CN114574004B - Preparation method of carbon black nano material - Google Patents
Preparation method of carbon black nano material Download PDFInfo
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- CN114574004B CN114574004B CN202210074982.3A CN202210074982A CN114574004B CN 114574004 B CN114574004 B CN 114574004B CN 202210074982 A CN202210074982 A CN 202210074982A CN 114574004 B CN114574004 B CN 114574004B
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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
- C09C1/56—Treatment of carbon black ; Purification
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K9/00—Use of pretreated ingredients
- C08K9/02—Ingredients treated with inorganic substances
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08L9/06—Copolymers with styrene
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- 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
- C09C3/10—Treatment with macromolecular organic compounds
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Abstract
The invention discloses a preparation method of a carbon black nano material, which comprises the following steps: step 1, activating nano carbon black by using alkali liquor to obtain active nano carbon black; step 2, stirring the active nano carbon black by using polyallylamine to obtain polyallylamine/nano carbon black; step 3, dissolving p-anisaldehyde in a lower alcohol solvent to obtain a p-anisaldehyde solution; and 4, reacting the p-anisaldehyde solution with polyallylamine/nano carbon black to obtain p-anisyl piperonyl schiff base/nano carbon black, namely the carbon black nano material. The material is prepared by modifying and activating the nano carbon black by using a reaction product of polyallylamine and p-anisaldehyde, so that the obtained nano carbon black material has better dispersibility and antibacterial activity, and the mechanical property and the antibacterial property of the rubber material can be better improved after the nano carbon black material is applied to the rubber material.
Description
Technical Field
The invention relates to the field of nano materials, in particular to a preparation method of a carbon black nano material.
Background
According to research reports, carbon black materials for rubber products and ink production always occupy the front of requirements of nano materials, the carbon black nano materials have certain reinforcing effect in a rubber matrix due to unique nano size effect and higher surface activity, but the dispersion performance of the carbon black nano materials in the rubber matrix is poor due to the strong agglomeration effect between the carbon black material bodies, poor interface compatibility with rubber macromolecules and the like, and the exertion of the reinforcing performance of the carbon black nano materials is greatly influenced. In addition, the existing rubber materials have poor antibacterial activity, and the added antibacterial ingredients are often used for a period of time, so that the antibacterial effect is seriously reduced, and therefore, an additive capable of inhibiting bacteria for a long time is needed.
Disclosure of Invention
Aiming at the problems in the prior art, the invention aims to provide a preparation method of a carbon black nano material with good dispersibility, good antibacterial activity and good rubber mechanical property improvement effect.
The purpose of the invention is realized by adopting the following technical scheme:
in a first aspect, the present invention provides a method for preparing a carbon black nanomaterial, comprising the steps of:
step 1, activating nano carbon black by using alkali liquor to obtain active nano carbon black;
step 2, stirring the active nano carbon black by using polyallylamine to obtain polyallylamine/nano carbon black;
step 3, dissolving p-anisaldehyde in a lower alcohol solvent to obtain a p-anisaldehyde solution;
and 4, reacting the p-anisaldehyde solution with polyallylamine/nano carbon black to obtain p-anisyl piperonyl schiff base/nano carbon black, namely the carbon black nano material.
Preferably, in the step 1, the type of the nano carbon black is Vulcan XC-72, and the particle size of the nano carbon black is 600-800 nm.
Preferably, in the step 1, the alkali liquor is one of a NaOH solution, a KOH solution and ammonia water, and the mass fraction of the alkali liquor is 5% -10%.
Preferably, in the step 1, the mass ratio of the nano carbon black to the alkali liquor is 1.
Preferably, in the step 1, the temperature of the activation treatment is 50-60 ℃ and the time is 2-4 h.
Preferably, in the step 2, the polyallylamine is dissolved in the anhydrous ethanol and then mixed with the active nano carbon black, wherein the mass ratio of the polyallylamine to the anhydrous ethanol is 1.2-1.6, 20-30, and the mass ratio of the active nano carbon black to the polyallylamine is 1.
Preferably, in the step 2, the temperature of the stirring treatment is room temperature, and the time is 8-12 h.
Preferably, in the step 3, the lower alcohol solvent comprises one of ethanol, n-propanol and isopropanol.
Preferably, in the step 3, the mass ratio of the p-anisaldehyde to the lower alcohol solvent is 0.15-0.2.
Preferably, in the step 4, the polyallylamine/nanocarbon is firstly dispersed uniformly in absolute ethyl alcohol to form a polyallylamine/nanocarbon solution, and then the solution reacts with the p-anisaldehyde solution, wherein the mass ratio of the polyallylamine/nanocarbon to the absolute ethyl alcohol is 1.
Preferably, in the step 4, the mass ratio of the polyallylamine/the nanocarbon to the p-anisaldehyde in the p-anisaldehyde solution is 1.
Preferably, in the step 4, the polyallylamine/nanocarbon solution is placed in an ice water bath condition and uniformly mixed, glacial acetic acid is added dropwise, the p-anisaldehyde solution is added dropwise, and after the dropwise addition is continuously completed, the temperature is gradually increased to the reflux temperature for continuous reaction.
Preferably, in the step 4, the reaction is continued for 2 to 4 hours after the temperature is raised to the reflux temperature.
In a second aspect, the present invention provides a carbon black nanomaterial for use in rubber products.
The invention has the beneficial effects that:
1. the invention discloses a carbon black nano material, which is prepared by modifying and activating nano carbon black by using a reaction product of polyallylamine and p-anisaldehyde, so that the obtained nano carbon black material has better dispersibility and antibacterial activity when being applied, and the mechanical property and the antibacterial property of a rubber material can be better improved after the nano carbon black material is applied to the rubber material.
2. According to the invention, firstly, the polymer polyallylamine is adsorbed and fixed on the surface and in the pore diameter of the carbon black, then, a Schiff base structure (Schiff base) is generated by utilizing the condensation reaction of amino in the polyallylamine and aldehyde group in p-anisaldehyde, so that the p-anisaldehyde is grafted on the polyallylamine, and meanwhile, the polymer polyallylamine has strong fixity and can be well fixed on the surface of the carbon black material.
3. In addition, although the carbon black material has a certain pore diameter and a certain adsorption property, and has a certain binding property to polyallylamine, in order to enhance the fixing effect of the carbon black material to polyallylamine, the invention carries out alkali liquor activation treatment on the nano carbon black in advance, and abundant hydroxyl groups are adsorbed on the surface and in the pore diameter of the activated nano carbon black, and the hydroxyl groups are easier to form hydrogen bonding action with amino groups in the polyallylamine, thereby enhancing the fixing effect.
Drawings
The invention is further illustrated by means of the attached drawings, but the embodiments in the drawings do not constitute any limitation to the invention, and for a person skilled in the art, other drawings can be obtained on the basis of the following drawings without inventive effort.
FIG. 1 is an SEM image of a carbon black nanomaterial prepared in example 1 of the present invention.
Detailed Description
For the purpose of more clearly illustrating the present invention and more clearly understanding the technical features, objects and advantages of the present invention, the technical solutions of the present invention will now be described in detail below, but the present invention should not be construed as being limited to the implementable scope of the present invention.
The polyallylamine used in the invention is a polymer molecule containing a large amount of polar amino groups, has good immobilization and adsorption, and is generally used in water treatment and textile color fixing industries. The invention is used for modifying carbon black materials, and is further used in rubber materials. In the case of carbon black nano-modification, it has been found that, although dispersibility is improved by combining polyallylamine with nano-carbon black, the water resistance of the product is poor because polyallylamine itself has high water solubility, and further improvement is desired. The molecular structure of polyallylamine is as follows:
the p-anisaldehyde used in the invention is extracted from natural plants, mainly exists in plants such as fennel, star anise, vanilla bean and the like, is in a liquid state at normal temperature, has good antibacterial and bacteriostatic effects, emits the faint scent of the fennel, and is generally used for manufacturing spices or medical products. The invention utilizes the condensation reaction of the aldehyde group and the amino group in the polyallylamine, so that the p-anisaldehyde is connected to the nano carbon black through the generated Schiff base structure, and the generated condensation compound has more active groups, so that the rubber material has better crosslinking property and fusion property, and the p-anisaldehyde also has better antibacterial activity. The molecular structural formula of p-anisaldehyde is as follows:
the condensation reaction of polyallylamine with p-anisaldehyde is given by the equation:
the invention is further described below with reference to the following examples.
Example 1
A preparation method of carbon black nano material comprises the following steps:
step 1, weighing nano carbon black with the model of Vulcan XC-72 and the particle size of 600-800 nm, ultrasonically dispersing the nano carbon black in a NaOH solution with the mass fraction of 5%, wherein the mass ratio of the nano carbon black to the NaOH solution is 1;
step 2, dissolving polyallylamine in absolute ethyl alcohol, wherein the mass ratio of the polyallylamine to the absolute ethyl alcohol is 1.4;
step 3, weighing p-anisic aldehyde, dissolving the p-anisic aldehyde in absolute ethyl alcohol, wherein the mass ratio of the p-anisic aldehyde to the absolute ethyl alcohol is 0.18;
and 4, dispersing the polyallylamine/the nano carbon black into absolute ethyl alcohol, wherein the mass ratio of the polyallylamine/the nano carbon to the absolute ethyl alcohol is 1.
Example 2
A preparation method of carbon black nano material comprises the following steps:
step 1, weighing nanometer carbon black with the model of Vulcan XC-72 and the particle size of 600-800 nm, ultrasonically dispersing the nanometer carbon black in a KOH solution with the mass fraction of 5%, wherein the mass ratio of the nanometer carbon black to the KOH solution is 1;
step 2, dissolving polyallylamine in absolute ethyl alcohol, wherein the mass ratio of the polyallylamine to the absolute ethyl alcohol is 1.2;
step 3, weighing p-anisic aldehyde, dissolving the p-anisic aldehyde in n-propanol, wherein the mass ratio of the p-anisic aldehyde to the n-propanol is 0.15;
and 4, dispersing the polyallylamine/the nano carbon black into absolute ethyl alcohol, wherein the mass ratio of the polyallylamine/the nano carbon to the absolute ethyl alcohol is 1.
Example 3
A preparation method of carbon black nano material comprises the following steps:
step 1, weighing nano carbon black with the model of Vulcan XC-72 and the particle size of 600-800 nm, ultrasonically dispersing the nano carbon black into ammonia water with the mass fraction of 10%, wherein the mass ratio of the nano carbon black to the ammonia water is 1;
step 2, dissolving polyallylamine in absolute ethyl alcohol, wherein the mass ratio of the polyallylamine to the absolute ethyl alcohol is 1.6, slowly adding active nano carbon black, the mass ratio of the active nano carbon black to the polyallylamine is 1.35, stirring at room temperature for 12h, and carrying out vacuum drying on filter residues obtained by reduced pressure filtration to obtain the polyallylamine/nano carbon black;
step 3, weighing p-anisic aldehyde, dissolving the p-anisic aldehyde in isopropanol, wherein the mass ratio of the p-anisic aldehyde to the isopropanol is 0.2;
and 4, dispersing the polyallylamine/the nano carbon black into absolute ethyl alcohol, wherein the mass ratio of the polyallylamine/the nano carbon to the absolute ethyl alcohol is 1.
Comparative example 1
A carbon black nano material is prepared by the same method as the example 1, except that no p-anisaldehyde reaction is added, namely, the step 3 and the step 4 are omitted, and the finally obtained carbon black nano material is polyallylamine/nano carbon black.
Comparative example 2
The carbon black nano material sold in the market is Vulcan XC-72 and has the grain diameter of 600-800 nm.
In order to more clearly illustrate the present invention, the carbon black nanomaterials prepared in example 1, comparative example 1 and comparative example 2 were applied to a rubber material, thereby examining the enhancing effect on the rubber material.
The rubber material comprises the following components in parts by weight: 80 parts of styrene butadiene rubber, 25 parts of butadiene rubber, 30 parts of carbon black nano material, 3 parts of sulfur, 2.7 parts of sulfonamide accelerator, 2.2 parts of amine antioxidant, 5.2 parts of stearic acid and 4.5 parts of nano zinc oxide. Wherein the carbon black nanomaterials are the carbon black nanomaterials prepared in example 1, comparative example 1 and comparative example 2, respectively.
The preparation method of the rubber material comprises the following steps:
(1) Mixing styrene butadiene rubber, butadiene rubber and carbon black nano materials in a double-roll open mill, and mixing for 5min at the temperature of 150 ℃, wherein the rubber discharging temperature is 150 ℃;
(2) Adding amine anti-aging agent, stearic acid and nano zinc oxide, and continuously mixing for 2min at the rubber discharging temperature of 150 ℃;
(3) Adding sulfur and sulfonamide accelerator, and mixing for 3min at 100 deg.C.
(4) The prepared rubber materials are respectively marked as example 1, comparative example 1 and comparative example 2, and corresponding performance tests are carried out.
And (3) detection standard: the tensile strength and the elongation at break are referred to GB/T528-2009, the Shore A hardness is referred to GB/T531.1-2008, the tearing strength is referred to GB/T529-2008, and the bacterial inhibition is referred to ISO22196:2007.
The results are shown in the following table:
finally, it should be noted that the above embodiments are only used for illustrating the technical solutions of the present invention, and not for limiting the protection scope of the present invention, although the present invention is described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions can be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention.
Claims (8)
1. A preparation method of carbon black nano material is characterized by comprising the following steps:
step 1, activating nano carbon black by using alkali liquor to obtain active nano carbon black;
step 2, stirring the active nano carbon black by using polyallylamine to obtain polyallylamine/nano carbon black;
step 3, dissolving p-anisaldehyde in a lower alcohol solvent to obtain a p-anisaldehyde solution;
step 4, reacting the p-anisic aldehyde solution with polyallylamine/nano carbon black to obtain p-anisyl piperonyl schiff base/nano carbon black, namely a carbon black nano material;
in the step 2, the polyallylamine is dissolved in absolute ethyl alcohol and then mixed with the active nano carbon black, wherein the mass ratio of the polyallylamine to the absolute ethyl alcohol is 1.2 to 1.6, and the mass ratio of the active nano carbon black to the polyallylamine is 1; the stirring temperature is room temperature, and the stirring time is 8 to 12h;
in the step 4, the mass ratio of the polyallylamine/the nano carbon black to the p-anisaldehyde in the p-anisaldehyde solution is 1 to 0.18 to 0.32.
2. The method for preparing the carbon black nano material according to the claim 1, wherein in the step 1, the type of the nano carbon black is Vulcan XC-72, and the particle size of the nano carbon black is 600 to 800nm.
3. The method for preparing the carbon black nano material according to the claim 1, wherein in the step 1, the alkali solution is one of NaOH solution, KOH solution and ammonia water, and the mass fraction of the alkali solution is 5% -10%.
4. The method for preparing the carbon black nano material according to claim 1, wherein in the step 1, the mass ratio of the nano carbon black to the alkali liquor is 1; the temperature of the activation treatment is 50 to 60 ℃, and the time is 2 to 4 hours.
5. The method for preparing carbon black nano-material according to claim 1, wherein in the step 3, the lower alcohol solvent comprises one of ethanol, n-propanol and isopropanol.
6. The method for preparing the carbon black nanomaterial according to claim 1, wherein in the step 3, the mass ratio of p-anisaldehyde to lower alcohol solvent is 0.15 to 0.2.
7. The method for preparing the carbon black nanomaterial according to claim 1, wherein in the step 4, the polyallylamine/the nano carbon black is uniformly dispersed in the absolute ethyl alcohol to form a polyallylamine/the nano carbon black solution, and then the solution is reacted with the p-anisaldehyde solution, wherein the mass ratio of the polyallylamine/the nano carbon black to the absolute ethyl alcohol is 1 to 6-10.
8. The method for preparing carbon black nano-material according to claim 7, wherein in the step 4, the polyallylamine/nano-carbon black solution is uniformly mixed under the condition of ice-water bath, glacial acetic acid is added dropwise, p-anisaldehyde solution is added dropwise, and after the continuous addition, the temperature is gradually raised to the reflux temperature to continue the reaction.
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