CN114574002A - Carbon black nano material with high filtering precision and preparation method thereof - Google Patents
Carbon black nano material with high filtering precision and preparation method thereof Download PDFInfo
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- 239000006229 carbon black Substances 0.000 title claims abstract description 185
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 53
- 238000001914 filtration Methods 0.000 title claims abstract description 49
- 238000002360 preparation method Methods 0.000 title abstract description 20
- 229910021392 nanocarbon Inorganic materials 0.000 claims abstract description 60
- 238000006243 chemical reaction Methods 0.000 claims abstract description 36
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 17
- 239000002270 dispersing agent Substances 0.000 claims abstract description 17
- 239000003607 modifier Substances 0.000 claims abstract description 17
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000007822 coupling agent Substances 0.000 claims abstract description 16
- 239000002904 solvent Substances 0.000 claims abstract description 5
- 239000002994 raw material Substances 0.000 claims abstract description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 48
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 32
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims description 28
- 150000001721 carbon Chemical class 0.000 claims description 25
- 238000001291 vacuum drying Methods 0.000 claims description 20
- 238000001035 drying Methods 0.000 claims description 19
- 238000011049 filling Methods 0.000 claims description 16
- 229910052757 nitrogen Inorganic materials 0.000 claims description 16
- 238000002156 mixing Methods 0.000 claims description 10
- 238000000227 grinding Methods 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 8
- 238000001556 precipitation Methods 0.000 claims description 8
- 239000000376 reactant Substances 0.000 claims description 8
- 238000007789 sealing Methods 0.000 claims description 8
- 238000003756 stirring Methods 0.000 claims description 8
- 238000005406 washing Methods 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 6
- AGBXYHCHUYARJY-UHFFFAOYSA-N 2-phenylethenesulfonic acid Chemical compound OS(=O)(=O)C=CC1=CC=CC=C1 AGBXYHCHUYARJY-UHFFFAOYSA-N 0.000 claims description 3
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 claims description 3
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Natural products C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims description 3
- UKLDJPRMSDWDSL-UHFFFAOYSA-L [dibutyl(dodecanoyloxy)stannyl] dodecanoate Chemical compound CCCCCCCCCCCC(=O)O[Sn](CCCC)(CCCC)OC(=O)CCCCCCCCCCC UKLDJPRMSDWDSL-UHFFFAOYSA-L 0.000 claims description 3
- 239000012975 dibutyltin dilaurate Substances 0.000 claims description 3
- FWDBOZPQNFPOLF-UHFFFAOYSA-N ethenyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C=C FWDBOZPQNFPOLF-UHFFFAOYSA-N 0.000 claims description 3
- NKSJNEHGWDZZQF-UHFFFAOYSA-N ethenyl(trimethoxy)silane Chemical compound CO[Si](OC)(OC)C=C NKSJNEHGWDZZQF-UHFFFAOYSA-N 0.000 claims description 3
- FPYJFEHAWHCUMM-UHFFFAOYSA-N maleic anhydride Chemical compound O=C1OC(=O)C=C1 FPYJFEHAWHCUMM-UHFFFAOYSA-N 0.000 claims description 3
- 229940051841 polyoxyethylene ether Drugs 0.000 claims description 3
- 229920000056 polyoxyethylene ether Polymers 0.000 claims description 3
- 125000003011 styrenyl group Chemical group [H]\C(*)=C(/[H])C1=C([H])C([H])=C([H])C([H])=C1[H] 0.000 claims description 3
- DVKJHBMWWAPEIU-UHFFFAOYSA-N toluene 2,4-diisocyanate Chemical compound CC1=CC=C(N=C=O)C=C1N=C=O DVKJHBMWWAPEIU-UHFFFAOYSA-N 0.000 claims description 3
- VTHOKNTVYKTUPI-UHFFFAOYSA-N triethoxy-[3-(3-triethoxysilylpropyltetrasulfanyl)propyl]silane Chemical compound CCO[Si](OCC)(OCC)CCCSSSSCCC[Si](OCC)(OCC)OCC VTHOKNTVYKTUPI-UHFFFAOYSA-N 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 claims description 2
- 238000000605 extraction Methods 0.000 claims description 2
- 238000003760 magnetic stirring Methods 0.000 claims description 2
- GBMDVOWEEQVZKZ-UHFFFAOYSA-N methanol;hydrate Chemical compound O.OC GBMDVOWEEQVZKZ-UHFFFAOYSA-N 0.000 claims description 2
- 238000005086 pumping Methods 0.000 claims 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 125000000751 azo group Chemical group [*]N=N[*] 0.000 abstract description 8
- 239000002245 particle Substances 0.000 abstract description 6
- 230000002708 enhancing effect Effects 0.000 abstract description 3
- 239000000463 material Substances 0.000 description 9
- 230000000052 comparative effect Effects 0.000 description 7
- 239000007864 aqueous solution Substances 0.000 description 6
- 239000000126 substance Substances 0.000 description 6
- 230000006872 improvement Effects 0.000 description 5
- 230000004048 modification Effects 0.000 description 4
- 238000012986 modification Methods 0.000 description 4
- 229920000642 polymer Polymers 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 230000002776 aggregation Effects 0.000 description 2
- 238000004220 aggregation Methods 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 230000003993 interaction Effects 0.000 description 2
- 230000002787 reinforcement Effects 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 238000005299 abrasion Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000005728 strengthening Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C1/00—Treatment of specific inorganic materials other than fibrous fillers; Preparation of carbon black
- C09C1/44—Carbon
- C09C1/48—Carbon black
- C09C1/487—Separation; Recovery
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09C—TREATMENT OF INORGANIC MATERIALS, OTHER THAN FIBROUS FILLERS, TO ENHANCE THEIR PIGMENTING OR FILLING PROPERTIES ; PREPARATION OF CARBON BLACK ; PREPARATION OF INORGANIC MATERIALS WHICH ARE NO SINGLE CHEMICAL COMPOUNDS AND WHICH ARE MAINLY USED AS PIGMENTS OR FILLERS
- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/08—Treatment with low-molecular-weight non-polymer organic compounds
Abstract
The invention relates to the technical field of carbon black nano materials, in particular to a carbon black nano material with high filtering precision and a preparation method thereof. The feed comprises the following raw materials: nano carbon black, nano white carbon black, a coupling agent, a grafting agent, a modifier and a dispersant, and the balance being a solvent; according to the carbon black nano material with high filtering precision and the preparation method thereof, the added modifier can lead out the surface azo group of the nano carbon black to form reactive carbon black containing the azo group, the grafting reaction is carried out on the reactive carbon black and the nano carbon black through the added grafting agent, so that the dispersity among nano carbon black particles is improved, the filtering precision of the nano carbon black is improved, and the added nano carbon black can be matched with the nano carbon black to play a role in enhancing the physical strength of the carbon black.
Description
Technical Field
The invention relates to the technical field of carbon black nano materials, in particular to a carbon black nano material with high filtering precision and a preparation method thereof.
Background
Numerous experimental and theoretical studies have shown that efficient reinforcement of rubber must be "nano" reinforcement. The compounding method of the nano carbon black and the rubber solves the problems of dispersion of nano materials and strengthening of an interface effect between the nano carbon black and a matrix to a certain extent, but the nano carbon black is poor in dispersibility, and if the nano carbon black is used in a filter element, the filter precision is quite insufficient, so that in order to improve the application range of the carbon black, a carbon black nano material with high filter precision is needed to overcome the defects in the prior art.
Disclosure of Invention
The invention aims to provide a carbon black nano material with high filtering precision and a preparation method thereof, so as to solve the problems in the background technology.
In order to achieve the above purpose, in one aspect, the present invention provides a carbon black nanomaterial with high filtration precision, which comprises the following raw materials in parts by weight: 50-70 parts of nano carbon black, 10-20 parts of nano white carbon black, 1-3 parts of coupling agent, 5-9 parts of grafting agent, 1-5 parts of modifier and 0.1-3 parts of dispersing agent, and the balance of solvent.
As a further improvement of the technical scheme, the coupling agent is selected from at least one of bis (3-triethoxysilylpropyl) tetrasulfide, vinyl triethoxysilane and vinyl trimethoxysilane, and the main function of the coupling agent is to further enhance the interaction between the polymer and the filler and improve the wear resistance and the processability.
As a further improvement of the technical scheme, the grafting agent is styrene, so that the aggregation of the carbon black material is reduced, and the carbon black material has better dispersibility in a polymer matrix.
As a further improvement of the technical scheme, the modifier at least comprises dimethyl sulfoxide, toluene diisocyanate and dibutyl tin dilaurate, and is used for preparing the reactive carbon black containing azo groups, so that the modification of the nano carbon black is facilitated.
As a further improvement of the technical scheme, the dispersing agent is selected from at least one of maleic anhydride, methacrylic acid, styrene sulfonic acid and polyoxyethylene ether, and the dispersing agent is mainly used for improving the dispersing performance of all materials and enabling all materials to be better mixed.
As a further improvement of the technical scheme, the solvent at least comprises methanol and toluene.
In another aspect, the present invention provides a method for preparing a carbon black nanomaterial with high filtration precision as described in any one of the above, comprising the steps of:
s1, adding the nano carbon black and the modifier into a reaction kettle, sealing, vacuumizing, filling nitrogen, and then stirring by magnetic force;
s2, filtering the reacted nano carbon black, repeatedly washing the nano carbon black by a methanol water solution, drying the nano carbon black in vacuum at room temperature, and grinding the nano carbon black to obtain reactive carbon black;
s3, adding a grafting agent and reactive carbon black into a reaction kettle, vacuumizing and filling nitrogen, then heating in a constant-temperature water bath, after the reaction is finished, performing methanol reverse precipitation on a reactant, filtering, and then placing at room temperature for vacuum drying;
s4, adding the dried matter into a Soxhlet extractor, repeatedly extracting the dried matter through methylbenzene, and then drying the product in vacuum at room temperature to obtain modified carbon black;
and S5, adding the modified carbon black, the nano white carbon black, the coupling agent and the dispersing agent into a reaction kettle, mixing, and drying to obtain the carbon black nano material.
Preferably, in the S1, the vacuumizing frequency is 5-7 times, the magnetic stirring time is 24-30h, the temperature is 25-60 ℃, and in the S2, the vacuum drying time is 22-26 h.
Preferably, in the step S3, the vacuumizing times are 5-7 times, and the vacuum drying time is 22-26 h.
Preferably, in S4, the extraction times are 5-6 times, and the vacuum drying time is 22-26 h.
Compared with the prior art, the invention has the beneficial effects that:
1. according to the carbon black nano material with high filtering precision and the preparation method thereof, the surface azo group of the nano carbon black can be led out through the added modifier to form reactive carbon black containing the azo group, and the grafting reaction is carried out on the reactive carbon black and the nano carbon black through the added grafting agent, so that the dispersibility among nano carbon black particles is improved, and the filtering precision of the nano carbon black is improved.
2. In the carbon black nano material with high filtering precision and the preparation method thereof, the added nano white carbon black can be matched with the nano carbon black, so that the effect of enhancing the physical strength of the carbon black is achieved.
Drawings
Fig. 1 is a schematic view of the entire structure of embodiment 1.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without any inventive step based on the embodiments of the present invention, are within the scope of the present invention.
Embodiment 1 a carbon black nanomaterial with high filtering precision and a preparation method thereof, comprising:
firstly, preparing modified carbon black;
1. adding 50 parts of nano carbon black and 1 part of modifier into a reaction kettle, sealing, vacuumizing, filling nitrogen for 5 times, and then magnetically stirring for 24 hours at the temperature of 25 ℃;
2. filtering the reacted nano carbon black, repeatedly washing the nano carbon black by using a methanol aqueous solution, carrying out vacuum drying for 22 hours at room temperature, and grinding the nano carbon black to obtain reactive carbon black;
3. adding 5 parts of grafting agent and reactive carbon black into a reaction kettle, vacuumizing and filling nitrogen for 5 times, then heating in a constant-temperature water bath, after the reaction is finished, performing methanol reverse precipitation on a reactant, filtering, and then placing at room temperature for vacuum drying for 22 hours;
4. adding the dried substance into a Soxhlet extractor, repeatedly extracting for 5 times by toluene, and then drying the product in vacuum at room temperature for 22 hours to obtain modified carbon black;
second, preparation of carbon black nano material
Adding 10 parts of modified carbon black and nano white carbon black, 1 part of coupling agent and 0.1 part of dispersing agent into a reaction kettle, mixing, and drying to obtain the carbon black nano material.
Embodiment 2 a carbon black nanomaterial with high filtering precision and a preparation method thereof, comprising the following steps:
firstly, preparing modified carbon black;
1. adding 55 parts of nano carbon black and 2 parts of modifier into a reaction kettle, sealing, vacuumizing, filling nitrogen for 5 times, and then magnetically stirring for 25 hours at the temperature of 30 ℃;
2. filtering the reacted nano carbon black, repeatedly washing the nano carbon black by using a methanol aqueous solution, carrying out vacuum drying at room temperature for 23 hours, and grinding the nano carbon black to obtain reactive carbon black;
3. adding 7 parts of grafting agent and reactive carbon black into a reaction kettle, vacuumizing and filling nitrogen for 5 times, then heating in a constant-temperature water bath, after the reaction is finished, performing methanol reverse precipitation on a reactant, filtering, and then placing at room temperature for vacuum drying for 23 hours;
4. adding the dried substance into a Soxhlet extractor, repeatedly extracting for 5 times by toluene, and then drying the product in vacuum at room temperature for 23h to obtain modified carbon black;
second, preparation of carbon black nano material
Adding 13 parts of modified carbon black and nano white carbon black, 1 part of coupling agent and 1 part of dispersing agent into a reaction kettle for mixing, and drying to obtain the carbon black nano material.
Embodiment 3 a carbon black nanomaterial with high filtering precision and a preparation method thereof, comprising:
firstly, preparing modified carbon black;
1. adding 60 parts of nano carbon black and 3 parts of modifier into a reaction kettle, sealing, vacuumizing, filling nitrogen for 6 times, and then magnetically stirring for 26 hours at the temperature of 40 ℃;
2. filtering the reacted nano carbon black, repeatedly washing the nano carbon black by using a methanol aqueous solution, carrying out vacuum drying at room temperature for 24 hours, and grinding the nano carbon black to obtain reactive carbon black;
3. adding 7 parts of grafting agent and reactive carbon black into a reaction kettle, vacuumizing and filling nitrogen for 6 times, then heating in a constant-temperature water bath, after the reaction is finished, performing methanol reverse precipitation on a reactant, filtering, and then placing at room temperature for vacuum drying for 24 hours;
4. adding the dried substance into a Soxhlet extractor, repeatedly extracting for 6 times by toluene, and then drying the product in vacuum at room temperature for 24 hours to obtain modified carbon black;
second, preparation of carbon black nano material
Adding 15 parts of modified carbon black and nano white carbon black, 2 parts of coupling agent and 2 parts of dispersing agent into a reaction kettle for mixing, and drying to obtain the carbon black nano material.
Embodiment 4 a carbon black nanomaterial with high filtering precision and a preparation method thereof, comprising:
firstly, preparing modified carbon black;
1. adding 65 parts of nano carbon black and 4 parts of modifier into a reaction kettle, sealing, vacuumizing, filling nitrogen for 7 times, and then stirring for 28 hours by magnetic force at the temperature of 50 ℃;
2. filtering the reacted nano carbon black, repeatedly washing the nano carbon black by using a methanol aqueous solution, carrying out vacuum drying for 25 hours at room temperature, and grinding the nano carbon black to obtain reactive carbon black;
3. adding 8 parts of grafting agent and reactive carbon black into a reaction kettle, vacuumizing and filling nitrogen for 7 times, then heating in a constant-temperature water bath, after the reaction is finished, performing methanol reverse precipitation on a reactant, filtering, and then placing at room temperature for vacuum drying for 25 hours;
4. adding the dried substance into a Soxhlet extractor, repeatedly extracting for 6 times by toluene, and then drying the product at room temperature in vacuum for 25 hours to obtain modified carbon black;
second, preparation of carbon black nano material
Adding 17 parts of modified carbon black and nano white carbon black, 3 parts of coupling agent and 3 parts of dispersing agent into a reaction kettle for mixing, and drying to obtain the carbon black nano material.
Embodiment 5 a carbon black nanomaterial with high filtering precision and a preparation method thereof, comprising:
firstly, preparing modified carbon black;
1. adding 70 parts of nano carbon black and 5 parts of modifier into a reaction kettle, sealing, vacuumizing, filling nitrogen for 7 times, and then magnetically stirring for 30 hours at the temperature of 60 ℃;
2. filtering the reacted nano carbon black, repeatedly washing the nano carbon black by using a methanol aqueous solution, carrying out vacuum drying for 26 hours at room temperature, and grinding the nano carbon black to obtain reactive carbon black;
3. adding 9 parts of grafting agent and reactive carbon black into a reaction kettle, vacuumizing and filling nitrogen for 7 times, then heating in a constant-temperature water bath, after the reaction is finished, performing methanol reverse precipitation on a reactant, filtering, and then placing at room temperature for vacuum drying for 26 hours;
4. adding the dried substance into a Soxhlet extractor, repeatedly extracting for 6 times by toluene, and then drying the product in vacuum at room temperature for 26 hours to obtain modified carbon black;
second, preparation of carbon black nano material
And adding 20 parts of modified carbon black and nano white carbon black, 3 parts of coupling agent and 3 parts of dispersing agent into a reaction kettle, mixing, and drying to obtain the carbon black nano material.
In the above examples 1 to 5, the coupling agent is selected from at least one of bis (3-triethoxysilylpropyl) tetrasulfide, vinyltriethoxysilane and vinyltrimethoxysilane, which mainly functions to further enhance the interaction between the polymer and the filler, to improve the abrasion resistance and processability;
the grafting agent is styrene, so that the aggregation of the carbon black material is reduced, and the carbon black material has good dispersibility in a polymer matrix;
the modifier at least comprises dimethyl sulfoxide, toluene diisocyanate and dibutyl tin dilaurate, and is used for preparing reactive carbon black containing azo groups, so that modification of the nano carbon black is facilitated;
the dispersing agent is selected from at least one of maleic anhydride, methacrylic acid, styrene sulfonic acid and polyoxyethylene ether, and the dispersing agent is mainly used for improving the dispersing performance of all materials and better mixing all the materials;
according to the invention, the added modifier can lead out the surface azo group of the nano carbon black to form reactive carbon black containing the azo group, and the grafting reaction is carried out on the reactive carbon black and the nano carbon black through the added grafting agent, so that the dispersibility among nano carbon black particles is improved, and the filtering precision of the nano carbon black is improved;
the added nano white carbon black can be matched with the nano carbon black, so that the effect of enhancing the physical strength of the carbon black is achieved.
The relevant indexes of the carbon black nano material with high filtering precision prepared by the invention are shown in the following table 1:
TABLE 1
| Example 1 | Example 2 | Example 3 | Example 4 | Example 5 | |
| Particle size (nm) | 24 | 23 | 22 | 25 | 27 |
| Filter fineness (um) | 0.10 | 0.08 | 0.05 | 0.10 | 0.12 |
| Shore Hardness (HA) | 53 | 58 | 65 | 66 | 66 |
As shown in Table 1, in examples 1-5, the particle size of each carbon black nano material is 20-30nm, the expressive ability of the filter precision is 0.05-0.15, and the Shore hardness is 50-70.
Comparative example 1 a carbon black nanomaterial and a method of preparing the same, comprising:
adding 60 parts of nano carbon black, 15 parts of nano white carbon black, 2 parts of coupling agent and 2 parts of dispersing agent into a reaction kettle, mixing, and drying to obtain the carbon black nano material.
Comparative example 2 a carbon black nanomaterial and a method of preparing the same, comprising:
firstly, preparing modified carbon black;
1. adding 60 parts of nano carbon black and 3 parts of modifier into a reaction kettle, sealing, vacuumizing, filling nitrogen for 6 times, and then magnetically stirring for 26 hours at the temperature of 40 ℃;
2. filtering the reacted nano carbon black, repeatedly washing the nano carbon black by using a methanol aqueous solution, carrying out vacuum drying at room temperature for 24 hours, and grinding the nano carbon black to obtain reactive carbon black;
3. adding 7 parts of grafting agent and reactive carbon black into a reaction kettle, vacuumizing and filling nitrogen for 6 times, then heating in a constant-temperature water bath, after the reaction is finished, performing methanol reverse precipitation on a reactant, filtering, and then placing at room temperature for vacuum drying for 24 hours;
4. adding the dried substance into a Soxhlet extractor, repeatedly extracting for 6 times by toluene, and then drying the product in vacuum at room temperature for 24 hours to obtain modified carbon black;
preparation of carbon black nano material
Adding the modified carbon black, 2 parts of coupling agent and 2 parts of dispersing agent into a reaction kettle for mixing, and drying to obtain the carbon black nano material.
The carbon black nano material with high filtering precision prepared by the invention has higher filtering precision and strength, and has a larger relation with the prepared modified carbon black and the added nano white carbon black, and in order to verify the related technical scheme, the applicant performs the following tests:
comparative examples 1 to 2: by adopting the method of example 3, under the condition that the preparation of the modified carbon black material is removed and the nano white carbon black is removed, the relevant indexes of the prepared carbon black nano material are detected, and the specific table is shown in table 2:
TABLE 2
| Comparative example 1 | Comparative example 2 | Example 3 | |
| Particle size (nm) | 23 | 25 | 22 |
| Filter fineness (um) | 1.20 | 0.05 | 0.05 |
| Shore Hardness (HA) | 63 | 39 | 65 |
As shown in table 2, in comparative example 1, when the step of preparing modified carbon black is removed alone, the filtration precision of the carbon black nanomaterial is significantly reduced compared to example 3, and in comparative example 2, when the nano white carbon black is removed alone, the hardness of the carbon black nanomaterial is significantly reduced compared to example 3, so that it can be demonstrated that the carbon black nanomaterial prepared by the present invention has the characteristics of high filtration precision and high hardness.
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and the preferred embodiments of the present invention are described in the above embodiments and the description, and the present invention is not limited to the embodiments, and various changes and modifications may be made without departing from the spirit and scope of the present invention, and these changes and modifications fall within the scope of the claimed invention. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (10)
1. The carbon black nano material with high filtering precision is characterized by comprising the following raw materials in parts by weight: 50-70 parts of nano carbon black, 10-20 parts of nano white carbon black, 1-3 parts of coupling agent, 5-9 parts of grafting agent, 1-5 parts of modifier and 0.1-3 parts of dispersing agent, and the balance of solvent.
2. The carbon black nanomaterial of high filtration precision according to claim 1, characterized in that: the coupling agent is at least one selected from bis (3-triethoxysilylpropyl) tetrasulfide, vinyltriethoxysilane and vinyltrimethoxysilane.
3. The carbon black nanomaterial of high filtration precision according to claim 1, characterized in that: the grafting agent is styrene.
4. The carbon black nanomaterial of high filtration precision according to claim 1, characterized in that: the modifier at least comprises dimethyl sulfoxide, toluene diisocyanate and dibutyl tin dilaurate.
5. The carbon black nanomaterial of high filtration precision according to claim 1, characterized in that: the dispersing agent is selected from at least one of maleic anhydride, methacrylic acid, styrene sulfonic acid and polyoxyethylene ether.
6. The carbon black nanomaterial of high filtration precision according to claim 1, characterized in that: the solvent includes at least methanol and toluene.
7. A method for producing the carbon black nanomaterial with high filtration accuracy according to any one of claims 1 to 6, comprising the steps of:
s1, adding the nano carbon black and the modifier into a reaction kettle, sealing, vacuumizing, filling nitrogen, and then stirring by magnetic force;
s2, filtering the reacted nano carbon black, repeatedly washing the nano carbon black by a methanol water solution, drying the nano carbon black in vacuum at room temperature, and grinding the nano carbon black to obtain reactive carbon black;
s3, adding a grafting agent and reactive carbon black into a reaction kettle, vacuumizing and filling nitrogen, then heating in a constant-temperature water bath, after the reaction is finished, performing methanol reverse precipitation on a reactant, filtering, and then placing at room temperature for vacuum drying;
s4, adding the dried matter into a Soxhlet extractor, repeatedly extracting the dried matter through methylbenzene, and then drying the product in vacuum at room temperature to obtain modified carbon black;
and S5, adding the modified carbon black, the nano white carbon black, the coupling agent and the dispersing agent into a reaction kettle, mixing, and drying to obtain the carbon black nano material.
8. The method for preparing carbon black nanomaterial of high filtration precision according to claim 7, characterized in that: in the step S1, the number of times of vacuum pumping is 5-7, the magnetic stirring time is 24-30h, the temperature is 25-60 ℃, and in the step S2, the vacuum drying time is 22-26 h.
9. The method for preparing carbon black nanomaterial of high filtration precision according to claim 7, characterized in that: in the step S3, the number of times of vacuum pumping is 5-7 times, and the vacuum drying time is 22-26 h.
10. The method for preparing carbon black nanomaterial of high filtration precision according to claim 7, characterized in that: in the S4, the extraction times are 5-6 times, and the vacuum drying time is 22-26 h.
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Citations (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5952429A (en) * | 1995-06-14 | 1999-09-14 | Nippon Shokubai Co., Ltd. | Carbon black graft polymer, method for production thereof, and use thereof |
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