CN114836059A - Low-odor carbon black composite filler and preparation method thereof - Google Patents
Low-odor carbon black composite filler and preparation method thereof Download PDFInfo
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
- C09C3/04—Physical treatment, e.g. grinding, treatment with ultrasonic vibrations
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
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- C09C3/00—Treatment in general of inorganic materials, other than fibrous fillers, to enhance their pigmenting or filling properties
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- C09C3/08—Treatment with low-molecular-weight non-polymer organic compounds
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Abstract
The invention discloses a low-odor carbon black composite filler and a preparation method thereof, and the preparation method comprises the following steps: (1) soaking the waste tire cracking carbon black in acid liquor for activation treatment to obtain activated cracking carbon black; (2) mixing the activated pyrolysis carbon black with a nano molecular sieve, uniformly ball-milling, and then carrying out microwave treatment to obtain a pyrolysis carbon black composite material; (3) and uniformly mixing the cracking carbon black composite material with the cardanol sulfonate intercalated hydrotalcite dispersion liquid, and drying to obtain the low-odor carbon black composite filler. The carbon black composite filler has low odor and excellent reinforcing performance, is suitable for being used in industries such as sealing strips, sealing elements and the like with higher odor requirements, and can widen the application range of waste tire cracking carbon black.
Description
Technical Field
The invention relates to the technical field of rubber materials, in particular to a low-odor carbon black composite filler and a preparation method thereof.
Background
With the continuous development of the automobile industry, a large amount of waste tires are generated every year under the influence of the service life of automobile tires and the updating of products, and how to properly treat the waste tires becomes an important environmental problem and a social problem. One recycling method of the waste tires is to crack the waste tires, and the main product of cracking is cracking carbon black which accounts for about 30-35% of all cracking products. These waste tire cracking carbon blacks can enhance the strength, durability and coloring properties of rubber and are therefore generally used as reinforcing agents for rubber. However, the raw materials in the waste tires are complex, so that the components of the cracked carbon black are complex, and the components with bad odor such as polycyclic aromatic hydrocarbon with high content exist, so that the components can only be applied to the fields of low-end products such as tires and adhesive tapes with low odor requirements, and cannot be used in industries such as sealing strips and sealing elements with high odor requirements, and the reinforcing performance of the components is far inferior to that of commercial carbon black. In order to better apply the waste tire cracking carbon black to the rubber field, especially the high-end rubber product field, the waste tire cracking carbon black composite filler with better reinforcing effect and low odor needs to be developed.
Disclosure of Invention
The invention aims to make up the defects of the prior art and provides a low-odor carbon black composite filler and a preparation method thereof.
The invention is realized by the following technical scheme:
a preparation method of a low-odor carbon black composite filler comprises the following steps:
(1) soaking the waste tire cracking carbon black in acid liquor for activation treatment to obtain activated cracking carbon black;
(2) mixing the activated pyrolysis carbon black with a nano molecular sieve, uniformly ball-milling, and then carrying out microwave treatment to obtain a pyrolysis carbon black composite material;
(3) and uniformly mixing the cracking carbon black composite material with the cardanol sulfonate intercalated hydrotalcite dispersion liquid, and drying to obtain the low-odor carbon black composite filler.
Preferably, in the step (1), the acid solution is one or more aqueous solutions of hydrochloric acid, sulfuric acid and nitric acid, and the concentration of the acid solution is 1-3 mol/L.
Preferably, in the step (1), the temperature of the activation treatment is 30-50 ℃ and the time is 2-5 h.
Preferably, in the step (2), the weight ratio of the activated carbon black to the nano molecular sieve is 1: (0.1-0.25); the nano molecular sieve is a nano ZSM-5 molecular sieve.
Preferably, in the step (2), the rotation speed of the ball milling is 100-; in the step (2), the power of the microwave treatment is 300-500W, and the time is 20-60 s.
Preferably, in the step (3), the mass ratio of the cracking carbon black composite material to the cardanol sulfonate intercalated hydrotalcite dispersion liquid is 1: (10-20).
Preferably, in the step (3), the preparation method of the cardanol sulfonate intercalated hydrotalcite dispersion liquid comprises the following steps: dissolving anacardol sulfonate in water, adding magnesium-aluminum hydrotalcite to disperse uniformly, heating and stirring to react to obtain the anacardol sulfonate.
Preferably, the mass ratio of the cardanol sulfonate to the magnesium-aluminum hydrotalcite is (0.1-0.2): 1, the mass ratio of the cardanol sulfonate to water is (0.1-0.2): 10.
in the present invention, the cardanol sulfonate can be prepared by a conventional method, for example:
dissolving cardanol in dichloromethane, dropwise adding chlorosulfonic acid at 0-4 ℃, reacting at 20-30 ℃ for 2-4h after dropwise adding, then adding ethanol, adjusting the pH to 7-8 with NaOH aqueous solution, continuing to react at 20-30 ℃ for 2-4h, filtering to remove inorganic salt, and then distilling under reduced pressure to remove the solvent to obtain the cardanol-containing water-soluble organic solvent. Preferably, the weight ratio of cardanol to chlorosulfonic acid is 1: (1-2).
In the invention, the magnesium-aluminum hydrotalcite can be prepared by a conventional method such as a coprecipitation method, and the specific method can be as follows:
dissolving magnesium chloride and aluminum chloride in water to obtain Mg 2+ The concentration is 0.1-0.4mol/L, Al 3+ Mixing the solution with the concentration of 0.1-0.2mol/L, adjusting the pH to 10-11 by using NaOH aqueous solution, firstly stirring and reacting for 20-40min, then standing for 1-2h, filtering, washing and drying to obtain the catalyst.
Preferably, the pH value of the heating stirring reaction is 5-6, the temperature is 60-80 ℃, and the time is 2-4 h.
A low-odor carbon black composite filler is prepared by the preparation method.
The invention has the advantages that:
the invention takes waste tire cracking carbon black as a raw material, the waste tire cracking carbon black is activated firstly, the activated waste tire cracking carbon black and a nano molecular sieve are subjected to ball milling and microwave treatment to form a carbon black-nano molecular sieve compound, then a cardanol sulfonate magnesium aluminum hydrotalcite coating layer is coated on the basis of the carbon black-nano molecular sieve compound, the volatilization of smell can be blocked through the blocking effect, the odor can be obviously reduced by the synergistic effect with the adsorption effect of the nano molecular sieve, and the cardanol sulfonate intercalated magnesium aluminum hydrotalcite coating layer is coated, so that the combination of the hydrotalcite, the carbon black and a rubber matrix can be firmer by utilizing the active groups of cardanol, such as phenolic hydroxyl and the like, the blocking effect and the odor reducing synergistic effect of a molecular sieve adsorbent can be better exerted, the smell of the rubber material can be obviously improved, and the reinforcing effect of the mechanical property of the rubber can be improved simultaneously, the carbon black composite filler has low odor and excellent reinforcing performance, can meet the requirements of high odor and high mechanical performance for manufacturing high-end rubber products, and particularly meets the manufacturing and using requirements of sealing strips and sealing elements.
Detailed Description
Example 1
A preparation method of a low-odor carbon black composite filler comprises the following steps:
(1) soaking the waste tire cracking carbon black in a hydrochloric acid aqueous solution with the concentration of 1mol/L, and performing activation treatment for 2 hours at the temperature of 30 ℃ to obtain activated cracking carbon black;
(2) mixing the activated pyrolysis carbon black and a nano ZSM-5 molecular sieve in a weight ratio of 1: 0.1, uniformly ball-milling, wherein the rotating speed of ball milling is 100r/min, the ball milling time is 5h, and then performing microwave treatment, wherein the power of the microwave treatment is 300W, and the time is 20s to obtain the cracking carbon black composite material;
(3) the cracking carbon black composite material and the cardanol sulfonate intercalated hydrotalcite dispersion liquid are mixed according to the mass ratio of 1: 10, and drying to obtain the low-odor carbon blackThe preparation method of the cardanol sulfonate intercalated hydrotalcite dispersion liquid comprises the following steps: dissolving 0.15g of cardanol sulfonate in 10g of water, then adding 1g of magnesium-aluminum hydrotalcite to disperse uniformly, and heating and stirring for reaction for 3 hours under the conditions that the pH value is 5 and the temperature is 70 ℃, wherein the preparation method of the cardanol sulfonate comprises the following steps: dissolving 1g of cardanol in 5mL of dichloromethane, dropwise adding 1g of chlorosulfonic acid at 0 ℃, reacting for 3h at 25 ℃ after dropwise adding, then adding ethanol, adjusting the pH to 7 with NaOH aqueous solution, continuing to react for 3h at 25 ℃, filtering to remove inorganic salts, and then distilling under reduced pressure to remove the solvent to obtain the cardanol-containing water-soluble cardanol hydrochloride; the magnesium-aluminum hydrotalcite is prepared by a coprecipitation method, and the method comprises the following steps: dissolving magnesium chloride and aluminum chloride in water to obtain Mg 2+ The concentration is 0.3mol/L, Al 3+ And (3) adjusting the pH value to 10 by using a NaOH aqueous solution, stirring for reacting for 30min, standing for 1.5h, filtering, washing and drying to obtain the aqueous solution with the concentration of 0.1 mol/L.
Example 2
A preparation method of a low-odor carbon black composite filler comprises the following steps:
(1) soaking the waste tire cracking carbon black in a hydrochloric acid aqueous solution with the concentration of 1mol/L, and performing activation treatment for 5 hours at the temperature of 50 ℃ to obtain activated cracking carbon black;
(2) mixing the activated pyrolysis carbon black and a nano ZSM-5 molecular sieve in a weight ratio of 1: 0.25, uniformly ball-milling, wherein the rotating speed of the ball-milling is 300r/min, the ball-milling time is 10h, and then carrying out microwave treatment, wherein the power of the microwave treatment is 500W, and the time is 60s to obtain the cracking carbon black composite material;
(3) the cracking carbon black composite material and the cardanol sulfonate intercalated hydrotalcite dispersion liquid are mixed according to the mass ratio of 1: 20, uniformly mixing, and drying to obtain the low-odor carbon black composite filler, wherein the preparation method of the cardanol sulfonate intercalated hydrotalcite dispersion liquid comprises the following steps: dissolving 0.15g of cardanol sulfonate in 10g of water, then adding 1g of magnesium-aluminum hydrotalcite to disperse uniformly, and heating and stirring for reaction for 3 hours under the conditions that the pH value is 5 and the temperature is 70 ℃, wherein the preparation method of the cardanol sulfonate comprises the following steps: dissolving 1g cardanol in 5mL dichloromethane, dripping 1g chlorosulfonic acid at 0 ℃, and dripping offAfter the reaction is finished, reacting at 25 ℃ for 3h, then adding ethanol, adjusting the pH to 7 by using NaOH aqueous solution, continuing to react at 25 ℃ for 3h, filtering to remove inorganic salt, and then distilling under reduced pressure to remove the solvent to obtain the compound; the magnesium-aluminum hydrotalcite is prepared by a coprecipitation method, and the specific method comprises the following steps: dissolving magnesium chloride and aluminum chloride in water to obtain Mg 2+ The concentration is 0.3mol/L, Al 3+ And (3) adjusting the pH value to 10 by using a NaOH aqueous solution, stirring for reacting for 30min, standing for 1.5h, filtering, washing and drying to obtain the aqueous solution with the concentration of 0.1 mol/L.
Example 3
A preparation method of a low-odor carbon black composite filler comprises the following steps:
(1) soaking the waste tire cracking carbon black in a hydrochloric acid aqueous solution with the concentration of 1mol/L, and performing activation treatment for 3 hours at the temperature of 40 ℃ to obtain activated cracking carbon black;
(2) mixing the activated pyrolysis carbon black and a nano ZSM-5 molecular sieve in a weight ratio of 1: 0.2, uniformly ball-milling at a ball-milling rotation speed of 200r/min for 8h, and then performing microwave treatment at a microwave treatment power of 400W for 30s to obtain a cracking carbon black composite material;
(3) the cracking carbon black composite material and the cardanol sulfonate intercalated hydrotalcite dispersion liquid are mixed according to the mass ratio of 1: 15, uniformly mixing, and drying to obtain the low-odor carbon black composite filler, wherein the preparation method of the cardanol sulfonate intercalated hydrotalcite dispersion liquid comprises the following steps: dissolving 0.15g of cardanol sulfonate in 10g of water, then adding 1g of magnesium-aluminum hydrotalcite to disperse uniformly, and heating and stirring for reaction for 3 hours under the conditions that the pH value is 5 and the temperature is 70 ℃, wherein the preparation method of the cardanol sulfonate comprises the following steps: dissolving 1g of cardanol in 5mL of dichloromethane, dropwise adding 1g of chlorosulfonic acid at 0 ℃, reacting for 3h at 25 ℃ after dropwise adding, then adding ethanol, adjusting the pH to 7 with NaOH aqueous solution, continuing to react for 3h at 25 ℃, filtering to remove inorganic salts, and then distilling under reduced pressure to remove the solvent to obtain the cardanol-containing water-soluble cardanol hydrochloride; the magnesium-aluminum hydrotalcite is prepared by a coprecipitation method, and the specific method comprises the following steps: dissolving magnesium chloride and aluminum chloride in water to obtain Mg 2+ The concentration is 0.3mol/L, Al 3+ Mixing the solution with the concentration of 0.1mol/L, and thenAdjusting pH to 10 with NaOH water solution, stirring for reaction for 30min, standing for 1.5h, filtering, washing, and drying.
Comparative example 1
A preparation method of a cracking carbon black composite filler comprises the following steps:
(1) soaking the waste tire cracking carbon black in a hydrochloric acid aqueous solution with the concentration of 1mol/L, and performing activation treatment for 3 hours at the temperature of 40 ℃ to obtain activated cracking carbon black;
(2) mixing the activated pyrolysis carbon black and a nano ZSM-5 molecular sieve in a weight ratio of 1: 0.2, uniformly ball-milling at a rotation speed of 200r/min for 8h, and then performing microwave treatment at a power of 400W for 30s to obtain the cracking carbon black composite filler.
Comparative example 2
A preparation method of carbon black composite filler comprises the following steps:
(1) soaking the waste tire cracking carbon black in a hydrochloric acid aqueous solution with the concentration of 1mol/L, and performing activation treatment for 3 hours at the temperature of 40 ℃ to obtain activated cracking carbon black;
(2) mixing the activated pyrolysis carbon black and a nano ZSM-5 molecular sieve in a weight ratio of 1: 0.2, uniformly ball-milling at a ball-milling rotation speed of 200r/min for 8h, and then performing microwave treatment at a microwave treatment power of 400W for 30s to obtain a cracking carbon black composite material;
(3) mixing a cracking carbon black composite material and a hydrotalcite dispersion liquid according to the mass ratio of 1: 15, uniformly mixing, and drying to obtain the low-odor carbon black composite filler, wherein the preparation method of the hydrotalcite dispersion liquid comprises the following steps: uniformly dispersing 1g of magnesium-aluminum hydrotalcite in 10g of water to obtain the magnesium-aluminum hydrotalcite, wherein the magnesium-aluminum hydrotalcite is prepared by a coprecipitation method, and the specific method comprises the following steps: dissolving magnesium chloride and aluminum chloride in water to obtain Mg 2+ The concentration is 0.3mol/L, Al 3+ And (3) adjusting the pH value to 10 by using a NaOH aqueous solution, stirring for reacting for 30min, standing for 1.5h, filtering, washing and drying to obtain the aqueous solution with the concentration of 0.1 mol/L.
Test examples
The carbon black composite filler prepared in example 3 and comparative examples 1-2 and untreated waste tire cracking carbon black are used for preparing rubber, wherein the formula of the rubber comprises the following components in parts by weight: 100 parts of SMR20 rubber, 3 parts of stearic acid, 5 parts of zinc oxide, 0.6 part of accelerator DM, 2.5 parts of sulfur and 50 parts of carbon black composite filler (or untreated waste tire cracking carbon black). The properties of the finished rubber were tested, wherein the odor rating test was referenced to the VDA270 standard and test method. The test results are shown in table 1:
TABLE 1
Note: the odor rating evaluation criteria were as follows: 1 no odour; 2 feeling unknown as smell; 3 the smell can be felt very weakly, also know what; 4 a strong smell is easily felt; 5 very strong odor; 6 feeling dyspnea, strong smell hardly tolerated.
As can be seen from table 1, in comparative example 1, only the activated waste tire cracking carbon black and the nano molecular sieve are subjected to ball milling and microwave treatment to form a carbon black-nano molecular sieve composite, the odor is reduced only through the adsorption effect, the reduction range of the odor is not large, and the nano molecular sieve occupies part of active sites on the surface of the carbon black to block the combination of the carbon black and the rubber matrix, so that the reinforcing effect of the composite material on the rubber material is not obviously improved though the composite material is subjected to acid leaching, activation and other treatments; comparative example 2 is based on the carbon black-nano molecular sieve composite, the magnesium aluminum hydrotalcite coating layer is coated, volatilization of smell can be hindered through the barrier effect, the smell can be obviously reduced by the synergistic effect with the adsorption effect of the nano molecular sieve, but the hydrotalcite, the rubber matrix and the carbon black have low bonding force, slight smell is still left, the effect is not ideal enough, and the enhancement effect on the rubber material is limited; and embodiment 3 has wrapped the coating of cardanol sulfonate intercalation magnalium hydrotalcite on the basis of carbon black-nanometer molecular sieve complex, utilize the active group such as phenolic hydroxyl group of cardanol, make hydrotalcite and carbon black, rubber matrix combine more firmly, also can disperse in rubber matrix better, give play to its separation effect and improve the reinforcement effect of the mechanical property of rubber better, thus show the smell that improves the rubber material, give play to better reinforcement effect at the same time, can satisfy the smell and require higher, the user demand of the sealing strip, sealing member to the mechanical property requirement at the same time.
Claims (10)
1. A preparation method of a low-odor carbon black composite filler is characterized by comprising the following steps:
(1) soaking the waste tire cracking carbon black in acid liquor for activation treatment to obtain activated cracking carbon black;
(2) mixing the activated pyrolysis carbon black with a nano molecular sieve, uniformly ball-milling, and then carrying out microwave treatment to obtain a pyrolysis carbon black composite material;
(3) and uniformly mixing the cracking carbon black composite material with the cardanol sulfonate intercalated hydrotalcite dispersion liquid, and drying to obtain the low-odor carbon black composite filler.
2. The method for preparing a low-odor carbon black composite filler according to claim 1, wherein in the step (1), the acid solution is an aqueous solution of one or more of hydrochloric acid, sulfuric acid and nitric acid, and the concentration of the acid solution is 1-3 mol/L.
3. The method for preparing a low-odor carbon black composite filler according to claim 1, wherein the activation treatment in the step (1) is carried out at a temperature of 30 to 50 ℃ for 2 to 5 hours.
4. The method for preparing a low-odor carbon black composite filler according to claim 1, wherein in the step (2), the weight ratio of the activated pyrolysis carbon black to the nano molecular sieve is 1: (0.1-0.25); the nano molecular sieve is a nano ZSM-5 molecular sieve.
5. The method for preparing a low-odor carbon black composite filler as claimed in claim 1, wherein in the step (2), the rotation speed of the ball milling is 100-300r/min, and the ball milling time is 5-10 h; in the step (2), the power of the microwave treatment is 300-500W, and the time is 20-60 s.
6. The method for preparing a low-odor carbon black composite filler according to claim 1, wherein in the step (3), the mass ratio of the cracking carbon black composite material to the cardanol sulfonate intercalated hydrotalcite dispersion liquid is 1: (10-20).
7. The method for preparing a low-odor carbon black composite filler according to claim 1, wherein in the step (3), the method for preparing the cardanol sulfonate intercalated hydrotalcite dispersion liquid comprises: dissolving anacardol sulfonate in water, adding magnesium-aluminum hydrotalcite to disperse uniformly, heating and stirring to react to obtain the anacardol sulfonate.
8. The method for preparing a low-odor carbon black composite filler according to claim 7, wherein the mass ratio of the cardanol sulfonate to the magnesium-aluminum hydrotalcite is (0.1-0.2): 1, the mass ratio of the cardanol sulfonate to water is (0.1-0.2): 10.
9. the method for preparing a low-odor carbon black composite filler according to claim 7, wherein the heating and stirring reaction is carried out at a pH of 5 to 6, a temperature of 60 to 80 ℃ and a time of 2 to 4 hours.
10. A low odor carbon black composite filler, characterized by being produced by the production method according to any one of claims 1 to 9.
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