts of graphene oxide solution with the concentration of 1mg/mL, adjusting the pH value to 10 by using anhydrous sodium carbonate solution with the mass fraction of 5%, carrying out ultrasonic treatment, adding 20 parts of 0.2mol/L sodium borohydride solution, washing the mixture with water to be neutral after reaction to obtain partially reduced graphene oxide solution, adding 2.1 parts of 4-aminobenzenesulfonic acid in parts by weight into 10 parts of 5% NaOH solution to dissolve the 4-aminobenzenesulfonic acid, dissolving 0.8 part of sodium nitrite into 6 parts of deionized water, adding the sodium nitrite into a mixed solution of the 4-aminobenzenesulfonic acid and NaOH, and carrying out ice-water bath at the temperature of 2 ℃, adding 3.1 parts of concentrated hydrochloric acid with the mass fraction of 36% and 10 parts of deionized water into the reaction solution, reacting for 20min, adding the reaction solution into a partially reduced graphene oxide solution, reacting at 25 ℃, adding 5 parts of sodium hyposulfite into a reaction system after carrying out ultrasonic treatment on the reaction solution for 10min, carrying out small stirring reaction at 90-95 ℃ for 20min, and washing to be neutral to obtain sulfonated graphene; (2) plasma-induced graft acrylic acid treatment of polychlorotrifluoroethylene powder: adopting a ZYHD-1A plasma treatment instrument to carry out plasma treatment on polychlorotrifluoroethylene powder, placing the pretreated polychlorotrifluoroethylene powder in a reaction chamber between two electrodes in the reaction chamber, connecting one end of the reaction chamber with a vacuum pump, connecting the other end of the reaction chamber with an air inlet system, closing a reaction chamber cover plate and all vacuum valves, pressing a switch of a thermocouple vacuum gauge, measuring the vacuum degree, simultaneously observing a pointer of the vacuum gauge, pumping the vacuum degree to 1Pa, slowly screwing off an adjusting valve on a rotor flow meter, adjusting the oxygen gas inlet amount of working gas, starting a high-frequency power supply when the air pressure in the reaction chamber is stabilized to 28Pa, treating for 600s under the power of 65W, firstly closing the radio-frequency power supply after the treatment is finished, then closing an air inlet gas circuit and the vacuum pump, taking out the polychlorotrifluoroethylene powder and placing the polychlorotrifluoroethylene powder in the air for 30 min; adding the plasma-treated polychlorotrifluoroethylene powder into an acrylic acid aqueous solution with the mass fraction of 10% in a fume hood, wherein the mass ratio of the polychlorotrifluoroethylene powder to the acrylic acid aqueous solution is 5.5: 100, introducing nitrogen as protective gas, and magnetically stirring at 70 ℃ to obtain a suspension; stirring and reacting for 30h, then carrying out centrifugal separation on the suspension, wherein the rotating speed of a centrifugal machine is 4000r/min, the centrifugal time is 10min, repeatedly cleaning the suspension by using deionized water to remove acrylic monomers on the surface of the polychlorotrifluoroethylene powder, and then drying the suspension in a drying oven at 70 ℃ for 12h to obtain the polychlorotrifluoroethylene powder subjected to acrylic acid grafting treatment; (3) sulfonated graphene prepared in the step (1), acrylic acid grafted polychlorotrifluoroethylene powder prepared in the step (2) and a toughening agent; the dosage of the raw materials has the following mass proportion relation: sulfonated graphene, acrylic acid grafted polychlorotrifluoroethylene powder and a toughening agent are 20: 95: 40; uniformly mixing the sulfonated graphene prepared in the step (1), a toughening agent and acrylic acid grafted polychlorotrifluoroethylene powder, and pouring the mixture into a 190 ℃ mould pressing die for pressing and forming, wherein the pressing pressure is 45Mpa, and the pressing time is 20 min; after the mixed powder is pressed, taking out the mixed powder from a cold mould pressing die, trimming and deburring the mixed powder to make the mixed powder smooth and flat to prepare a sulfonated graphene-polytrifluorochloroethylene composite material sheet, placing the sulfonated graphene-polytrifluorochloroethylene composite material sheet in a low-temperature lining plate to carry out heat treatment in a temperature-controlled electric furnace, raising the temperature of the electric furnace from room temperature to 225 ℃ at the heating rate of 5 ℃/min, preserving the heat at 225 ℃ for 30min, then cooling the electric furnace from 225 ℃ to 200 ℃ for 2-3 min, preserving the heat of the electric furnace at 200 ℃ for 35min, finally turning off a power supply of the electric furnace, naturally cooling the temperature of the electric furnace from 200 ℃ to room temperature, taking out the heat-treated sheet after the electric furnace is naturally cooled to the room temperature, thus obtaining the low-temperature adhesive for the low-temperature pump activated carbon adsorption material, wherein the toughening agent is a vinylidene fluoride-chlorotrifluoroethylene copolymer, the polychlorotrifluoroethylene is powder with an average particle size of 500 μm.
Example 2
(1) Mixing 3 parts by weight of natural flake graphite powder, 2 parts by weight of sodium nitrate and 100 parts by weight of 98% concentrated sulfuric acid, placing the mixture into a reaction kettle, stirring the mixture in an ice-water bath at the temperature of-1 ℃ to fully mix the mixture, weighing 14 parts by weight of potassium permanganate fine powder, slowly adding the potassium permanganate fine powder into the mixed solution for 0.5 hour, raising the temperature of the water bath to 10 ℃, continuously stirring the mixture for 1 hour, raising the temperature of a water bath kettle to 20 ℃, continuously stirring the mixture for 20 minutes when the temperature is raised to the temperature, continuously and slowly adding 200 parts by weight of distilled water into the mixture by using a constant pressure funnel, adding the distilled water for 30 minutes, raising the temperature of the water bath kettle to 95 ℃, continuously reacting the reaction liquid for 10 minutes, after the reaction is finished, adding 12 parts by weight of 30% hydrogen peroxide into the reaction kettle, uniformly stirring the hydrogen peroxide to change the solution into bright yellow, continuously stirring the solution for 8 minutes, adding 130 parts by weight of distilled water for dilution, standing the mixture for 1 hour, removing a supernatant, washing with deionized water for three times, dissolving in deionized water until the pH value is 7.0, obtaining a product which is graphene oxide hydrosol, pouring the hydrosol into a watch glass, stirring and leveling, vacuumizing and drying in a vacuum drying oven at 60 ℃, taking out after complete drying to obtain solid graphene oxide, preparing 8 parts of graphene oxide solution with the concentration of 1mg/mL, adjusting the pH value to 9 with 5% anhydrous sodium carbonate solution by mass fraction, carrying out ultrasonic treatment, adding 15 parts of 0.2mol/L sodium borohydride solution, washing with water to be neutral after reaction to obtain partially reduced graphene oxide solution, adding 2.1 parts of 4-aminobenzenesulfonic acid in parts by weight into 8 parts of 5% NaOH solution for dissolution, dissolving 0.6 part of sodium nitrite in 5 parts of deionized water, adding the mixture into the mixture of 4-aminobenzenesulfonic acid and NaOH, under the condition of ice-water bath at the temperature of 2 ℃, adding 2.8 parts of concentrated hydrochloric acid with the mass fraction of 36% and 10 parts of deionized water into the reaction solution, reacting for 10min, adding the reaction solution into a partially reduced graphene oxide solution, reacting at the temperature of 20 ℃, adding 5 parts of sodium hyposulfite into a reaction system after carrying out ultrasonic treatment on the reaction solution for 8min, carrying out small stirring reaction at the temperature of 90 ℃ for 15min, and washing to be neutral to obtain sulfonated graphene; (2) plasma-induced graft acrylic acid treatment of polychlorotrifluoroethylene powder: adopting a ZYHD-1A plasma treatment instrument to carry out plasma treatment on polychlorotrifluoroethylene powder, placing the pretreated polychlorotrifluoroethylene powder in a reaction chamber between two electrodes in the reaction chamber, connecting one end of the reaction chamber with a vacuum pump, connecting the other end of the reaction chamber with an air inlet system, closing a reaction chamber cover plate and all vacuum valves, pressing a switch of a thermocouple vacuum gauge, measuring the vacuum degree, simultaneously observing a pointer of the vacuum gauge, pumping the vacuum degree to 0.8Pa, slowly screwing off an adjusting valve on a rotor flow meter, adjusting the oxygen gas inlet amount of working gas, starting a high-frequency power supply when the air pressure in the reaction chamber is stabilized to 25Pa, treating for 400s under the power of 65W, firstly closing the radio-frequency power supply after the treatment is finished, then closing an air inlet gas circuit and the vacuum pump, taking out the polychlorotrifluoroethylene powder and placing the polychlorotrifluoroethylene powder in the air for 15 min; adding the plasma-treated polychlorotrifluoroethylene powder into an acrylic acid aqueous solution with the mass fraction of 8% in a fume hood, wherein the mass ratio of the polychlorotrifluoroethylene powder to the acrylic acid aqueous solution is 4: 100, introducing nitrogen as protective gas, and magnetically stirring at 65 ℃ to obtain a suspension; stirring for 24 hours, carrying out centrifugal separation on the suspension, wherein the rotating speed of a centrifugal machine is 3500r/min, the centrifugal time is 8min, repeatedly cleaning the suspension by using deionized water to remove acrylic monomers on the surface of the polychlorotrifluoroethylene powder, and then drying the suspension in an oven at 65 ℃ for 12 hours to obtain the polychlorotrifluoroethylene powder subjected to acrylic acid grafting treatment; (3) sulfonated graphene prepared in the step (1), acrylic acid grafted polychlorotrifluoroethylene powder prepared in the step (2) and a toughening agent; the dosage of the raw materials has the following mass proportion relation: sulfonated graphene, acrylic acid grafted polychlorotrifluoroethylene powder and a toughening agent are 15: 80: 20; uniformly mixing the sulfonated graphene prepared in the step (1), a toughening agent and acrylic acid grafted polychlorotrifluoroethylene powder, and pouring the mixture into a mould pressing die at 170 ℃ for pressing and forming, wherein the pressing pressure is 30Mpa, and the pressing time is 10 min; after the mixed powder is pressed, taking out the mixed powder from a cold mould pressing die, trimming and removing burrs of the mixed powder to make the mixed powder smooth and flat to prepare a sulfonated graphene-polytrifluorochloroethylene composite material sheet, placing the sulfonated graphene-polytrifluorochloroethylene composite material sheet in a low-temperature lining plate to carry out heat treatment in a temperature-controlled electric furnace, raising the temperature of the electric furnace from room temperature to 225 ℃ at the heating rate of 5 ℃/min, preserving the heat at 225 ℃ for 30min, then cooling the temperature of the electric furnace from 225 ℃ to 200 ℃ for 2min, preserving the heat of the electric furnace at 200 ℃ for 20min, finally turning off a power supply of the electric furnace, naturally cooling the temperature of the electric furnace from 200 ℃ to room temperature, taking out the heat-treated sheet after the temperature of the electric furnace is naturally cooled to the room temperature, and obtaining the low-temperature adhesive for the low-temperature pump activated carbon adsorption material, wherein the toughening agent is a chlorotrifluoroethylene-ethylene copolymer, the polychlorotrifluoroethylene is a powder having an average particle diameter of 300.
Comparative example 1
This comparative example compares to example 2 in step (3) the toughening agent is omitted except that the process steps are otherwise the same.
Comparative example 2
This comparative example compares to example 2 in step (3), the sulfonated graphene is omitted, except that the process steps are the same.
The performance of the low-temperature glue for the activated carbon adsorbing materials of the low-temperature pumps of the examples 1-2 and the comparative examples 1-2 is tested, and the test results are shown in Table 1
TABLE 1 comparative results of performance tests of low-temperature gels for cryopumping activated carbon adsorbent materials of examples and comparative examples
| Example 1 | Example 2 | Comparative example 1 | Comparative example 2 | |
| Low temperature embrittlement temperature DEG C | -108.3 | -105.2 | -100.1 | -98.5 |
| Adhesion after ultraviolet irradiation | Without destruction | Without destruction | Without destruction | Without destruction |
| Fixed-elongation cohesiveness after immersion in water | Without destruction | Without destruction | Without destruction | Without destruction |
| Elastic recovery rate% | 80 | 80 | 80 | 80 |
| Definite elongation adhesion | Without destruction | Without destruction | Without destruction | Without destruction |
| Cold drawing after irradiation-hot pressing after adhesion | Without destruction | Without destruction | Without destruction | Without destruction |
| Tensile strength MPa | 34.3 | 32.9 | 31.4 | 30.5 |
| Elongation at break% | 67.5 | 68.6 | 65.4 | 69.4 |
| Strength loss temperature deg.C | 278 | 270 | 275 | 265 |
| Impact toughness KJ/m2 | 13.5 | 13.2 | 14.8 | 12.5 |
| Thermal stability% | 0.12 | 0.12 | 0.14 | 0.13 |
| Hardness Shore A | 85.4 | 82.8 | 82.4 | 80.2 |
Note: after ultraviolet irradiation, the cohesive ultraviolet irradiation box is required to meet the regulation of 5.12.1 in JC/T485-1992, continuous illumination is carried out for 300 hours under the condition of no water immersion, and if a test piece is damaged, another group of spare test pieces are taken for re-examination. The test method of the test piece is the same; the definite elongation caking property after soaking is tested according to GB/T13477.11-2002; the performance at ultralow temperature is measured according to the method specified by the GJB2157-1994 ultralow temperature resistant silicon rubber material specification; test method for adhesion after cold drawing-hot pressing after irradiation GB/T13477.13-2002 building sealing materials part 13: measuring the cohesiveness after cold drawing-hot pressing; measured according to the method specified in the measurement of the hardness of the HG/T3846-2008 hard rubber; the tensile strength is measured according to the method specified for measuring the tensile strength and the elongation at break of the HG/T3849-2008 hard rubber; the elongation at break is measured according to the method specified for measuring the tensile strength and the elongation at break of the HG/T3849-2008 hard rubber; the tear strength is determined according to the method specified in GB/T529-2008 for determination of the tear strength of vulcanized rubber or thermoplastic rubber; HG 2167-1991 polychlorotrifluoroethylene resin.
Claims (3)
1. A preparation method of low-temperature glue for a low-temperature pump activated carbon adsorption material is characterized by comprising the following steps: (1) mixing 3-5 parts by weight of natural flake graphite powder, 2-2.5 parts by weight of sodium nitrate and 100-115 parts by weight of 98% concentrated sulfuric acid, placing the mixture into a reaction kettle, stirring the mixture in an ice-water bath at the temperature of-1-2 ℃ to fully mix the mixture, weighing 14-15 parts by weight of potassium permanganate fine powder, slowly adding the potassium permanganate fine powder into the mixed solution for 0.5-1 hour, raising the temperature of the water bath to 10-15 ℃, continuously stirring the mixture for 1-2 hours, raising the temperature of the water bath to 20-35 ℃, continuously stirring the mixture for 20-30 minutes after the temperature is raised to the temperature, continuously and slowly adding 200-230 parts by weight of distilled water into the mixture by using a constant-pressure funnel, adding the distilled water bath for 30-60 minutes, raising the temperature of the water bath to 95-98 ℃, continuously reacting the reaction liquid for 10-15 minutes after the reaction is finished, adding 12-15 parts by weight of 30% hydrogen peroxide into the reaction kettle, uniformly stirring the mixture to make the solution turn into bright yellow, continuously stirring for 8-10 min, adding 130-140 parts of distilled water for dilution, standing for 1-2 h, removing supernatant, washing with deionized water for three times, dissolving in deionized water until the pH value is 7.0-7.2, pouring the obtained product, namely graphene oxide hydrosol, into a watch glass, stirring flatly, vacuumizing and drying at 60 ℃ in a vacuum drying oven, taking out after drying completely to obtain solid graphene oxide, preparing 8-10 parts of graphene oxide solution with the concentration of 1mg/mL, adjusting the pH value to 9-10 with 5% by mass of anhydrous sodium carbonate solution, carrying out ultrasonic treatment, adding 15-20 parts of 0.2mol/L sodium borohydride solution, washing with water to be neutral after reaction to obtain partially reduced graphene oxide solution, adding 1.9-2.1 parts of 4-aminobenzenesulfonic acid in parts by weight into 8-10 parts of 5% NaOH solution for dissolution, dissolving 0.6-0.8 part of sodium nitrite in 5-6 parts of deionized water, adding the sodium nitrite into a mixed solution of 4-aminobenzenesulfonic acid and NaOH, adding 2.8-3.1 parts of concentrated hydrochloric acid with the mass fraction of 36% and 8-10 parts of deionized water into the reaction solution under the condition of ice-water bath at the temperature of-1-2 ℃, reacting for 10-20 min, adding the reaction solution into a partially reduced graphene oxide solution for reaction at the temperature of 20-25 ℃, adding 4-5 parts of sodium hyposulfite into the reaction system after carrying out ultrasonic treatment on the reaction solution for 8-10 min, carrying out small stirring reaction at the temperature of 90-95 ℃ for 15-20 min, and washing to be neutral to obtain sulfonated graphene; (2) plasma-induced graft acrylic acid treatment of polychlorotrifluoroethylene powder: performing plasma treatment on polychlorotrifluoroethylene powder by adopting a ZYHD-1A plasma treatment instrument, placing the pretreated polychlorotrifluoroethylene powder in a reaction chamber between two electrodes in the reaction chamber, connecting one end of the reaction chamber with a vacuum pump, connecting the other end of the reaction chamber with an air inlet system, closing a reaction chamber cover plate and all vacuum valves, pressing a switch of a thermocouple vacuum gauge, measuring the vacuum degree, simultaneously observing a pointer of the vacuum gauge, pumping the vacuum degree to 0.8-1 Pa, slowly screwing off an adjusting valve on a rotor flow meter, adjusting the oxygen gas inlet amount of working gas, starting a high-frequency power supply when the air pressure in the reaction chamber is stabilized to 25-28 Pa, treating for 400-600 s under the power of 65W, closing a radio-frequency power supply firstly after the treatment is finished, then closing an air inlet gas circuit and the vacuum pump, taking out the polychlorotrifluoroethylene powder and placing the polychlorotrifluoroethylene powder in the air for 15-30 min; adding the plasma-treated polychlorotrifluoroethylene powder into an acrylic acid aqueous solution with the mass fraction of 8-10% in a fume hood, wherein the mass ratio of the polychlorotrifluoroethylene powder to the acrylic acid aqueous solution is (4-5.5): 100, introducing nitrogen as protective gas, and magnetically stirring at 65-70 ℃ to obtain a suspension; stirring and reacting for 24-30 h, then carrying out centrifugal separation on the suspension, wherein the rotating speed of a centrifugal machine is 3500-4000 r/min, the centrifugal time is 8-10 min, repeatedly cleaning the suspension by using deionized water to remove acrylic monomers on the surface of the polychlorotrifluoroethylene powder, and then placing the suspension in an oven to dry for 12h at 65-70 ℃ to obtain the polychlorotrifluoroethylene powder subjected to acrylic acid grafting treatment; (3) sulfonated graphene prepared in the step (1), acrylic acid grafted polychlorotrifluoroethylene powder prepared in the step (2) and a toughening agent; the dosage of the raw materials has the following mass proportion relation: sulfonated graphene, acrylic acid grafted polychlorotrifluoroethylene powder and a toughening agent are 15-20: 80-95: 20-40; uniformly mixing the sulfonated graphene prepared in the step (1), a toughening agent and acrylic acid grafted polychlorotrifluoroethylene powder, and pouring the mixture into a mould pressing die at 170-190 ℃ for pressing and forming, wherein the pressing pressure is 30-45 Mpa, and the pressing time is 10-20 min; and after the mixed powder is pressed, taking the mixed powder out of a cold mould pressing die, trimming and removing burrs of the mixed powder to enable the mixed powder to be smooth and flat to obtain a sulfonated graphene-polytrifluorochloroethylene composite material sheet, placing the sulfonated graphene-polytrifluorochloroethylene composite material sheet in a low-temperature lining plate to carry out heat treatment in a temperature-controlled electric furnace, raising the temperature of the electric furnace from room temperature to 225 ℃ at the heating rate of 5 ℃/min, carrying out heat preservation for 30min at 225 ℃, then cooling the temperature of the electric furnace from 225 ℃ to 200 ℃, carrying out the cooling process for 2-3 min, carrying out heat preservation for 20-35 min at 200 ℃, finally turning off a power supply of the electric furnace, naturally cooling the temperature of the electric furnace from 200 ℃ to room temperature, and taking out the heat-treated sheet after the electric furnace is naturally cooled to the room temperature to obtain the low-temperature adhesive for the low-temperature pump activated carbon adsorption material.
2. The method for preparing the low-temperature adhesive for the activated carbon adsorption material of the cryopump of claim 1, wherein the toughening agent is one of vinylidene fluoride-chlorotrifluoroethylene copolymer and chlorotrifluoroethylene-ethylene copolymer.
3. The method for preparing the low-temperature adhesive for the activated carbon adsorption material of the cryopump as claimed in claim 1, wherein the polychlorotrifluoroethylene is powder with an average particle size of 300-500 μm.
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