CN114407266A - Preparation method of carbon black/natural latex composite material - Google Patents
Preparation method of carbon black/natural latex composite material Download PDFInfo
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- CN114407266A CN114407266A CN202210019828.6A CN202210019828A CN114407266A CN 114407266 A CN114407266 A CN 114407266A CN 202210019828 A CN202210019828 A CN 202210019828A CN 114407266 A CN114407266 A CN 114407266A
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- 239000002131 composite material Substances 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 19
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- 229940096992 potassium oleate Drugs 0.000 claims abstract description 25
- MLICVSDCCDDWMD-KVVVOXFISA-M potassium;(z)-octadec-9-enoate Chemical compound [K+].CCCCCCCC\C=C/CCCCCCCC([O-])=O MLICVSDCCDDWMD-KVVVOXFISA-M 0.000 claims abstract description 25
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- MLGZWBPQUONOQV-UHFFFAOYSA-M potassium (Z)-octadec-9-enoate hydrate Chemical compound [OH-].[K+].C(CCCCCCCC=C/CCCCCCCC)(=O)O MLGZWBPQUONOQV-UHFFFAOYSA-M 0.000 claims description 2
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- 229910021536 Zeolite Inorganic materials 0.000 description 5
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 description 5
- 239000010457 zeolite Substances 0.000 description 5
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- 235000021355 Stearic acid Nutrition 0.000 description 3
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- KEQXNNJHMWSZHK-UHFFFAOYSA-L 1,3,2,4$l^{2}-dioxathiaplumbetane 2,2-dioxide Chemical group [Pb+2].[O-]S([O-])(=O)=O KEQXNNJHMWSZHK-UHFFFAOYSA-L 0.000 description 1
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Images
Classifications
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C44/00—Shaping by internal pressure generated in the material, e.g. swelling or foaming ; Producing porous or cellular expanded plastics articles
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C44/00—Shaping by internal pressure generated in the material, e.g. swelling or foaming ; Producing porous or cellular expanded plastics articles
- B29C44/34—Auxiliary operations
- B29C44/3415—Heating or cooling
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C44/00—Shaping by internal pressure generated in the material, e.g. swelling or foaming ; Producing porous or cellular expanded plastics articles
- B29C44/34—Auxiliary operations
- B29C44/3442—Mixing, kneading or conveying the foamable material
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- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Processes Of Treating Macromolecular Substances (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention belongs to the technical field of wet mixing of natural rubber, and relates to a preparation method of a carbon black natural latex composite material, which comprises the steps of firstly, respectively mixing a prepared carbon black aqueous solution and a potassium oleate aqueous solution with foamed natural latex, then, stirring at a high speed to ensure that the natural latex is fully contacted with carbon black, preparing carbon black master batch by a foaming flocculation method, and finally, putting the carbon black master batch into an internal mixer for mixing, wherein the obtained mixed rubber has uniform quality, not only the physical property and the dynamic mechanical property are obviously improved compared with the mixing process of a conventional wet method and a conventional dry method, but also the aging property is greatly improved, simultaneously, the carbon black achieves better dispersion effect in the natural latex, can solve the problems of filler residue and overlarge energy consumption caused by acid flocculation, shorten the vulcanization time, greatly improve the rubber production efficiency and improve the rubber property, the problem of environmental pollution caused by flying of the rubber additive is avoided, and the rubber additive is green, environment-friendly, energy-saving and consumption-reducing.
Description
The technical field is as follows:
the invention belongs to the technical field of wet mixing of natural rubber, and relates to a preparation method of a carbon black/natural latex composite material, which can shorten the production period, realize micro dispersion of a reinforcing filler in the natural rubber and improve the rubber performance.
Background art:
mixing is a process of uniformly mixing rubber and various raw materials, is carried out by an open mill or an internal mixer, is the first step of processing and producing rubber materials, and is also the most important step. The wet mixing is a processing process of uniformly mixing rubber in a latex state with a reinforcing filler dispersion system which is dispersed in advance, uniformly dispersing reinforcing filler particles in the latex system, and forming a rubber and filler composite material through flocculation and coprecipitation.
The traditional mixing method in the rubber industry is an internal mixer multi-section mixing method, but the viscoelasticity of rubber enables the rubber to be heated quickly because of being continuously sheared in the mixing process, and in order to prevent rubber scorching from influencing the safety of rubber processing, the mixing process is very short, so that the dispersion of a rubber auxiliary agent in the rubber is difficult to achieve an ideal state; in order to improve the mixing efficiency, the rubber industry has developed new mixing methods and processes, including low-temperature one-shot methods, tandem mixing, continuous mixing and the like, and although the new mixing techniques can improve the mixing efficiency and quality, the dispersion level of the filler in the rubber compound is still not expected due to the essential characteristics of the rubber, especially for the natural rubber composite prepared by wet mixing.
Carbon black is a typical ingredient in rubber, and can only play a role in uniformly distributing in rubber, so that an elastic network of the rubber can have unique structural properties, but in actual production, the carbon black is difficult to uniformly disperse in the rubber and needs to be realized by a high-shear and high-power mixing mill. The natural latex is a milk white colloid, consists of cis-1, 4-polyisoprene, water, a small amount of protein and phospholipid, has good film forming property, and the solidified raw rubber has good physical properties including high elasticity, high tensile strength and the like, and is widely applied to the fields of medicine and life, and is used for preparing tablet coatings, transdermal agents and condoms, adhesives, carpets, leather boards, various gloves and balloons. Natural rubber is prepared from natural latex through the steps of collection, coagulation, washing, drying and the like, wherein coagulation is an important step in forming natural rubber.
The carbon black master batch in the prior art has the problems of low dispersion degree of reinforcing filler, complicated manufacturing process (including high-energy-consumption mixing), low solidification efficiency when mixing carbon black and latex, and the like. The research finds that: although the wet kneading process can increase the degree of microdispersion of the carbon black filler, the flocculation drying method is often a chemical means such as acid flocculation, and therefore, it affects the performance of the rubber product. For example, chinese patent 201110064299.3 discloses a method for preparing a wet-process mixed natural rubber material, which comprises the following steps: A. the prepared slurry consists of a white carbon black dry material, deionized water, a coupling agent and a surfactant, and the preparation process comprises the following steps: 1) soaking 15-40% of white carbon black dry material in 60-85% of deionized water for 3-6 h; 2) adding a coupling agent accounting for 1-10% of the content of the dry white carbon black and a surfactant accounting for 0.2-5%, and mechanically stirring to uniformly mix the dry white carbon black, the coupling agent and the surfactant to prepare white carbon black slurry; B. grinding the slurry by a grinding machine until the sedimentation amount of the white carbon black aqueous dispersion is less than 80 mg/h; C. preparing latex mixed solution 1), taking field latex of natural rubber with dry rubber content of 15-60% or centrifugally concentrated natural latex; 2) adding the prepared white carbon black aqueous dispersion into latex, and stirring for 20-50 minutes at normal temperature; 3) uniformly mixing latex and the aqueous dispersion of white carbon black to form a latex mixed solution; D. flocculation, glue washing and dehydration 1), adding 0.3-1% acetic acid of the total amount of the mixed solution into the mixed solution after uniform mixing to ensure that the pH value is 3-5, and uniformly flocculating latex and co-precipitating with white carbon black; 2) washing the solidified rubber material with clear water to remove redundant acetic acid, and washing the rubber material with a rubber washing machine to remove rubber and water; 3) feeding the dehydrated rubber material to a rubber granulator for granulation, and then feeding the rubber material granules into a box type drying cabinet for drying at the temperature of 90-120 ℃ for 4-6 h; E. drying completely to obtain a mixed rubber material of the natural rubber; the preparation method of the zeolite rubber composite material disclosed in the Chinese patent 201811575766.7 comprises the following steps: (1) preparing raw materials in parts by mass: NR 100; 3-5 parts of zinc oxide; 1-3 parts of stearic acid; anti-aging agent 4010NA 1; promoter CZ 1-1.5; 2, sulfur; 1-50 parts of zeolite powder; adding zeolite powder into distilled water, stirring uniformly, mixing with natural latex, mechanically stirring uniformly, manually stirring with a glass rod, and slowly adding acetic acid solution to flocculate; (2) pressing and crazing, washing and granulating the flocculated coprecipitation material, and finally dehydrating by an electric heating blast box and drying by a vacuum drying box to constant weight to obtain zeolite/NR wet coprecipitation glue; (3) sequentially adding an anti-aging agent, an accelerator, stearic acid, zinc oxide, zeolite and sulfur into an open mill, and uniformly mixing by adopting a conventional mixing method to prepare a rubber compound; (4) and (3) measuring the positive vulcanization time t of the mixed rubber by using a rubber vulcanization instrument, and vulcanizing and molding the mixed rubber which is placed for 10-12h on a flat vulcanizing machine. The defects existing in the acid flocculation method, which cannot be eliminated, not only can affect the health of operators and corrode equipment, but also acid gas which affects the environment is easily generated after long-time drying after flocculation, if strong acid is not cleaned, the subsequent vulcanization time can also be affected, and the vulcanization time of the rubber material can generate a hysteresis phenomenon in the acid environment, so that over-vulcanization is easily caused, and the performance of rubber products is affected. Therefore, a preparation method of the carbon black natural latex composite material is researched and designed to obtain wet masterbatch with uniformly dispersed carbon black.
The invention content is as follows:
the invention aims to overcome the defects in the prior art, and designs a preparation method of a carbon black natural latex composite material, which improves the dispersion degree of carbon black in rubber and further enables rubber compound to have better performance.
In order to realize the aim, the preparation method of the carbon black/natural latex composite material is a foaming self-flocculation method, and the specific process comprises three steps of preparing a carbon black aqueous solution, preparing a potassium oleate aqueous solution and preparing the carbon black/natural latex composite material:
(1) preparing a carbon black aqueous solution: mixing 60 parts by mass of powdered carbon black with deionized water to prepare a 25 wt% carbon black aqueous solution;
(2) preparation of aqueous potassium oleate solution: mixing 1.5g of potassium oleate with deionized water to prepare a 10 wt% potassium oleate aqueous solution, placing the potassium oleate aqueous solution on a magnetic stirrer with the rotating speed of 20rpm, and stirring for 30min at the temperature of 70 ℃ to fully dissolve the potassium oleate in the deionized water and generate foam;
(3) preparation of carbon black/natural latex composite:
mixing potassium oleate water solution with 166.67 parts by mass of 60 wt% NRL (natural latex), stirring for 5min under the condition of frequency of 10-20HZ, and foaming;
mixing the carbon black aqueous solution with the foamed NRL, and stirring until flocculation is carried out to obtain carbon black masterbatch;
compressing and drying the carbon black masterbatch until the dry rubber level is reached, wherein the drying temperature is 100 ℃, and obtaining the carbon black/natural latex composite material foamed by the potassium oleate.
The carbon blacks to which the present invention relates include N115, N234, cracked carbon blacks and other carbon black materials used in the rubber product and tire industry.
After the carbon black/natural latex composite material is put into an internal mixer, internal mixing is carried out under the conditions that the temperature is 100 ℃ and the rotating speed is 80r/min, and rubber compound can be obtained.
Compared with the prior art, the method has the advantages that the natural latex is foamed through the potassium oleate by utilizing a wet mixing process, so that the aqueous dispersion of the carbon black is fully contacted with the natural latex, the molecular chain of the natural latex can be more dispersed, the wet masterbatch with the uniformly dispersed carbon black can be obtained, the dispersion condition of the carbon black in the rubber is improved, the produced rubber compound has better comprehensive performance, the use of acid is avoided, the pollution generation and the influence of acid residue on the rubber performance are reduced, and the aim of environmental protection is fulfilled; the method mixes the water dispersion of the carbon black with the natural latex subjected to the potassium oleate foaming treatment, has simple process operation, is green and environment-friendly, and solves the problems of large smell, damage to equipment, unstable product quality and the like of the conventional acid flocculation process.
Description of the drawings:
FIG. 1 is a block diagram of the process flow of the present invention.
The specific implementation mode is as follows:
the invention is further illustrated by the following examples in conjunction with the accompanying drawings.
Example 1:
the specific process of the preparation method of the carbon black/natural latex composite material related by the embodiment comprises three steps of preparing carbon black aqueous solution, preparing potassium oleate aqueous solution and preparing the carbon black/natural latex composite material:
(1) preparing a carbon black aqueous solution: filtering and screening the granulated carbon black N115 through an electric sieve with a 100-mesh screen to obtain powder carbon black with smaller particle size; mixing 60 parts by mass of powdered carbon black with deionized water to prepare a 25 wt% carbon black aqueous solution, and manually stirring the mixture by using a stirring rod;
(2) preparation of aqueous potassium oleate solution: mixing 1.5g of potassium oleate with deionized water to prepare 10 wt% of potassium oleate aqueous solution, placing the potassium oleate aqueous solution on a magnetic stirrer with the rotating speed of 20rpm, and stirring for 30min at the temperature of 70 ℃;
(3) preparation of carbon black/natural latex composite:
mixing 15g of potassium oleate aqueous solution with 166.67 parts by mass of 60 wt% NRL (natural latex), and carrying out physical stirring foaming treatment by using a stirrer, wherein the stirring time is 5min, and the rotating speed is 1200 r/min;
mixing the carbon black aqueous solution with the foamed NRL, and stirring until flocculation is carried out to obtain carbon black masterbatch;
compressing and drying the carbon black masterbatch until the dry rubber level is reached, wherein the drying temperature is 100 ℃, and obtaining the carbon black/natural latex composite material foamed by the potassium oleate.
Example 2:
the example relates to the comprehensive performance test of the vulcanized rubber compound of the carbon black/natural latex composite material, wherein the carbon black/natural latex composite material prepared by the conventional wet stirring flocculation method, the conventional dry method and the example 1 (foaming flocculation method) is respectively prepared into the rubber compound, and the specific process comprises the following steps: putting the carbon black/natural latex composite material, 1.06 parts by mass of stearic acid, 3.72 parts by mass of zinc oxide, 1.59 parts by mass of microcrystalline wax, 1.59 parts by mass of 4020 (antioxidant) and 1.59 parts by mass of RD (antioxidant) into an internal mixer, and carrying out internal mixing under the conditions that the temperature is 100 ℃ and the rotating speed is 80r/min to obtain rubber compound; mixing 1.69 parts by mass of S (sulfur) and 1.28 parts by mass of NS (vulcanization accelerator) with the rubber compound on an open mill, and performing thin passing, wherein the rubber compound is obtained by rolling and triangular wrapping for four times respectively;
the mechanical properties and dynamic mechanical properties of the three rubber materials were tested, and the results are shown in the following table:
as can be seen from the above table: compared with the conventional dry method and stirring flocculation T90, the foaming flocculation method is obviously reduced, thereby reducing the energy consumption; the tensile strength, the elongation at break and the tearing strength are obviously improved, which shows that the carbon black/natural latex composite material prepared by the foaming flocculation method can effectively disperse carbon black filler in a rubber matrix and improve the combination of the carbon black and rubber molecular chains, so that more filler-rubber molecular chain network structures are formed by rubber materials, the densification of a cross-linked network structure is caused, and the comprehensive performance is improved; payne effect data show that the carbon black/natural latex composite material prepared by the foaming flocculation method is beneficial to the dispersion of the filler in colloid and the combination of the filler and rubber; DIN abrasion data shows that the carbon black/natural latex composite material prepared by the foaming flocculation method has better filler dispersibility, more attachment points of the filler and a molecular chain and better wear resistance.
Example 3:
the preparation method of the carbon black/natural latex composite material related to the example selects the pelletized carbon black N235, and adopts the specific process of the example 1 to prepare the carbon black/natural latex composite material.
Example 4:
the example relates to the comprehensive performance test of the vulcanized rubber compound of the carbon black/natural latex composite material, wherein the carbon black/natural latex composite material prepared by the conventional wet stirring flocculation method, the conventional dry method and the example 3 (foaming flocculation method) is respectively prepared into the rubber compound, and the specific process is the same as that of the example 1;
the mechanical properties and dynamic mechanical properties of the three rubber materials were tested, and the results are shown in the following table:
| test items | Smoked sheet glue-dry method | Stirring flocculation-wet method | Foaming flocculation method-wet method |
| T10 | 3.01 | 2.35 | 1.7 |
| T90 | 6.95 | 6.65 | 5.53 |
| ML | 2.66 | 2.96 | 1.88 |
| MH | 19.34 | 18.62 | 16.84 |
| Hardness (Shao's A) | 61.5 | 64 | 63 |
| 10% definite elongation (MPa) | 0.82 | 0.88 | 0.91 |
| 100% definite elongation (MPa) | 2.81 | 2.68 | 3.09 |
| 300% definite elongation (MPa) | 13.99 | 12.95 | 14.64 |
| Tensile Strength (MPa) | 23.83 | 22.60 | 25.25 |
| Elongation at Break (%) | 480.77 | 435.03 | 520.69 |
| Tensile product | 11456.75 | 9831.68 | 13147.42 |
| Payne | 1007.95 | 867.92 | 802.88 |
| DIN abrasion | 0.1658 | 0.1616 | 0.1507 |
| Degree of dispersion of carbon black | 6 | 6.3 | 6.9 |
As can be seen from the above table: the MH-ML of the NR sizing material prepared by adopting the foaming self-flocculation method is the largest, the processing performance is better, the MH-ML of the NR sizing material prepared by adopting stirring flocculation is the second, and the MH-ML of the NR sizing material prepared by the conventional dry method is the worst, and the processing performance is the worst;
the NR sizing material prepared by adopting the foaming self-flocculation method has higher definite elongation, tensile strength, elongation at break and tensile product than the NR sizing material prepared by the conventional wet stirring flocculation method and the conventional dry method, and has better comprehensive performance, because the damage effect of the foaming self-flocculation process on a rubber molecular chain is relatively small, the combination of carbon black and the rubber molecular chain can be effectively realized, the reinforcing performance of the sizing material is improved, and a stable filler-rubber molecular chain network structure is formed;
the Payne of the NR rubber material prepared by adopting the foaming self-flocculation method is minimum, which shows that the dispersion of the filler is better combined with a rubber molecular chain, and the physical network structure of the filler and the filler is less, thereby being beneficial to improving the physical property of the rubber material;
DIN abrasion data shows that the carbon black/natural latex composite material prepared by the foaming flocculation method has better filler dispersibility, more attachment points of the filler and a molecular chain and better wear resistance.
Claims (4)
1. A preparation method of a carbon black natural latex composite material is characterized in that the preparation method is a foaming self-flocculation method, and the specific process comprises three steps of preparing a carbon black aqueous solution, preparing a potassium oleate aqueous solution and preparing the carbon black/natural latex composite material:
(1) preparing a carbon black aqueous solution: mixing the powdered carbon black with deionized water to prepare a 25 wt% carbon black aqueous solution;
(2) preparation of aqueous potassium oleate solution: mixing potassium oleate with deionized water to prepare a 10 wt% potassium oleate aqueous solution, and stirring the potassium oleate aqueous solution to fully dissolve the potassium oleate in the deionized water and generate foam;
(3) preparation of carbon black/natural latex composite:
mixing potassium oleate water solution with 60 wt% NRL, stirring at frequency of 10-20Hz for 5min, and foaming;
mixing the carbon black aqueous solution with the foamed NRL, and stirring until flocculation is carried out to obtain carbon black masterbatch;
compressing and drying the carbon black masterbatch until the dry rubber level is reached, wherein the drying temperature is 100 ℃, and obtaining the carbon black/natural latex composite material foamed by the potassium oleate.
2. The method for preparing carbon black natural latex composite according to claim 1, wherein the stirring process involved in the step (2) is to place the aqueous solution of potassium oleate on a magnetic stirrer rotating at 20rpm and stir at 70 ℃ for 30 min.
3. The method of preparing carbon black natural latex composite as claimed in claim 1 or 2, wherein carbon black includes N115, N234, cracked carbon black and other carbon black materials used in the manufacture of rubber products and tire industry.
4. The method of producing a carbon black natural latex composite as claimed in claim 3, wherein the carbon black/natural latex composite is put into an internal mixer, and then internal mixing is carried out at a temperature of 100 ℃ and a rotational speed of 80r/min, thereby obtaining a rubber compound.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202210019828.6A CN114407266A (en) | 2022-01-10 | 2022-01-10 | Preparation method of carbon black/natural latex composite material |
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| CN115073827A (en) * | 2022-08-09 | 2022-09-20 | 青岛科技大学 | Wet preparation method of pyrolysis carbon black/natural rubber composite material |
| CN115970569A (en) * | 2023-03-17 | 2023-04-18 | 青岛黑猫新材料研究院有限公司 | Carbon black intermediate product treatment system and method |
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