CN115216055A - Preparation method of perfume volatilization medium graphite core rod - Google Patents
Preparation method of perfume volatilization medium graphite core rod Download PDFInfo
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- CN115216055A CN115216055A CN202210723883.3A CN202210723883A CN115216055A CN 115216055 A CN115216055 A CN 115216055A CN 202210723883 A CN202210723883 A CN 202210723883A CN 115216055 A CN115216055 A CN 115216055A
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- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 title claims abstract description 129
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 239000002304 perfume Substances 0.000 title claims abstract description 22
- 229910021389 graphene Inorganic materials 0.000 claims description 86
- 239000002131 composite material Substances 0.000 claims description 35
- 229920005575 poly(amic acid) Polymers 0.000 claims description 30
- 239000006185 dispersion Substances 0.000 claims description 21
- 239000007788 liquid Substances 0.000 claims description 21
- 239000004642 Polyimide Substances 0.000 claims description 20
- RRAFCDWBNXTKKO-UHFFFAOYSA-N eugenol Chemical compound COC1=CC(CC=C)=CC=C1O RRAFCDWBNXTKKO-UHFFFAOYSA-N 0.000 claims description 20
- 229920001721 polyimide Polymers 0.000 claims description 20
- 238000003756 stirring Methods 0.000 claims description 15
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 14
- 238000010438 heat treatment Methods 0.000 claims description 14
- 239000002904 solvent Substances 0.000 claims description 14
- 239000011521 glass Substances 0.000 claims description 13
- -1 dimethyl silicon diethylamine Chemical compound 0.000 claims description 12
- 238000009210 therapy by ultrasound Methods 0.000 claims description 12
- HLBLWEWZXPIGSM-UHFFFAOYSA-N 4-Aminophenyl ether Chemical compound C1=CC(N)=CC=C1OC1=CC=C(N)C=C1 HLBLWEWZXPIGSM-UHFFFAOYSA-N 0.000 claims description 11
- 239000004698 Polyethylene Substances 0.000 claims description 11
- 239000002253 acid Substances 0.000 claims description 11
- 238000007710 freezing Methods 0.000 claims description 11
- 230000008014 freezing Effects 0.000 claims description 11
- 150000004687 hexahydrates Chemical class 0.000 claims description 11
- 239000000203 mixture Substances 0.000 claims description 11
- 229920000573 polyethylene Polymers 0.000 claims description 11
- 238000012545 processing Methods 0.000 claims description 11
- 239000002356 single layer Substances 0.000 claims description 11
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- KIFDSGGWDIVQGN-UHFFFAOYSA-N 4-[9-(4-aminophenyl)fluoren-9-yl]aniline Chemical compound C1=CC(N)=CC=C1C1(C=2C=CC(N)=CC=2)C2=CC=CC=C2C2=CC=CC=C21 KIFDSGGWDIVQGN-UHFFFAOYSA-N 0.000 claims description 10
- NPBVQXIMTZKSBA-UHFFFAOYSA-N Chavibetol Natural products COC1=CC=C(CC=C)C=C1O NPBVQXIMTZKSBA-UHFFFAOYSA-N 0.000 claims description 10
- 239000005770 Eugenol Substances 0.000 claims description 10
- ZWNPUELCBZVMDA-CMDGGOBGSA-N Methyl 2-nonenoate Chemical compound CCCCCC\C=C\C(=O)OC ZWNPUELCBZVMDA-CMDGGOBGSA-N 0.000 claims description 10
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 10
- UVMRYBDEERADNV-UHFFFAOYSA-N Pseudoeugenol Natural products COC1=CC(C(C)=C)=CC=C1O UVMRYBDEERADNV-UHFFFAOYSA-N 0.000 claims description 10
- GTDPSWPPOUPBNX-UHFFFAOYSA-N ac1mqpva Chemical compound CC12C(=O)OC(=O)C1(C)C1(C)C2(C)C(=O)OC1=O GTDPSWPPOUPBNX-UHFFFAOYSA-N 0.000 claims description 10
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- 238000004821 distillation Methods 0.000 claims description 10
- 229960002217 eugenol Drugs 0.000 claims description 10
- 238000002156 mixing Methods 0.000 claims description 10
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 10
- 238000004108 freeze drying Methods 0.000 claims description 9
- 239000002243 precursor Substances 0.000 claims description 9
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 7
- 239000003054 catalyst Substances 0.000 claims description 4
- 239000002270 dispersing agent Substances 0.000 claims description 4
- ZFPGARUNNKGOBB-UHFFFAOYSA-N 1-Ethyl-2-pyrrolidinone Chemical compound CCN1CCCC1=O ZFPGARUNNKGOBB-UHFFFAOYSA-N 0.000 claims description 3
- 229920000587 hyperbranched polymer Polymers 0.000 claims description 3
- 229910052757 nitrogen Inorganic materials 0.000 claims description 3
- 239000003921 oil Substances 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 8
- 238000000034 method Methods 0.000 description 15
- ADTGAVILDBXARD-UHFFFAOYSA-N diethylamino(dimethyl)silicon Chemical compound CCN(CC)[Si](C)C ADTGAVILDBXARD-UHFFFAOYSA-N 0.000 description 9
- 229910001873 dinitrogen Inorganic materials 0.000 description 8
- 239000012530 fluid Substances 0.000 description 7
- 230000008719 thickening Effects 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 4
- 239000007789 gas Substances 0.000 description 4
- 238000001179 sorption measurement Methods 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- 239000000047 product Substances 0.000 description 3
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- NDJKXXJCMXVBJW-UHFFFAOYSA-N heptadecane Chemical compound CCCCCCCCCCCCCCCCC NDJKXXJCMXVBJW-UHFFFAOYSA-N 0.000 description 2
- 239000010410 layer Substances 0.000 description 2
- MBHINSULENHCMF-UHFFFAOYSA-N n,n-dimethylpropanamide Chemical compound CCC(=O)N(C)C MBHINSULENHCMF-UHFFFAOYSA-N 0.000 description 2
- 230000001681 protective effect Effects 0.000 description 2
- 235000012239 silicon dioxide Nutrition 0.000 description 2
- 208000005156 Dehydration Diseases 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000012159 carrier gas Substances 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 229910052681 coesite Inorganic materials 0.000 description 1
- 239000013065 commercial product Substances 0.000 description 1
- 229910052906 cristobalite Inorganic materials 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001962 electrophoresis Methods 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 230000009969 flowable effect Effects 0.000 description 1
- 229910002804 graphite Inorganic materials 0.000 description 1
- 239000010439 graphite Substances 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
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 238000001819 mass spectrum Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 229910052759 nickel Inorganic materials 0.000 description 1
- 239000003960 organic solvent Substances 0.000 description 1
- 239000012466 permeate Substances 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 238000004729 solvothermal method Methods 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 229910052682 stishovite Inorganic materials 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
- 229910052905 tridymite Inorganic materials 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J9/00—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof
- C08J9/28—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum
- C08J9/286—Working-up of macromolecular substances to porous or cellular articles or materials; After-treatment thereof by elimination of a liquid phase from a macromolecular composition or article, e.g. drying of coagulum the liquid phase being a solvent for the monomers but not for the resulting macromolecular composition, i.e. macroporous or macroreticular polymers
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- A61L9/00—Disinfection, sterilisation or deodorisation of air
- A61L9/015—Disinfection, sterilisation or deodorisation of air using gaseous or vaporous substances, e.g. ozone
- A61L9/04—Disinfection, sterilisation or deodorisation of air using gaseous or vaporous substances, e.g. ozone using substances evaporated in the air without heating
- A61L9/12—Apparatus, e.g. holders, therefor
- A61L9/127—Apparatus, e.g. holders, therefor comprising a wick
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/20—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising free carbon; comprising carbon obtained by carbonising processes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
- B01J20/262—Synthetic macromolecular compounds obtained otherwise than by reactions only involving carbon to carbon unsaturated bonds, e.g. obtained by polycondensation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/28—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties
- B01J20/28014—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof characterised by their form or physical properties characterised by their form
- B01J20/28042—Shaped bodies; Monolithic structures
- B01J20/28045—Honeycomb or cellular structures; Solid foams or sponges
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/194—After-treatment
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- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B32/00—Carbon; Compounds thereof
- C01B32/15—Nano-sized carbon materials
- C01B32/182—Graphene
- C01B32/198—Graphene oxide
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
- C08G73/1003—Preparatory processes
- C08G73/1007—Preparatory processes from tetracarboxylic acids or derivatives and diamines
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- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/06—Polycondensates having nitrogen-containing heterocyclic rings in the main chain of the macromolecule
- C08G73/10—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
- C08G73/1075—Partially aromatic polyimides
- C08G73/1078—Partially aromatic polyimides wholly aromatic in the diamino moiety
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- C08J2379/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing nitrogen with or without oxygen, or carbon only, not provided for in groups C08J2361/00 - C08J2377/00
- C08J2379/04—Polycondensates having nitrogen-containing heterocyclic rings in the main chain; Polyhydrazides; Polyamide acids or similar polyimide precursors
- C08J2379/08—Polyimides; Polyester-imides; Polyamide-imides; Polyamide acids or similar polyimide precursors
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Abstract
The invention relates to the field of perfume volatile materials, in particular to a preparation method of a perfume volatile medium graphite core rod.
Description
Technical Field
The invention relates to the field of perfume volatile materials, in particular to a preparation method of a perfume volatile medium graphite core rod.
Background
Due to the excellent performance, hydrophobic and oleophilic characteristics and high specific surface area of graphene, graphene becomes a research hotspot of high-performance oil absorption materials. The graphene has high elasticity and high strength, so that the graphene sponge with a low-density high-elasticity three-dimensional structure can be prepared. The graphene sponge is a three-dimensional reticular porous material formed by stacking graphene sheets, and has higher adsorption capacity on oil products and organic solvents due to the fact that the graphene sponge has more pore diameters and larger specific surface area inside the graphene sponge.
However, the current graphene sponge can only select a certain specific treatment method. The foamed nickel supported three-dimensional graphene is sold as a commodity material, but most of the synthetic methods are chemical vapor deposition, and the price is higher. In addition, the preparation methods such as water/solvothermal method often require harsh experimental conditions such as high temperature or high pressure.
CN110655072A provides a shear thickening fluid composite graphene sponge protective material and a preparation method thereof, wherein the shear thickening fluid composite graphene sponge protective material comprises graphene sponge and a shear thickening fluid, the shear thickening fluid permeates into the graphene sponge, and the shear thickening fluid comprises SiO2. By adopting the technical scheme, the graphene sponge with soft mechanical property and the flowable shear thickening fluid are combined to obtain the novel shear thickening fluid composite graphene sponge.
CN201410032234.4 applies for a method for preparing graphene sponge based on traditional sponge as a template, and the invention relates to a method for preparing graphene sponge. The invention aims to solve the problem that the size of the existing graphene sponge product is limited by equipment. The method comprises the following steps: 1. preparing graphene oxide; 2. reducing graphene oxide; 3. preparing a graphene dispersion liquid; 4. preparing graphene sponge by an electrophoresis method; 5. and drying to obtain the graphene sponge material based on the traditional sponge as the template.
Disclosure of Invention
The existing volatile perfume fiber core rod medium has the defects of poor modification effect, low perfume adsorption capacity, long adsorption time, poor recycling efficiency and the like. Based on the above, the invention provides a preparation method of a graphite core rod as a perfume volatilization medium, belonging to the field of perfume volatilization materials.
A preparation method of a perfume volatilization medium graphite core rod comprises the following specific steps:
s1: preparing polyamic acid, namely putting 400-450 parts of solvent by weight into a glass reactor, then adding 12-18 parts of 4,4' -diaminodiphenyl ether, 10-16 parts of 9, 9-bis (4-aminophenyl) fluorene, 3-7 parts of dimethyl silyl diethylamine, 30-55 parts of norbornane-2-spiro-alpha-cyclopentanone-alpha ' -spiro-2 ' -norbornane-5, 5 ', 6 ' -tetracarboxylic dianhydride into the glass reactor, introducing nitrogen, and reacting under set reaction conditions;
s2: adding 0.02-0.1 part of catalyst, 0.5-2.6 parts of methyl nonenoate and 0.5-2.5 parts of eugenol, controlling the temperature to react for 2-4 hours, and removing white oil by distillation to obtain a polyamic acid solution;
s3: dispersing single-layer graphene oxide, mixing 0.3-3 parts of graphene oxide and 50-100 parts of deionized water according to parts by weight, adding 0.2-1.2 parts of auxiliary dispersing agent, and performing ultrasonic treatment to obtain a graphene oxide dispersion liquid;
s4: preparing a graphite core rod, namely taking the graphene oxide dispersion liquid and the polyamic acid solution according to the volume ratio of 1.5-3, uniformly stirring, freezing for 10-16h, and then vacuumizing and freeze-drying for 30-50h to obtain a polyimide precursor/graphene oxide composite sponge; heating the prepared composite sponge in a nitrogen atmosphere, and keeping the temperature for 2-5h to obtain polyimide/reduced graphene oxide composite sponge; and then cutting and processing to prepare the graphite core rod.
The method provided by the invention can be used for solving the problem that the solvent in S1 can be N-methyl-2-pyrrolidone, N-dimethylpropionamide, N-dimethylformamide and N-ethyl-2-pyrrolidone.
According to the method provided by the invention, the solvent can be one or a mixture of two or more.
The method provided by the invention is characterized in that the reaction conditions set in the S1 are as follows: reacting for 10-16h at 30-40 ℃, and controlling the stirring speed to be 120-180rpm.
According to the method provided by the invention, the catalyst in S2 is chloroplatinic acid hexahydrate.
According to the method provided by the invention, the temperature-controlled reaction temperature in the S2 is 50-60 ℃.
The method provided by the invention is characterized in that the auxiliary dispersant in S3 is a hyperbranched polymer, and can be hyperbranched polyethylene.
The method provided by the invention is characterized in that the ultrasonic treatment conditions in the S3 are as follows: the ultrasonic frequency is 20-32kHz, and the ultrasonic time is 6-18mins.
The method provided by the invention is characterized in that the freezing temperature in the S4 is-10-0 ℃.
According to the method provided by the invention, the heating temperature in the S4 is 170-190 ℃.
Compared with the prior art, the technical scheme has the following beneficial effects:
1. the hyperbranched polymer is used for stripping graphite to obtain single-layer or few-layer graphene, so that the graphene stably exists in an few-layer state, and conditions are provided for subsequent processes;
2. the polyimide/reduced graphene oxide composite sponge has a larger pore size, and is beneficial to full volatilization of the perfume by the volatilization stick;
3. the composite material film-making rod has excellent high and low temperature resistance, can be suitable for various high and low temperature occasions, and has wide product application occasions;
4. the composite material membrane-making rod has excellent mechanical property, is not easy to lose, and can be repeatedly used for a long time.
Detailed Description
Several implementations of the invention are described in detail below by way of different embodiments.
Example 1
A preparation method of a perfume volatilization medium graphite core rod comprises the following specific steps:
s1: preparation of polyamic acid, 400g of N-methyl-2-pyrrolidone as a solvent was placed in a glass reactor, then 12g of 4,4 '-diaminodiphenyl ether, 10g of 9, 9-bis (4-aminophenyl) fluorene, 3g of dimethylsilyldiethylamine, 30g of norbornane-2-spiro- α -cyclopentanone- α' -spiro-2 ″ -norbornane-5, 5 ″,6 ″ -tetracarboxylic dianhydride were added thereto, nitrogen gas was passed through, and the mixture was stirred at 30 ℃ for 10 hours at a stirring speed of 120rpm;
s2: then adding 0.02g of chloroplatinic acid hexahydrate, 0.5g of methyl nonenoate and 0.5g of eugenol, controlling the temperature to be 50 ℃, reacting for 2 hours, and removing white oil through distillation to obtain a polyamic acid solution;
s3: dispersing single-layer graphene oxide, namely mixing 0.3g of graphene oxide with 50g of deionized water, and adding 0.2g of hyperbranched polyethylene, performing ultrasonic treatment for 6mins at the ultrasonic frequency of 20kHz to obtain a graphene oxide dispersion liquid;
s4: preparing a graphite core rod, namely uniformly stirring a graphene oxide dispersion liquid and a polyamic acid solution according to the volume ratio of 1.5, freezing at the temperature of-10 ℃ for 10 hours, and then vacuumizing and freeze-drying for 30 hours to obtain a polyimide precursor/graphene oxide composite sponge; heating the prepared composite sponge to 170 ℃ in a nitrogen atmosphere, and keeping the temperature for 5 hours to obtain polyimide/reduced graphene oxide composite sponge; and cutting and processing to prepare the graphite core rod.
Example 2
S1: preparation of polyamic acid, 400g of N, N-dimethylpropionamide was placed in a glass reactor as a solvent, then 14g of 4,4 '-diaminodiphenyl ether, 12g of 9, 9-bis (4-aminophenyl) fluorene, 3g of dimethylsilyldiethylamine, 35g of norbornane-2-spiro- α -cyclopentanone- α' -spiro-2 "-norbornane-5, 5",6 "-tetracarboxylic dianhydride were added thereto, nitrogen gas was passed through, and the mixture was stirred at 30 ℃ for 12 hours at a stirring rotation speed of 120rpm;
s2: then adding 0.04g of chloroplatinic acid hexahydrate, 0.8g of methyl nonenoate and 0.8g of eugenol, controlling the temperature to be 50 ℃, reacting for 3 hours, and removing white oil through distillation to obtain a polyamic acid solution;
s3: dispersing single-layer graphene oxide, mixing 0.5g of graphene oxide with 60g of deionized water, adding 0.3g of hyperbranched polyethylene, and performing ultrasonic treatment for 8mins at an ultrasonic frequency of 20kHz to obtain a graphene oxide dispersion liquid;
s4: preparing a graphite core rod, namely taking the graphene oxide dispersion liquid and the polyamic acid solution according to the volume ratio of 1.5, uniformly stirring, freezing at-10 ℃ for 12 hours, and then vacuumizing and freeze-drying for 30 hours to obtain a polyimide precursor/graphene oxide composite sponge; heating the prepared composite sponge to 170 ℃ in a nitrogen atmosphere, and keeping the temperature for 4 hours to obtain polyimide/reduced graphene oxide composite sponge; and cutting and processing to prepare the graphite core rod.
Example 3
S1: preparation of polyamic acid, 420g of N, N-dimethylformamide was placed as a solvent in a glass reactor, then 14g of 4,4 '-diaminodiphenyl ether, 14g of 9, 9-bis (4-aminophenyl) fluorene, 4g of dimethylsilyldiethylamine, 35g of norbornane-2-spiro- α -cyclopentanone- α' -spiro-2 "-norbornane-5, 5",6 "-tetracarboxylic dianhydride were added thereto, nitrogen gas was passed through, and the mixture was stirred at 30 ℃ for 14 hours at a stirring speed of 120rpm;
s2: then adding 0.06g of chloroplatinic acid hexahydrate, 0.8g of methyl nonenoate and 1.0g of eugenol, controlling the temperature to be 50 ℃, reacting for 4 hours, and removing white oil through distillation to obtain a polyamic acid solution;
s3: dispersing single-layer graphene oxide, mixing 0.8g of graphene oxide with 60g of deionized water, adding 0.3g of hyperbranched polyethylene, and performing ultrasonic treatment for 8mins at an ultrasonic frequency of 20kHz to obtain a graphene oxide dispersion liquid;
s4: preparing a graphite core rod, namely uniformly stirring a graphene oxide dispersion liquid and a polyamic acid solution according to the volume ratio of 1.8, freezing at the temperature of-10 ℃ for 12 hours, and then vacuumizing and freeze-drying for 35 hours to obtain a polyimide precursor/graphene oxide composite sponge; heating the prepared composite sponge to 175 ℃ in a nitrogen atmosphere, and keeping the temperature for 3 hours to obtain polyimide/reduced graphene oxide composite sponge; and then cutting and processing to prepare the graphite core rod.
Example 4
S1: preparation of polyamic acid, 420g of N-methyl-2-pyrrolidone as a solvent was placed in a glass reactor, then 1lg of 4,4 '-diaminodiphenyl ether, 14g of 9, 9-bis (4-aminophenyl) fluorene, 5g of dimethylsilyldiethylamine, 40g of norbornane-2-spiro- α -cyclopentanone- α' -spiro-2 ″ -norbornane-5, 5 ″,6 ″ -tetracarboxylic dianhydride were added thereto, nitrogen gas was blown in, and the mixture was stirred at 35 ℃ for 16 hours at a stirring rate of 120rpm;
s2: then 0.08g of chloroplatinic acid hexahydrate, 1.2g of methyl nonenoate and 1.2g of eugenol are added, the temperature is controlled to be 55 ℃, the reaction is carried out for 2 hours, and white oil is removed by distillation to obtain polyamic acid solution;
s3: dispersing single-layer graphene oxide, mixing 1.0g of graphene oxide with 60g of deionized water, adding 0.5g of hyperbranched polyethylene, and performing ultrasonic treatment for 10mins at the ultrasonic frequency of 26kHz to obtain a graphene oxide dispersion liquid;
s4: preparing a graphite core rod, uniformly stirring the graphene oxide dispersion liquid and the polyamic acid solution according to the volume ratio of 1.0, freezing at-8 ℃ for 15 hours, and then vacuumizing and freeze-drying for 40 hours to obtain a polyimide precursor/graphene oxide composite sponge; heating the prepared composite sponge to 175 ℃ in a nitrogen atmosphere, and keeping the temperature for 3 hours to obtain polyimide/reduced graphene oxide composite sponge; and cutting and processing to prepare the graphite core rod.
Example 5
S1: preparation of polyamic acid, 435g of N-methyl-2-pyrrolidone as a solvent was placed in a glass reactor, then 1lg of 4,4 '-diaminodiphenyl ether, 1lg of 9, 9-bis (4-aminophenyl) fluorene, 6g of dimethylsilyldiethylamine, 40g of norbornane-2-spiro- α -cyclopentanone- α' -spiro-2 "-norbornane-5, 5",6 "-tetracarboxylic dianhydride were added thereto, nitrogen gas was passed through, and the mixture was stirred at 40 ℃ for 10 hours;
s2: then adding 0.05g of chloroplatinic acid hexahydrate, 1.5g of methyl nonenoate and 1.4g of eugenol, controlling the temperature to be 60 ℃, reacting for 2 hours, and removing white oil through distillation to obtain a polyamic acid solution;
s3: dispersing single-layer graphene oxide, mixing 1.2g of graphene oxide with 70g of deionized water, adding 0.6g of hyperbranched polyethylene, and performing ultrasonic treatment for 10mins at the ultrasonic frequency of 26kHz to obtain a graphene oxide dispersion liquid;
s4: preparing a graphite core rod, namely uniformly stirring the graphene oxide dispersion liquid and the polyamic acid solution according to the volume ratio of 1.2, freezing at the temperature of-5 ℃ for 15 hours, and then vacuumizing and freeze-drying for 40 hours to obtain a polyimide precursor/graphene oxide composite sponge; heating the prepared composite sponge to 180 ℃ in a nitrogen atmosphere, and keeping the temperature for 3 hours to obtain polyimide/reduced graphene oxide composite sponge; and cutting and processing to prepare the graphite core rod.
Example 6
S1: preparation of polyamic acid, 435g of N-ethyl-2-pyrrolidone as a solvent was placed in a glass reactor, then 18g of 4,4 '-diaminodiphenyl ether, 1lg of 9, 9-bis (4-aminophenyl) fluorene, 6g of dimethylsilyldiethylamine, 45g of norbornane-2-spiro- α -cyclopentanone- α' -spiro-2 "-norbornane-5, 5",6 "-tetracarboxylic dianhydride were added thereto, nitrogen gas was passed through, and the mixture was stirred at 40 ℃ for 12 hours;
s2: then adding 0.07g of chloroplatinic acid hexahydrate, 1.8g of methyl nonenoate and 1.6g of eugenol, controlling the temperature to be 60 ℃, reacting for 3 hours, and removing white oil through distillation to obtain a polyamic acid solution;
s3: dispersing single-layer graphene oxide, mixing 1.8g of graphene oxide with 80g of deionized water, adding 0.8g of hyperbranched polyethylene, performing ultrasonic treatment for 14mins at the ultrasonic frequency of 26kHz, and obtaining graphene oxide dispersion liquid;
s4: preparing a graphite core rod, namely uniformly stirring the graphene oxide dispersion liquid and the polyamic acid solution according to the volume ratio of 1.4, freezing at-4 ℃ for 16h, and then vacuumizing and freeze-drying for 45h to obtain a polyimide precursor/graphene oxide composite sponge; heating the prepared composite sponge to 180 ℃ in a nitrogen atmosphere, and keeping the temperature for 3 hours to obtain polyimide/reduced graphene oxide composite sponge; and cutting and processing to prepare the graphite core rod.
Example 7
S1: preparation of polyamic acid, 450g of N, N-dimethylpropionamide was placed in a glass reactor as a solvent, then 18g of 4,4 '-diaminodiphenyl ether, 1lg of 9, 9-bis (4-aminophenyl) fluorene, 7g of dimethylsilyldiethylamine, 50g of norbornane-2-spiro- α -cyclopentanone- α' -spiro-2 "-norbornane-5, 5",6 "-tetracarboxylic dianhydride were added thereto, nitrogen gas was passed through the mixture, and the mixture was stirred at 40 ℃ for 14 hours;
s2: then adding 0.1g of chloroplatinic acid hexahydrate, 2.4g of methyl nonenoate and 2.2g of eugenol, controlling the temperature to be 60 ℃, reacting for 4 hours, and removing white oil through distillation to obtain a polyamic acid solution;
s3: dispersing single-layer graphene oxide, mixing 2.4g of graphene oxide with 90g of deionized water, adding 1.0g of hyperbranched polyethylene, and performing ultrasonic treatment for 12mins at an ultrasonic frequency of 32kHz to obtain a graphene oxide dispersion liquid;
s4: preparing a graphite core rod, namely taking the graphene oxide dispersion liquid and the polyamic acid solution according to the volume ratio of 1.7, uniformly stirring, freezing at 0 ℃ for 14h, and then vacuumizing and freeze-drying for 50h to obtain a polyimide precursor/graphene oxide composite sponge; heating the prepared composite sponge to 190 ℃ in a nitrogen atmosphere, and keeping the temperature for 3 hours to obtain polyimide/reduced graphene oxide composite sponge; and cutting and processing to prepare the graphite core rod.
Example 8
S1: preparation of polyamic acid, 450g of N, N-dimethylformamide was placed in a glass reactor as a solvent, then 18g of 4,4 '-diaminodiphenyl ether, 1lg of 9, 9-bis (4-aminophenyl) fluorene, 7g of dimethylsilyldiethylamine, 55g of norbornane-2-spiro- α -cyclopentanone- α' -spiro-2 "-norbornane-5, 5",6 "-tetracarboxylic dianhydride were added thereto, nitrogen gas was passed through, and the mixture was stirred at 40 ℃ for 16 hours;
s2: then adding 0.1g of chloroplatinic acid hexahydrate, 2.6g of methyl nonenoate and 2.5g of eugenol, controlling the temperature at 60 ℃, reacting for 4 hours, and removing white oil through distillation to obtain a polyamic acid solution;
s3: dispersing single-layer graphene oxide, mixing 3g of graphene oxide with 100g of deionized water, adding 1.2g of hyperbranched polyethylene, and performing ultrasonic treatment for 18mins at an ultrasonic frequency of 32kHz to obtain a graphene oxide dispersion liquid;
s4: preparing a graphite core rod, namely taking oxidized graphene dispersion liquid and polyamic acid solution according to the volume ratio of 1; heating the prepared composite sponge to 190 ℃ in a nitrogen atmosphere, and keeping the temperature for 5 hours to obtain polyimide/reduced graphene oxide composite sponge; and cutting and processing to prepare the graphite core rod.
Comparative example 1
In this example, S1 was prepared in the same manner as in example 1 except that 4,4' -diaminodiphenyl ether was not added.
Comparative example 2
In this example, S2 was the same as in example 1 except that chloroplatinic acid hexahydrate was not added.
Comparative example 3
In this example S3 is the same as example 1 without the addition of hyperbranched polyethylene.
Examples evaluation:
the test method comprises the following steps:
1. instrument for measuring the position of a moving object
Agilent6890N gas chromatograph, agilent5973N gas chromatograph-mass spectrometer
2. Sample processing
The perfume sample is a commercial product, and is subjected to dehydration treatment and to be tested.
3. Conditions of analysis
A. Chromatographic conditions are as follows:
and (3) chromatographic column: HP-5 elastic quartz capillary column (50 m.times.0.32 m.times.0.25 um), column temperature: heating to 250 ℃ at 50 ℃, wherein the heating rate is 2 ℃/min, keeping the temperature at 250 ℃ for 10mins, and carrying gas: high purity nitrogen, column flow rate: 1.6ml/min, internal standard: n-heptadecane
B. Mass spectrum conditions:
the temperature of the transmission line is 280 ℃, the temperature of the ion source is 230 ℃, and the temperature of the quadrupole rod is 150 DEG C
An ionization mode: EI (electronic instrument)
Ionization energy: 70ev
Multiplier voltage: 1400V
Scanning range: 33 to 425amu
And (3) sample introduction mode: split-flow sample introduction, split-flow ratio: 40:1
Carrier gas: high purity helium, column flow rate: 1ml/mim
Search by adopting series connection of Nist98 and Wiley6 spectral library
4. The analysis method comprises the following steps: the graphite core rods prepared in the above examples and comparative examples are subjected to adsorption rate and volatilization time tests of the same type of perfume purchased in the market for 1 time, 10 times and 20 times, and the components and the content of the perfume volatilized by the volatilization rod are analyzed and detected by a gas chromatograph and a mass spectrometer,
the results are shown in the following table:
Claims (10)
1. a preparation method of a perfume volatilization medium graphite core rod comprises the following specific steps:
s1: preparing polyamic acid, namely putting 400-450 parts of solvent into a glass reactor according to parts by weight, then adding 12-18 parts of 4,4' -diaminodiphenyl ether, 10-16 parts of 9, 9-bis (4-aminophenyl) fluorene, 3-7 parts of dimethyl silicon diethylamine, 30-55 parts of norbornane-2-spiro-alpha-cyclopentanone-alpha ' -spiro-2 ' -norbornane-5, 5 ', 6 ' -tetracarboxylic dianhydride into the glass reactor, introducing nitrogen into the glass reactor, and reacting under the set reaction conditions;
s2: adding 0.02-0.1 part of catalyst, 0.5-2.6 parts of methyl nonenoate and 0.5-2.5 parts of eugenol, controlling the temperature to react for 2-4 hours, and removing white oil by distillation to obtain a polyamic acid solution;
s3: dispersing single-layer graphene oxide, mixing 0.3-3 parts of graphene oxide and 50-100 parts of deionized water according to parts by weight, adding 0.2-1.2 parts of auxiliary dispersing agent, and performing ultrasonic treatment to obtain a graphene oxide dispersion liquid;
s4: preparing a graphite core rod, namely taking the graphene oxide dispersion liquid and the polyamic acid solution according to the volume ratio of 1.5-3, uniformly stirring, freezing for 10-16h, and then vacuumizing and freeze-drying for 30-50h to obtain a polyimide precursor/graphene oxide composite sponge; heating the prepared composite sponge in a nitrogen atmosphere, and keeping the temperature for 2-5h to obtain polyimide/reduced graphene oxide composite sponge; and cutting and processing to prepare the graphite core rod.
2. The preparation method of the graphite core rod for the perfume volatilization medium, according to the claim 1, is characterized in that: the solvent in S1 can be N-methyl-2-pyrrolidone, N-dimethylpropionamide, N-dimethylformamide and N-ethyl-2-pyrrolidone.
3. The preparation method of the graphite core rod as claimed in claim 2, wherein the graphite core rod comprises the following steps: the solvent may be one kind or a mixture of two or more kinds.
4. The preparation method of the graphite core rod as claimed in claim 1, wherein the graphite core rod comprises the following steps: the reaction conditions set in the step S1 are as follows: reacting for 10-16h at 30-40 ℃, and controlling the stirring speed to be 120-180rpm.
5. The preparation method of the graphite core rod for the perfume volatilization medium, according to the claim 1, is characterized in that: the catalyst in the S2 is chloroplatinic acid hexahydrate.
6. The preparation method of the graphite core rod for the perfume volatilization medium, according to the claim 1, is characterized in that: and the temperature-controlled reaction temperature in the S2 is 50-60 ℃.
7. The preparation method of the graphite core rod as claimed in claim 1, wherein the graphite core rod comprises the following steps: the auxiliary dispersing agent in S3 is hyperbranched polymer, and can be hyperbranched polyethylene.
8. The preparation method of the graphite core rod as claimed in claim 1, wherein the graphite core rod comprises the following steps: the ultrasonic treatment conditions in the S3 are as follows: the ultrasonic frequency is 20-32kHz, and the ultrasonic time is 6-18mins.
9. The preparation method of the graphite core rod for the perfume volatilization medium, according to the claim 1, is characterized in that: the freezing temperature in the S4 is-10-0 ℃.
10. The preparation method of the graphite core rod for the perfume volatilization medium, according to the claim 1, is characterized in that: the heating temperature in the S4 is 170-190 ℃.
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| CN103602065A (en) * | 2013-11-25 | 2014-02-26 | 中国科学院山西煤炭化学研究所 | Preparation method of reduced graphene and polyimide nano composite material |
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| CN107949597A (en) * | 2015-07-16 | 2018-04-20 | 宇部兴产株式会社 | Polyamic acid solution composition and polyimide film |
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