CN111675828B - Preparation process of liquid reclaimed rubber - Google Patents
Preparation process of liquid reclaimed rubber Download PDFInfo
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- CN111675828B CN111675828B CN202010276762.XA CN202010276762A CN111675828B CN 111675828 B CN111675828 B CN 111675828B CN 202010276762 A CN202010276762 A CN 202010276762A CN 111675828 B CN111675828 B CN 111675828B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J11/00—Recovery or working-up of waste materials
- C08J11/04—Recovery or working-up of waste materials of polymers
- C08J11/10—Recovery or working-up of waste materials of polymers by chemically breaking down the molecular chains of polymers or breaking of crosslinks, e.g. devulcanisation
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2317/00—Characterised by the use of reclaimed rubber
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/62—Plastics recycling; Rubber recycling
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Abstract
A preparation process of liquid regenerated rubber, belonging to the field of recycling of waste rubber. The preparation process comprises the following steps: the crushed rubber powder of the heavy truck radial tire meeting the national standard of 22 meshes to 100 meshes is extruded through the reaction of five sections of a screw rod of an extruder, such as a heat conveying section, a shearing mixing section, a homogenizing desulfurization section, a strengthening desulfurization section, an extrusion conveying section and the like, and the liquid reclaimed rubber with uniform product and stable performance is obtained. The liquid reclaimed rubber can be well mixed with the asphalt and the performance thereof is improved. The production process has the advantages of simplicity, high efficiency, continuity, energy conservation, environmental protection and the like, and can obviously improve the application of the waste rubber in the field of modifying rubber modified asphalt.
Description
Technical Field
A preparation process of liquid reclaimed rubber is suitable for the field of recycling of waste rubber, in particular to the field of rubber modified asphalt and waterproof materials.
Background
China is the first major country of world tire production and consumption and is also the major country of waste tire production. At present, the rubber consumption of China accounts for about 30 percent of the world rubber consumption, and the rubber continuously occupies the first place in the world for many years. According to statistics, the production of waste tires in China in 2017 is about 3 hundred million, 1300 ten thousand tons or more, and the production increases by 6% -8% every year, and the production of the waste tires is expected to exceed 2000 ten thousand tons in 2020. The proliferation of the number of waste tires puts new requirements on ecological environment protection. The resource utilization of waste tires is the only way to solve the increasingly serious 'black pollution'.
In foreign countries, rubberized asphalt is a heavy burden for consuming a large amount of waste tires. In China, although waste rubber is required in the rubber industry field such as reclaimed rubber, the annual rubber powder demand is far smaller than the production of waste tires. At present, China uses a large amount of waste tires crushed into powder in the road asphalt industry after imitating foreign countries, and a certain consumption 'black pollution' effect is achieved. However, in the practical engineering application process, the problems of high mixing temperature, incapability of long-time storage and the like caused by the doping of rubber powder cause that the rubber powder can not be efficiently used and popularized in a large area.
In order to improve the engineering problem caused in the using process, part of enterprises adopt the method of moderately desulfurizing rubber powder, preparing the activated rubber powder and then mixing the activated rubber powder with asphalt for use.
Rubber desulfurization includes chemical desulfurization, mechanical desulfurization, biological desulfurization, microwave desulfurization, supercritical desulfurization and other methods, and the chemical desulfurization and the mechanical desulfurization are combined to produce the rubber at present in China. The specific production mode is that rubber powder of about 22-40 meshes, an activating agent and a softening agent are fully mixed and preheated, and then the mixture enters desulfurization equipment for desulfurization. The desulfurization equipment mainly comprises a plasticizing machine, an extruding machine and the like. The temperature setting of the desulfurization is controlled within the range of 150-270 ℃ according to different equipment and different product performance requirements.
The rubber can emit low-molecular volatile matters during the desulfurization process, and the volatile matters come from the rubber and various auxiliary agents, anti-aging agents and the like added in the early processing process of the rubber. Meanwhile, under the current common process, the addition of the activating agent and the softening agent further enhances the volatilization of odor gas and low molecular substances, and restricts the popularization of the product. The use requirements of the modified asphalt field on the reclaimed rubber are greatly different from the requirements of the traditional reclaimed rubber industry, and the indexes of mechanical property, Mooney property and the like of the reclaimed rubber are not strictly required. In order to meet the use requirements of the modified asphalt industry on the reclaimed rubber, a brand-new reclaimed rubber preparation process is invented.
The invention completes deep desulfurization of rubber powder by means of mechanical shearing of an extruder and powerful heating of a machine barrel without the action of any desulfurizing agent and softening agent.
The heat conductivity coefficient of the rubber powder is very low, and the high-temperature machine barrel of the extruder cannot fully heat the whole rubber powder in the screw groove within a limited time. Under the relative static condition, the surface rubber powder close to the inner surface of the cylinder can be rapidly heated to a desulfurization state or even a deep desulfurization state in a short time. The rubber powder after deep desulfurization can become sticky and has the capability of adhering the rubber powder. The heat conveying section is used for carrying out concentrated efficient heating on surface rubber powder close to the inner surface of the machine barrel under a relatively static conveying condition so as to enable the surface rubber powder to quickly reach a deep desulfurization state. The material is then conveyed to a shear mixing section.
In the shearing and mixing section, due to the use of a large number of strong shearing kneading blocks, the relative static condition of the heat conveying section is broken, so that the rubber powder with different desulfurization degrees in the spiral groove is fully mixed, and particularly, the regenerated rubber which is deeply desulfurized and is close to the wall of the machine cylinder and the rubber powder at the position of the mandrel can be fully kneaded and mixed. The rubber powder forms a whole adhesion state of 'oil in powder' (oil refers to deeply desulfurized reclaimed rubber) in the screw groove, the surface friction coefficient of the whole rubber powder is improved, and the strong shearing capability of the co-rotating twin-screw is good.
And a homogenizing desulfurization section mainly adopts conveying elements with a lead of 56mm and a kneading block with an angle of 45 degrees. The materials entering the section are desulfurized continuously due to rubber powder, the content of oil is further improved, and the effect of oil-in-powder is further enhanced. In order to protect the rubber powder which has been subjected to deep desulfurization, the strong shearing capability of the co-rotating twin-screw extruder is appropriately weakened, so that a 45-degree kneading block with moderate shearing strength is adopted. Under the action of moderate shearing and continuous heat energy, over 80 percent of the desulfurized rubber powder is deeply removed.
The reinforced desulfurization section mainly adopts a 60-degree kneading block and a 90-degree meshing block which have stronger shearing capacity. The material form at this stage is mainly the regenerated rubber subjected to deep desulfurization, and meanwhile, a small part of rubber powder which does not reach the deep desulfurization state is mixed in the regenerated rubber. The 'stubborn molecules' hidden in the deep devulcanized rubber are pertinently subjected to the concentrated action of the dense strong shearing element and the fixed-point 'removing' action of mechanical shearing to enable the part of rubber powder to finish deep devulcanization. Finally, the reclaimed rubber in a liquid state with uniform quality and stable state is obtained.
And the extrusion conveying section is mainly designed by adopting a large-lead conveying element and has the main function of stably extruding the reclaimed rubber in a liquid state quickly and efficiently.
The liquid regenerated rubber prepared by the process has the following advantages: the source of low-molecular volatile substances is reduced, and the product is clean and odorless in the subsequent use process; greatly simplifying the production process of rubber regeneration in the asphalt industry and reducing the cost; the consumption of the waste rubber in the field of rubber modified asphalt is increased; the performance of the matrix asphalt is better improved.
Disclosure of Invention
The invention aims to prepare the regenerated rubber by deep desulfurization of waste rubber powder by utilizing mechanical shearing and heat energy of an extruder.
A preparation process of liquid reclaimed rubber is characterized in that crushed rubber powder of a heavy truck radial tire meeting the national standard of 22-100 meshes enters a heat conveying section 2 of an extruder screw, a cylinder is set to be 380-420 ℃, and a conveying element with the lead of 56mm is connected with a back rotating element of 6D-9D in the heat conveying section. After a material section entering an extruder from a feeding section passes through a reverse-rotation threaded element, rubber powder is in a compact full state in a machine barrel, the compaction and pressure building are 1 Mp-3 Mp, the rubber powder is stably conveyed at 30 rpm-80 rpm, a rubber powder layer with the thickness of 0.2 mm-1 mm close to the inner surface of the machine barrel is heated to 330-350 ℃ within 1s-10, and under the action of heat energy, deep desulfurization rubber powder with the Mooney viscosity of 5-15 [ ML (1+4)100 ℃) ] is obtained through desulfurization; entering a shearing and mixing section 3 with the length of the screw rod of 6D-8D, adopting 45-degree kneading blocks and 90-degree kneading blocks to be alternately arranged, setting the temperature of a machine barrel to be 350-380 ℃, and continuously heating, desulfurizing and fully mixing rubber powder with different desulfurization degrees within the retention time of 2-10 s; entering a homogenization and desulfurization section 4 with the length of a screw rod of 10D-15D, setting the temperature of a machine barrel to be 300-320 ℃, alternately arranging a conveying element with the lead of 56mm, a 45-degree kneading block and a 30-degree kneading block for a residence time of 10-30 s, and completing deep desulfurization of more than 80% of rubber powder under the action of shearing and heat energy of the screw rod, wherein the Mooney viscosity of the rubber powder is 20-30 [ ML (1+4)100 ℃; entering a reinforced desulfurization section 5 with the length of a screw rod of 10D-15D, setting the temperature of a machine barrel to be 290-310 ℃, alternately combining and arranging 90-degree kneading blocks and 60-degree kneading blocks for screw elements, keeping the residence time to be 10-20 s, realizing deep desulfurization of all rubber powder under the shearing action, and ensuring that the Mooney viscosity of the desulfurized rubber powder is 5-10 [ ML (1+4)100 ℃) ]; and finally, the mixture enters an extrusion conveying section 6 with the length of the screw being 3D-5D, the section adopts a conveying element with the lead of 96mm, the retention time is 2 s-4 s, and the temperature of a machine barrel is set to be 250-270 ℃. After the reaction extrusion of 5 sections, the deep regeneration of the waste rubber is realized, and the liquid regenerated rubber is obtained. As shown in fig. 2.
The extruder used in the process is a co-twin screw extruder or a co-rotating three screw extruder;
the raw materials adopted in the process are all tire rubber powder or tread rubber powder of the heavy truck radial tire meeting the national standard;
the length-diameter ratio (40-50) of the extruder screw in the process is as follows: 1;
the mesh number of the rubber powder adopted in the process is 22-100 meshes;
the screw element adopted in the process is composed of a kneading block element with 30-90 degrees, a conveying element and a reverse screw element, wherein the length proportion of the kneading block is not less than 50 percent;
the diameter of the screw rod adopted in the process is more than or equal to 30mm and less than or equal to 200 mm;
the clearance between the screw rod and the screw rod of the extruder adopted in the process is 0.5-1 mm, and the clearance between the screw rod and the machine barrel is 0.5-1.5 mm, as shown in figure 2.
Drawings
FIG. 1 is a schematic view of the process of the present invention.
FIG. 2 is a schematic view showing that the clearance between a screw and a barrel of the extruder is 0.5-1 mm, and the clearance between the screw and the barrel is 0.5-1.5 m.
FIG. 3 is an enlarged view of the extruder screw of the present invention.
The specific implementation mode is as follows:
examples
The liquid reclaimed rubber is prepared by adopting 22-mesh heavy truck radial tire full tire waste rubber powder meeting the national standard and a screw diameter phi 75 type co-rotating double-screw extruder with the length-diameter ratio of 48:1 (the total length of the screw is 48D), wherein the clearance between the screw and the screw is 1.5mm, and the clearance between the screw and a machine barrel is 1 mm. The main machine rotation speed was set to 70 rpm. The rubber powder was fed into the extruder via a feed section (4D, screw elements are 96mm long lead conveying elements) into a 9D hot conveying section, screw elements are 56mm conveying elements, the barrel temperature was set at 400 ℃ and the residence time was 10s, and the barrel material was heated with high intensity in a relatively static state. The rubber powder which is 1mm close to the inner surface of the machine barrel is deeply desulfurized and becomes sticky. The rubber powder enters a shearing and mixing section with the length of 6D, a screw element adopts 45-degree kneading blocks and 90-degree kneading blocks which are alternately combined for use, the set temperature of a machine barrel is 370 ℃, and the rubber powder in different desulfurization states in the section is fully mixed for 8s of residence time. The sticky rubber powder is fully mixed with other rubber powder to form the viscoelastic state of the whole rubber powder, so that the friction coefficient of the rubber powder with a screw and a machine barrel is increased, and mechanical shearing desulfurization is excited and strengthened. Entering a homogenization desulfurization section with the length of 14D, alternately arranging 45-degree kneading blocks and 30-degree kneading blocks in lead for screw elements, setting the temperature of a machine barrel to be 320 ℃, and further desulfurizing the whole rubber powder within 23s of reaction time under the action of moderate shear and heat energy to obtain the desulfurized rubber powder with the Mooney viscosity of 25[ ML (1+4)100 ℃). Entering a reinforced desulfurization section with the length of 13D, alternately arranging 90-degree kneading blocks and 60-degree kneading blocks in a combined manner by screw elements, setting the temperature of a machine barrel at 290 ℃, rapidly desulfurizing an underdesulfurized part in a material within a short time within 20s of residence reaction time by utilizing high-strength shearing to achieve the uniformity and stability of a product, and extruding the obtained liquid regenerated rubber with the Mooney viscosity of 7[ ML (1+4)100 ℃), and passing through an extrusion conveying section (with the length of 2D). The screw elements of the extrusion conveying section consist of 96mm and 56mm conveying elements, the temperature is set at 260 ℃ and the residence time is 2 s. Finally, the Mooney viscosity of the obtained liquid reclaimed rubber product is 7[ ML (1+4)100 ℃, and 10 parts, 20 parts and 30 parts of liquid reclaimed rubber are fully mixed with 100 parts of Esso 70# asphalt and developed to obtain the modified asphalt. The indexes before and after are compared as follows:
Claims (8)
1. a preparation process of liquid reclaimed rubber is characterized by comprising the following steps: broken rubber powder of a heavy truck radial tire meeting the national standard of 22 meshes to 100 meshes enters a heat conveying section of a screw of an extruder, a machine barrel is set to be 380 ℃ to 420 ℃, and a conveying element with the lead of 56mm is connected with the heat conveying section from a reverse rotation element to 6D to 9D; after a material section entering an extruder from a feeding section passes through a reverse-rotation thread element, rubber powder is in a compact full state in a machine barrel, the compaction pressure is built up by 1 Mp-3 Mp, the rubber powder is stably conveyed at 30 rpm-80 rpm, a rubber powder layer with the thickness of 0.2 mm-1 mm close to the inner surface of the machine barrel is heated to 330-350 ℃ within 1s-10s, and under the action of heat energy, deep desulfurization rubber powder with the Mooney viscosity of 5-15 [ ML (1+4)100 ℃) ] is obtained through desulfurization; entering a shearing and mixing section with the length of the screw being 6D-8D, alternately arranging 45-degree kneading blocks and 90-degree kneading blocks, setting the temperature of a machine barrel to be 350-380 ℃, and continuously heating, desulfurizing and fully mixing the rubber powder with different desulfurization degrees within the retention time of 2-10 s; entering a homogenization and desulfurization section with the length of a screw rod of 10-15D, setting the temperature of a machine barrel to be 300-320 ℃, alternately arranging a conveying element with a lead of 56mm, a kneading block with a degree of 45 degrees and a kneading block with a degree of 30 degrees by adopting a screw thread, keeping for 10-30 s, and setting the Mooney viscosity of the desulfurized rubber powder to be 20-30 [ ML (1+4)100 ℃; entering a reinforced desulfurization section with the length of a screw rod of 10D-15D, setting the temperature of a machine barrel to be 290-310 ℃, alternately combining and arranging 90-degree kneading blocks and 60-degree kneading blocks for a screw thread element, keeping the time for 10-20 s, and controlling the Mooney viscosity of the desulfurized rubber powder to be 5-10 [ ML (1+4)100 ℃; and finally, entering an extrusion conveying section with the length of 3D-5D of the screw, wherein the section adopts a conveying element with the lead of 96mm, the retention time is 2 s-4 s, the temperature of a machine barrel is set to be 250-270 ℃, and the liquid reclaimed rubber with the Mooney viscosity of 5-10 [ ML (1+4)100 ℃) is prepared.
2. A process as claimed in claim 1, wherein the extruder used is a co-rotating twin-screw extruder or a co-rotating triple-screw extruder.
3. The process of claim 1, wherein the raw material is rubber powder for full tires or tread rubber powder for heavy truck radial tires meeting national standards.
4. The process according to claim 1, wherein the extruder screw has a length to diameter ratio (40 to 50): 1.
5. the process as claimed in claim 1, wherein the rubber powder has a mesh size of 22-100 meshes.
6. The process as claimed in claim 1, wherein the screw elements used are kneading block elements and conveying elements of 30 ° to 90 ° and reverse screw elements, and wherein the proportion of the length of the kneading blocks is not less than 50%.
7. The process according to claim 1, wherein the screw diameter is 30mm or less and 200mm or less.
8. The process according to claim 1, wherein the extruder has a screw-to-screw clearance of 0.5 to 1mm and a barrel-to-barrel clearance of 0.5 to 1.5 mm.
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| CN202010276762.XA CN111675828B (en) | 2020-04-10 | 2020-04-10 | Preparation process of liquid reclaimed rubber |
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| CN202010276762.XA CN111675828B (en) | 2020-04-10 | 2020-04-10 | Preparation process of liquid reclaimed rubber |
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| CN111675828B true CN111675828B (en) | 2022-07-26 |
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| CN114381131B (en) * | 2021-11-22 | 2023-04-07 | 中远海运国际贸易有限公司 | Liquid rubber master batch and preparation method thereof, anti-aging high-toughness waterproof asphalt material and preparation method thereof |
| CN114316612B (en) * | 2021-11-22 | 2023-04-21 | 中远海运国际贸易有限公司 | Liquid rubber master batch and preparation method and application thereof |
| CN115160806B (en) * | 2022-07-18 | 2023-07-25 | 甘肃公航旅低碳科技有限公司 | Preparation method and application of low-carbon asphalt based on recycled resources |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104690844A (en) * | 2015-03-21 | 2015-06-10 | 南京绿金人橡塑高科有限公司 | Method for preparing granular rubber by adopting three screw rods to continuously extrude devulcanized rubber powder |
| CN110154359A (en) * | 2019-05-22 | 2019-08-23 | 南京绿金人橡塑高科有限公司 | A method of reclaimed rubber is refined and refined using Co rotating Twin Screw Extrusion |
| CN110591148A (en) * | 2019-09-05 | 2019-12-20 | 江苏睿博环保设备有限公司 | Reclaimed rubber without adding any auxiliary agent in desulfurization process and preparation method thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104690844A (en) * | 2015-03-21 | 2015-06-10 | 南京绿金人橡塑高科有限公司 | Method for preparing granular rubber by adopting three screw rods to continuously extrude devulcanized rubber powder |
| CN110154359A (en) * | 2019-05-22 | 2019-08-23 | 南京绿金人橡塑高科有限公司 | A method of reclaimed rubber is refined and refined using Co rotating Twin Screw Extrusion |
| CN110591148A (en) * | 2019-09-05 | 2019-12-20 | 江苏睿博环保设备有限公司 | Reclaimed rubber without adding any auxiliary agent in desulfurization process and preparation method thereof |
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