CN115449237A - High-dispersity dry granulation regenerated carbon black and preparation method thereof - Google Patents
High-dispersity dry granulation regenerated carbon black and preparation method thereof Download PDFInfo
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- CN115449237A CN115449237A CN202211189952.3A CN202211189952A CN115449237A CN 115449237 A CN115449237 A CN 115449237A CN 202211189952 A CN202211189952 A CN 202211189952A CN 115449237 A CN115449237 A CN 115449237A
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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
- C09C1/482—Preparation from used rubber products, e.g. tyres
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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
- C09C1/60—Agglomerating, pelleting, or the like by dry methods
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Abstract
The invention discloses high-dispersity dry granulation regenerated carbon black and a preparation method thereof, wherein the high-dispersity dry granulation regenerated carbon black comprises the following components in parts by weight: 90 to 100 portions of regenerated carbon black powder, 0.1 to 3 portions of plasticizer, 0.1 to 4 portions of wax, 0.1 to 2 portions of modifier and 0.1 to 1 portion of cross-linking agent, the dry granulation production operation of the regenerated carbon black is simple, the industrialization is easy to realize, the obtained product has high yield, low powder rate, easy dispersion in rubber, good dispersibility and reinforcement effect, and dust pollution can be reduced in the using process, thus the method belongs to an environment-friendly carbon black product. Compared with the existing wet granulation method, the method effectively reduces energy waste and production cost of enterprises.
Description
Technical Field
The invention relates to the technical field of rubber filler production, in particular to high-dispersity dry granulation regenerated carbon black and a preparation method thereof.
Background
The existing granulation methods of the regenerated carbon black mainly comprise dry granulation and wet granulation. The dry granulation mainly adopts a rolling process technology, and the powdery material is compressed into a sheet or a block, and then the sheet and the block are changed into granular materials meeting the use requirements through crushing, finishing and screening processes. Compared with wet granulation, the dry granulation process does not need to add water and then does not need subsequent drying, and the method is an energy-saving and consumption-saving continuous granulation method. However, the current dry granulation technology is still to be improved. Although the dry granulation has simple equipment, low energy consumption and low granulation cost, the granule strength is difficult to control, and the productivity is limited. When the particle strength is low, the particles are easy to break in the processes of production, packaging and transportation, so that the powder rate is high, the use of customers is influenced, and the productivity is low; when the particle strength is high, although the productivity is improved, the produced regenerated carbon black is difficult to disperse in rubber products, the reinforcing effect is influenced, and hard particles in the regenerated carbon black cause bubbling and packing of customer products and increase of the number of defective products.
The regenerated carbon black is obtained through a complex thermal cracking process, and the performance of the regenerated carbon black cannot be compared with the performance of the traditional carbon black. If the regenerated carbon black is subjected to deep processing treatment, the fineness of the regenerated carbon black can be obviously improved and can be crushed from 325 meshes to 1250 meshes, the increase of the fineness also improves the active groups and the adsorption capacity on the surface of the regenerated carbon black, and simultaneously improves the structure degree of the regenerated carbon black, so that the chemical properties of the regenerated carbon black, such as an oil absorption value, an iodine absorption value and the like, are improved, and the dispersibility in rubber is also obviously improved. However, when the powder regenerated carbon black is directly applied to the rubber field, certain dust pollution is brought in the production, transportation and use processes. Therefore, the invention provides a method for improving the dispersibility of dry granulation regenerated carbon black.
Disclosure of Invention
One of the purposes of the invention is to overcome the defects of low productivity, high hardness, high powder rate and the like of the existing regenerated carbon black dry granulation technology, and provide a production technology process which is efficient, energy-saving, environment-friendly and reduces the operation cost.
The second purpose of the invention is to provide an economical dry method modification method of regenerated carbon black with better performance, and endow the regenerated carbon black with better dispersibility and reinforcement in rubber.
In order to achieve the above purpose of the present invention, the following technical solutions are adopted:
the high-dispersity dry granulation regenerated carbon black is characterized by comprising the following components in parts by weight: 90 to 100 portions of regenerated carbon black powder, 0.1 to 3 portions of plasticizer, 0.1 to 4 portions of wax, 0.1 to 2 portions of modifier and 0.1 to 1 portion of cross-linking agent.
Preferably, the preparation method comprises the following steps:
s1, crushing waste tire cracking coke slag by using coarse powder equipment, removing iron and impurities, passing through an ultrafine pulverizer to obtain regenerated carbon black powder with the particle size D97 of 5-25 mu m, and transferring the regenerated carbon black powder into a storage bin for temporary placement;
s2, conveying the regenerated carbon black powder into a kneader through conveying equipment, starting a heating device, heating the material to a target temperature, sequentially adding a plasticizer, wax, a modifier and a cross-linking agent according to a proportion, uniformly mixing, and conveying the mixture into a cache bin for later use;
and S3, conveying the mixed materials to a dry-method granulator for extrusion granulation, and finally, carrying out granulation, granule finishing and screening, packaging and warehousing.
Preferably, the coke residue is one or a mixture of more of waste semi-steel tires or solid wastes obtained after rubber powder thermal cracking of all-steel tires.
Preferably, the coarse powder equipment is a jaw crusher, an impact crusher, a vertical mill or a dry-method ball mill; the ultrafine grinder is impact mill, mechanical mill, air flow mill, ring roller mill or stirring mill equipment, and the particle size D97 of the regenerated carbon black powder is 5-12 mu m.
Preferably, the present invention has at least one of the following features (1) to (5):
(1) The rotating speed of the kneader is 10-80 r/min;
(2) The heating mode of the kneader is heat conduction oil heating;
(3) The temperature of the kneader is 0-200 ℃;
(4) The mixing time of the materials is 0-60 min;
(5) The liquid modifier is added through a spray pipeline, and the spray flow is 0-100L/h.
Preferably, the resin composition has at least one of the following characteristics (1) to (4):
(1) The plasticizer is one or more of epoxidized soybean oil, castor oil, cardanol, polyol benzoate, fatty acid methyl ester, dioctyl phthalate, dibutyl phthalate, dioctyl terephthalate, dimethyl thiophenol, di (2-ethylhexyl) phthalate and polyethylene glycol;
(2) The wax is one or more of polyethylene wax, oxidized polyethylene wax and microcrystalline wax;
(3) The modifier is one or more of bis- [ gamma- (triethoxysilyl) propyl ] tetrasulfide, bis- [3- (triethoxysilyl) propyl ] -disulfide, vinyl tri (beta-methoxyethoxy) silane, vinyl trimethoxy silane, gamma-glycidoxypropyltrimethoxysilane, vinyl triethoxysilane and gamma- (methacryloyloxy) propyltrimethoxysilane;
(4) The cross-linking agent is one or more of hexamethylenetetramine, hexamethoxymethylmelamine, melamine, dicyandiamide (dicyandiamide), trimethylenediamine, diethylenetriamine and triethylenetetramine.
Preferably, the dry granulator has at least one of the following features (1) to (7):
(1) The dry-method granulator is a double-roller extrusion granulator;
(2) The dry-method granulator is provided with a pre-degassing device;
(3) The feeding frequency of the dry-method granulator is 0-50 Hz;
(4) The feeding main machine frequency of the dry granulating machine is 0-50 Hz;
(5) The ratio of the rotating speed of the feeding machine of the dry-method granulator to the rotating speed of the main machine is 1: (1-5);
(6) The roller spacing of the dry-method granulator is 0.1-5 mm;
(7) The pressure of the roller of the dry-method granulator is 0-20Mpa.
Preferably, the granulating device is one of a vibrating screen, a straight-line screen, a drum screen and a swinging screen.
The invention has the beneficial effects that:
(1) The invention starts with the coke residue raw material obtained by thermally cracking the waste tires, has sufficient raw material supply and stable source, and achieves the effect of recycling the waste resources with high added value.
(2) The invention improves the dry granulation speed and the granule forming rate through compounding various materials, and mainly ensures that the granule strength of the obtained product is controllable, thereby improving the dispersion performance and the reinforcing performance of the dry granulation regenerated carbon black in rubber.
(3) The dry granulation process is simple in production process operation, reduces dust pollution in the production process through closed operation, and provides a production technology process which is efficient, energy-saving, environment-friendly and low in operation cost.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the following technical solutions of the present invention are clearly and completely described with reference to specific embodiments, and it is obvious that the described embodiments are some, but not all, of the embodiments of the present invention, and are only used for illustrating the present invention, and should not be taken as limiting the present invention. All other embodiments, which can be obtained by a person skilled in the art without making any creative effort based on the embodiments in the present invention, belong to the protection scope of the present invention. The examples, in which specific conditions are not specified, were carried out according to conventional conditions or conditions recommended by the manufacturer. The reagents or instruments used are conventional products which are not indicated by manufacturers and are commercially available.
Example 1:
the high-dispersity dry granulation regenerated carbon black comprises the following components in parts by weight: 90 portions of regenerated carbon black powder, 1 portion of plasticizer, 0.1 portion of wax, 0.1 portion of modifier and 0.1 portion of cross-linking agent.
Example 2:
the high-dispersity dry granulation regenerated carbon black comprises the following components in parts by weight: 92 parts of regenerated carbon black powder, 1 part of plasticizer, 2 parts of wax, 1 part of modifier and 0.4 part of cross-linking agent.
Example 3:
the high-dispersity dry granulation regenerated carbon black comprises the following components in parts by weight: 95 parts of regenerated carbon black powder, 2 parts of plasticizer, 3 parts of wax, 2 parts of modifier and 0.5 part of cross-linking agent.
Example 4:
the high-dispersity dry granulation regenerated carbon black comprises the following components in parts by weight: 98 parts of regenerated carbon black powder, 3 parts of plasticizer, 2 parts of wax, 1 part of modifier and 0.6 part of cross-linking agent.
Example 5:
the high-dispersity dry granulation regenerated carbon black comprises the following components in parts by weight: 100 parts of regenerated carbon black powder, 3 parts of plasticizer, 4 parts of wax, 2 parts of modifier and 1 part of cross-linking agent.
Comparative example 1:
comparative example 1 is a commercially available wet granulation recycled carbon black from new materials science and technology limited, anhui Cought, product G385.
Comparative example 2:
comparative example 2 is a commercially available wet-pelletized recycled carbon black from EN330, product of environmental protection technologies ltd, clintel, anhui.
In the above examples, the plasticizer is one or more of epoxidized soybean oil, castor oil, cardanol, polyol benzoate, fatty acid methyl ester, dioctyl phthalate, dibutyl phthalate, dioctyl terephthalate, dimethyl thiophenol, di (2-ethylhexyl) phthalate, and polyethylene glycol;
the wax is one or more of polyethylene wax, oxidized polyethylene wax and microcrystalline wax;
the modifier is one or more of bis- [ gamma- (triethoxysilyl) propyl ] tetrasulfide, bis- [3- (triethoxysilyl) propyl ] -disulfide, vinyl tri (beta-methoxyethoxy) silane, vinyl trimethoxy silane, gamma-glycidoxypropyltrimethoxysilane, vinyl triethoxysilane and gamma- (methacryloyloxy) propyltrimethoxysilane;
the cross-linking agent is one or more of hexamethylenetetramine, hexamethoxymethylmelamine, melamine, dicyandiamide (dicyandiamide), trimethylenediamine, diethylenetriamine and triethylenetetramine.
The preparation method of the above embodiment comprises the following steps:
s1, crushing waste tire cracking coke slag by using coarse powder equipment, removing iron and impurities, then passing through an ultrafine pulverizer to obtain regenerated carbon black powder with the particle size D97 of 5-25 mu m, and transferring the regenerated carbon black powder into a storage bin for temporary placement;
wherein the coarse powder equipment is crushing equipment such as a jaw crusher, an impact crusher, a vertical mill or a dry-process ball mill; the ultrafine grinder is an impact mill, a mechanical mill, a jet mill, a ring roller mill or a stirring mill, and the average particle size of the carbon black powder obtained by grinding is 5-12 mu m.
The thermal cracking coke residue is one or more mixtures of solid wastes obtained after rubber powder thermal cracking of waste semi-steel tires or all-steel tires, and the waste tires comprise any one or more of but not limited to waste semi-steel cracking coke residue, waste all-steel cracking coke residue, waste oblique tire cracking coke residue, waste solid tire cracking coke residue and waste radial tire cracking coke residue;
s2, conveying the regenerated carbon black powder into a kneader through conveying equipment, starting a heating device, heating the material to a target temperature, sequentially adding a plasticizer, wax, a modifier and a cross-linking agent according to a proportion, uniformly mixing, and conveying the mixture into a cache bin for later use;
wherein the kneader has the following performance parameters:
(1) The rotating speed of the kneader is 10-80 r/min;
(2) The heating mode of the kneader is that heat conducting oil is used for heating;
(3) The temperature of the kneader is 0-200 ℃;
(4) The mixing time of the materials is 0-60 min;
(5) The liquid modifier is added through a spray pipeline, and the spray flow is 0-100L/h.
S3, after the mixed material enters a horizontal feeder, opening a vacuum degassing device, gradually degassing the material in the forward moving process under the driving of a rotating screw rod, forcibly feeding the material into a tablet machine, rolling the material into a regular shape with the thickness of 2-4 mm through a pair of rollers, and finally, packaging and warehousing after granulating, finishing and screening;
wherein, the performance parameters of the dry-method granulator are as follows:
(1) The dry-method granulator is a double-roller extrusion granulator;
(2) The dry-method granulator is provided with a pre-degasser;
(3) The feeding frequency of the dry method granulator is 0-50 Hz;
(4) The frequency of a feeding host machine of the dry-method granulator is 0-50 Hz;
(5) The ratio of the rotating speed of the feeding machine of the dry granulating machine to the rotating speed of the main machine is 1: (1-5);
(6) The roller spacing of the dry-method granulator is 0.1-5 mm;
(7) The pressure of the roller of the dry granulating machine is 0-20Mpa.
Experimental example 1
In order to compare and illustrate the properties of the regenerated carbon blacks obtained in the different examples and comparative examples, the properties of the regenerated carbon blacks obtained in the different examples and comparative examples were tested, and the test results are shown in Table 1.
TABLE 1 results of testing the Properties of different regenerated carbon blacks
Experimental example 2
In order to comparatively illustrate the influence of the regenerated carbon blacks obtained in different examples and comparative examples on the rubber performance, the mechanical properties and the like of the rubber were measured after the regenerated carbon blacks of different examples and comparative examples were applied to the rubber respectively according to the following methods, and the test results are shown in Table 2.
The concrete sizing material is prepared by mixing the following components in parts by weight: 100 parts of Natural Rubber (NR), 50 parts of regenerated carbon black in examples and comparative examples, 5.0 parts of zinc oxide, 3.0 parts of stearic acid, 0.6 part of accelerator DM and 2.5 parts of sulfur.
TABLE 2 Property test results for different rubbers
The test results show that the regenerated carbon black product has the advantages of high yield, low powder rate, low particle strength and the like. Compared with the regenerated carbon black produced by wet granulation, the regenerated carbon black is easy to disperse in rubber, has good dispersibility and reinforcement effect, can reduce dust pollution in the using process, and belongs to an environment-friendly carbon black product. The product produced by the invention not only effectively improves the dispersibility and the reinforcing property of the dry granulation regenerated carbon black, but also effectively reduces the energy waste and the production cost of enterprises.
The invention is not limited to the above embodiments, but rather should be construed as broadly as the invention can be embodied in various forms without departing from the spirit or essential characteristics thereof.
Claims (8)
1. The high-dispersity dry granulation regenerated carbon black is characterized by comprising the following components in parts by weight: 90 to 100 portions of regenerated carbon black powder, 0.1 to 3 portions of plasticizer, 0.1 to 4 portions of wax, 0.1 to 2 portions of modifier and 0.1 to 1 portion of cross-linking agent.
2. The high-dispersity dry granulation regenerated carbon black according to claim 1, wherein the preparation method comprises the following steps:
s1, crushing waste tire cracking coke slag by using coarse powder equipment, removing iron and impurities, then passing through an ultrafine pulverizer to obtain regenerated carbon black powder with the particle size D97 of 5-25 mu m, and transferring the regenerated carbon black powder into a storage bin for temporary placement;
s2, conveying the regenerated carbon black powder into a kneader through conveying equipment, starting a heating device, heating the material to a target temperature, sequentially adding a plasticizer, wax, a modifier and a cross-linking agent according to a proportion, uniformly mixing, and conveying the mixture into a cache bin for later use;
and S3, conveying the mixed materials to a dry-method granulator for extrusion granulation, and finally, packaging and warehousing after granulating, grading and screening.
3. The method for preparing high-dispersity dry granulation regenerated carbon black according to claim 2, wherein the coke residue is one or a mixture of more of solid wastes obtained after rubber powder of waste semi-steel tires or all-steel tires is thermally cracked.
4. The method for preparing high-dispersity dry granulation regenerated carbon black according to claim 2, wherein the coarse powder equipment is a jaw crusher, an impact crusher, a vertical mill or a dry ball mill; the ultrafine grinder is impact mill, mechanical mill, air flow mill, ring roller mill or stirring mill equipment, and the particle size D97 of the regenerated carbon black powder is 5-12 mu m.
5. The method for preparing highly dispersible dry granulation regenerated carbon black according to claim 2, characterized by at least one of the following features (1) to (5):
(1) The rotating speed of the kneader is 10-80 r/min;
(2) The heating mode of the kneader is heat conduction oil heating;
(3) The temperature of the kneader is 0-200 ℃;
(4) The mixing time of the materials is 0-60 min;
(5) The liquid modifier is added through a spray pipeline, and the spray flow is 0-100L/h.
6. The method for preparing high-dispersibility dry granulation regenerated carbon black according to claim 2, characterized by comprising at least one of the following characteristics (1) to (4):
(1) The plasticizer is one or more of epoxidized soybean oil, castor oil, cardanol, polyol benzoate, fatty acid methyl ester, dioctyl phthalate, dibutyl phthalate, dioctyl terephthalate, dimethyl thiophenol, di (2-ethylhexyl) phthalate and polyethylene glycol;
(2) The wax is one or more of polyethylene wax, oxidized polyethylene wax and microcrystalline wax;
(3) The modifier is one or more of bis- [ gamma- (triethoxysilyl) propyl ] tetrasulfide, bis- [3- (triethoxysilyl) propyl ] -disulfide, vinyl tri (beta-methoxyethoxy) silane, vinyl trimethoxy silane, gamma-glycidoxypropyltrimethoxysilane, vinyl triethoxysilane and gamma- (methacryloyloxy) propyltrimethoxysilane;
(4) The cross-linking agent is one or more of hexamethylenetetramine, hexamethoxymethylmelamine, melamine, dicyandiamide (dicyandiamide), trimethylenediamine, diethylenetriamine and triethylenetetramine.
7. The method for preparing high-dispersibility dry granulation regenerated carbon black according to claim 2, wherein the dry granulator has at least one of the following characteristics (1) to (7):
(1) The dry-method granulator is a double-roller extrusion granulator;
(2) The dry granulating machine is provided with a pre-degassing device;
(3) The feeding frequency of the dry-method granulator is 0-50 Hz;
(4) The feeding main machine frequency of the dry granulating machine is 0-50 Hz;
(5) The ratio of the rotating speed of the feeding machine of the dry-method granulator to the rotating speed of the main machine is 1: (1-5);
(6) The roller spacing of the dry-method granulator is 0.1-5 mm;
(7) The pressure of the roller of the dry-method granulator is 0-20Mpa.
8. The method for preparing the high-dispersibility dry granulation regenerated carbon black according to claim 2, characterized in that: the granulating equipment is one of a vibrating screen, a straight-line screen, a drum screen and a swing screen.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103304881A (en) * | 2013-06-26 | 2013-09-18 | 山东阳谷华泰化工股份有限公司 | Novel carbon black dispersing agent for rubber and preparation method thereof |
| CN108485245A (en) * | 2018-03-26 | 2018-09-04 | 袁峰 | A kind of versatility black agglomerate and preparation method thereof |
| CN113943500A (en) * | 2021-11-24 | 2022-01-18 | 安徽固瑞特新材料科技有限公司 | Modified pyrolytic carbon black and preparation method and application thereof |
| CN114381290A (en) * | 2022-02-12 | 2022-04-22 | 安徽固瑞特新材料科技有限公司 | Method for preparing superfine waste tire thermal cracking carbon black for rubber by wet method |
| CN114539821A (en) * | 2022-02-21 | 2022-05-27 | 安徽固瑞特新材料科技有限公司 | Method for modifying ultramicro cracking carbon black for rubber and preparing composite rubber |
-
2022
- 2022-09-28 CN CN202211189952.3A patent/CN115449237A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103304881A (en) * | 2013-06-26 | 2013-09-18 | 山东阳谷华泰化工股份有限公司 | Novel carbon black dispersing agent for rubber and preparation method thereof |
| CN108485245A (en) * | 2018-03-26 | 2018-09-04 | 袁峰 | A kind of versatility black agglomerate and preparation method thereof |
| CN113943500A (en) * | 2021-11-24 | 2022-01-18 | 安徽固瑞特新材料科技有限公司 | Modified pyrolytic carbon black and preparation method and application thereof |
| CN114381290A (en) * | 2022-02-12 | 2022-04-22 | 安徽固瑞特新材料科技有限公司 | Method for preparing superfine waste tire thermal cracking carbon black for rubber by wet method |
| CN114539821A (en) * | 2022-02-21 | 2022-05-27 | 安徽固瑞特新材料科技有限公司 | Method for modifying ultramicro cracking carbon black for rubber and preparing composite rubber |
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