LU501593B1 - Method for Producing Environment-friendly High-quality Ethylene-propylene Reclaimed Rubber by Temperature Reduction and Desulfurization - Google Patents

Method for Producing Environment-friendly High-quality Ethylene-propylene Reclaimed Rubber by Temperature Reduction and Desulfurization Download PDF

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Publication number
LU501593B1
LU501593B1 LU501593A LU501593A LU501593B1 LU 501593 B1 LU501593 B1 LU 501593B1 LU 501593 A LU501593 A LU 501593A LU 501593 A LU501593 A LU 501593A LU 501593 B1 LU501593 B1 LU 501593B1
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rubber
propylene
ethylene
desulfurization
activator
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LU501593A
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German (de)
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Yanqiu Wang
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Xuzhou College Ind Technology
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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
    • 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
    • C08J2323/00—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers
    • C08J2323/02—Characterised by the use of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Derivatives of such polymers not modified by chemical after treatment
    • C08J2323/16—Ethene-propene or ethene-propene-diene copolymers

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  • Chemical & Material Sciences (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Sustainable Development (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)

Abstract

The invention discloses a method for producing environment-friendly high-quality ethylene-propylene reclaimed rubber by temperature reduction and desulfurization, which comprises the following steps: putting waste ethylene-propylene rubber into an open mill at normal temperature, carrying out thin pass crushing, and thin pass 30 times; weighing waste ethylene-propylene rubber powder into an open mill with a roll distance of 0.2 mm, adding chlorinated polyethylene, regeneration activator 510, stearic acid, zinc oxide, tribasic lead sulfate and dibasic lead phosphite in proportion, rolling for 10 times through the open mill to prepare mixed rubber powder, putting into a desulfurization tank. The desulfurized rubber powder is parked at room temperature for more than 4 hours, the desulfurized rubber powder is refined by an open mill at low temperature until the surface of the film is smooth, sulfur S8, accelerator M and TMTD are added into the refined reclaimed rubber, vulcanized after parking for 16 hours.

Description

DESCRIPTION LU501593 Method for Producing Environment-friendly High-quality Ethylene-propylene Reclaimed Rubber by Temperature Reduction and Desulfurization
TECHNICAL FIELD The invention relates to a method for producing environment-friendly high-quality ethylene-propylene reclaimed rubber by temperature reduction and desulfurization, belonging to the field of reclaimed rubber preparation.
BACKGROUND Ethylene-propylene rubber has excellent heat resistance, ozone resistance, steam resistance, chemical resistance and insulation performance, and is widely used in tires, auto parts, heat-resistant hoses and tapes, wires and cables, sealing materials and other fields. With the development of ethylene-propylene rubber, a large amount of waste vulcanized rubber produced in the production and use of ethylene-propylene rubber products has also become a major problem in the industry. Reasonable recycling of waste ethylene-propylene rubber is of great significance to reduce costs, make full use of resources and ensure the large-scale production and application of waste ethylene-propylene rubber.
In the production of traditional recycled rubber from waste ethylene-propylene rubber products, the dynamic desulfurization tank is used to desulfurize at 350°C at high temperature, and the elastomer is changed into a plastic body. In the high-temperature production process, a large amount of toxic waste gas and wastewater are produced, which seriously pollutes the environment, especially affects the health of enterprise operators, and may even cause cancer in severe cases. In addition, the traditional process is complicated and wastes a lot of energy.
SUMMARY In order to overcome the shortcomings of the traditional regeneration technology of waste ethylene-propylene rubber mentioned above, the production of ethylene-propylene reclaimed rubber by lowering the temperature can effectively reduce the generation of waste gas and waste water, wherein the key technology is to develop a regeneration activator which decomposes and cuts off vulcanization bonds such as O-C bonds at a lower temperature, so as to provide a method for producing environment-friendly high-quality ethylene-propylene reclaimed rubber by lowering the temperature and desulfurizing.
The invention is realized by the following technical scheme: a method for producit&/501593 environment-friendly high-quality ethylene-propylene reclaimed rubber by temperature reduction and desulfurization and its application in aging-resistant products, which comprises the following raw materials in parts by mass: Waste ethylene propylene rubber 100 Regeneration activator 510 2.0 Stearic acid (SA) 3.0-5.0 Paraffin oil 5.0-10.0 Chlorinated polyethylene rubber CM 5.0-12.0 Tribasic lead sulfate 0.5 Dibasic lead phosphite 0.5 Zinc oxide 5.0 Accelerator TMTD 1.0 Accelerator M 0.5 Sulfur Sg 1.5 The mass ratio of regenerative activator 510 to stearic acid SA in the composite regenerative activator is 1:1.
The preparation method comprises the following steps: 1) Putting waste ethylene-propylene rubber into an open mill at normal temperature, crushing by thin pass for 30 times to obtain waste ethylene-propylene rubber powder; 2) Pre-processing chlorinated polyethylene CM master batch, namely adding paraffin oil, tribasic lead sulfate and dibasic lead phosphite evenly into powdered chlorinated polyethylene CM on an open mill to prepare chlorinated polyethylene CM master batch; 3) Weighing the waste ethylene-propylene rubber powder and putting it into an open mill with a roll distance of 0.2 mm, adding powdered chlorinated polyethylene CM masterbatch, regeneration activator 510, stearic acid (SA) and zinc oxide according to a certain proportion, and rolling it through the open mill for 10 times, so that all components are evenly dispersed in the waste ethylene-propylene rubber powder to prepare mixed rubber; 4) Putting the mixed rubber powder into a desulfurization tank, and desulfurization according to desulfurization regeneration conditions to prepare desulfurization rubber;
5) Parking the desulfurized rubber powder at normal temperature for more than 4 hours t&/501593 be refined; 6) Adjust the roller distance of the mill to 0.1 mm, refine the desulfurized rubber powder at low temperature until the surface of the film is smooth and uniform to obtain refined reclaimed rubber, take part of the refined reclaimed rubber and park it for 24 hours, and then test the Mooney viscosity of the rubber; 7) Add sulfur Ss, accelerator M and accelerant TMTD into the remaining refined reclaimed rubber, mix evenly, then park for 16 hours before vulcanization, and then park the vulcanized test piece for 24 hours before performance test.
Preferably, the composite regenerative activator refers to the combination of regenerative activator 510 and stearic acid (SA) in any proportion.
Preferably, the composite regenerative activator means that the mass ratio of regenerative activator 510 to stearic acid (SA) is 1:1.
Preferably, the chlorinated polyethylene rubber CM is 10-12 parts.
Preferably, there are 5-10 parts of paraffin hydrocarbon oil.
Preferably, the desulfurization regeneration conditions refer to the regeneration temperature of 210£5°C and the regeneration time of 15+5 min.
At the temperature of desulfurization regeneration condition, the compound high-efficiency regeneration activator can release a large amount of active free radicals to induce waste rubber powder to generate rubber active free radicals, that is, a large number of crosslinking bonds in waste rubber and the main chain of rubber molecules are broken, and elastic rubber becomes plastic reclaimed rubber; after the regeneration, the free radicals produced by the compound efficient regeneration activator can stop the activity of rubber active free radicals at 60°C, effectively preventing the rebound of Mooney viscosity of reclaimed rubber.
Effect of Invention (1) Compared with the traditional reclaimed ethylene-propylene rubber at 350+5'C, the reclaimed ethylene-propylene rubber at 210+5 C can obtain higher mechanical and technological properties. The regeneration process at lower temperature not only protects the molecular main chain from being destroyed, but also breaks the cross-linking bond, retaining the performance of recycling waste rubber. Waste rubber is regenerated at low temperature, which eliminates the disadvantage of easy coalescence of rubber free radicals at high temperature. Thé/501593 elastic recovery of broken rubber molecules is small and Mooney viscosity is stable. Table 2 shows the influence of the types and dosage of recycled activators on the processing technology and mechanical properties of recycled rubber.
(2) When regenerated at 210+5°C, SA can activate the regeneration activator 510 molecules and improve the regeneration efficiency.
(3) After regeneration at 21045 °C , ethylene-propylene rubber can basically avoid environmental pollution. Waste ethylene-propylene rubber powder contains a certain amount of pollutants which are combined with rubber through chemical bonds or physical bonds, and the volatilization temperature is generally above 245+5°C through detection.
(4) When chlorinated polyethylene rubber is added, it can play a reinforcing role when the dosage is small, and when the dosage is large, the breaking elongation will increase due to the unwinding of physical entanglement points during stretching.
(5) Adding paraffin hydrocarbon oil, which can penetrate between rubber macromolecules, the Mooney viscosity decreases significantly and the elongation at break increases.
DESCRIPTION OF THE INVENTION Embodiment 1 The raw materials and parts by mass are as follows: Waste ethylene propylene rubber 100 Regeneration activator 510 2.0 Stearic acid (SA) 2.0 Paraffin oil 5.0 Chlorinated polyethylene rubber (CM-3000) 5.0 Tribasic lead sulfate (three salts) 0.5 Dibasic lead phosphite (two salts) 0.5 Zinc oxide 5.0 Accelerator TMTD 1.0 Accelerator M 0.5 Sulfur Sg 1.5
Composite regeneration activator means that regeneration activator 510 and stearic acid (SIAJ501593 are used together.
The preparation method comprises the following steps: 1) Putting waste ethylene-propylene rubber into an open mill at normal temperature, crushing by thin pass for 30 times to obtain waste ethylene-propylene rubber powder; 2) Pre-processing of chlorinated polyethylene CM-3000 master batch: 15 g of paraffin oil,
1.5 g of tribasic lead sulfate and 1.5 g of dibasic lead phosphite are evenly added into powdered chlorinated polyethylene CM 15 g on an open mill to prepare 33 g of chlorinated polyethylene CM master batch; 3) Weighing 300 g of waste ethylene-propylene rubber powder and putting it into an open mill with a roll distance of 0.2 mm, adding 33 g of powdered chlorinated polyethylene CM-3000 masterbatch, 6 g of regenerative activator 510, 15 g of stearic acid (SA) and 15 g of zinc oxide according to a certain proportion, and rolling it through the open mill for 10 times, so that all components are uniformly dispersed in the waste ethylene-propylene rubber powder to prepare mixed rubber; 4) Put that mixed rub powder into a desulfurization tank, and desulfurization is carried out according to the regeneration temperature of 210+5°C and the regeneration time of 20 min to prepare desulfurized rub material; 5) After regeneration, the desulfurized rubber powder is quickly cooled to 60°C or below. Park at room temperature for more than 4 hours to be refined, 6) Adjust the roller distance of the mill to 0.1 mm, refine the desulfurized rubber powder at low temperature until the surface of the film is smooth and uniform to obtain refined reclaimed rubber, take part of the refined reclaimed rubber and park it for 24 hours, and then test the Mooney viscosity of the rubber; 7) Add 4.5 g sulfur Sg, 1.5 g accelerators M and 3.0 g accelerators TMTD to the remaining refined reclaimed rubber, mix evenly, and then park for 16 hours before vulcanization. After parking for 24 hours, test the performance of vulcanized test pieces. See Table 1 and Table 2 for the test performance.
Embodiment 2 The raw materials and parts by mass are as follows:
Ethylene propylene rubber powder 100 LU501593 Activator 510 2.0 Stearic acid (SA) 3.0 Paraffin oil 7.0 Chlorinated polyethylene rubber (CM-3000) 12.0 Tribasic lead sulfate (three salts) 0.5 Dibasic lead phosphite (two salts) 0.5 Zinc oxide 5.0 Accelerator TMTD 1.0 Accelerator M 0.5 Sulfur Sg 1.5 Composite regeneration activator means that regeneration activator 510 and stearic acid (SA) are used together.
The preparation method comprises the following steps: 1) Putting waste ethylene-propylene rubber into an open mill at normal temperature, crushing by thin pass for 30 times to obtain waste ethylene-propylene rubber powder; 2) Pre-processing of chlorinated polyethylene CM-7130 master batch: 21 g of paraffin oil,
1.5 g of tribasic lead sulfate and 1.5 g of dibasic lead phosphite are evenly added into powdered chlorinated polyethylene CM-7130 36 g on an open mill to prepare 60 g of chlorinated polyethylene CM-7130 master batch; 3) Weighing 300 g of waste ethylene-propylene rubber powder and putting it into an open mill with a roll distance of 0.2 mm, adding 60 g of powdered chlorinated polyethylene CM-7130 masterbatch, 6 g of regenerative activator 510, 9 g of stearic acid and 15 g of zinc oxide according to a certain proportion, and rolling it through the open mill for 10 times, so that all components are uniformly dispersed in the waste ethylene-propylene rubber powder to prepare mixed rubber; 4) Putting the mixed rubber powder into a desulfurization tank, and performing desulfurization according to the regeneration temperature of 215°Cand the regeneration time of minutes to prepare desulfurized rubber powder;
5) After regeneration, the desulfurized rubber powder is quickly cooled to 60°C or belok/501593 park at room temperature for more than 4 hours to be refined, 6) Adjust the roller distance of the mill to 0.1 mm, refine the desulfurized rubber powder at low temperature until the surface of the film is smooth and uniform to obtain refined reclaimed rubber, take part of the refined reclaimed rubber and park it for 24 hours, and then test the Mooney viscosity of the rubber; 7) Add sulfur Sg 4.5 g, accelerator M 1.5 g and accelerator TMTD 3.0 g to the remaining refined reclaimed rubber, mix evenly, then park for 16 hours, then vulcanize, and test the performance of vulcanized test pieces after parking for 24 hours. See Table 1 for the test performance.
Embodiment 3 The raw materials and parts by mass are as follows: Ethylene propylene rubber powder 100 Activator 510 2.0 Stearic acid (SA) 5.0 Paraffin oil 10.0 Chlorinated polyethylene rubber (CM-3000) 10.0 Tribasic lead sulfate (three salts) 0.5 Dibasic lead phosphite (two salts) 0.5 Zinc oxide 5.0 Accelerator TMTD 1.0 Accelerator M 0.5 Sulfur Sg 1.5 Composite regeneration activator means that regeneration activator 510 and stearic acid (SA) are used together.
The preparation method comprises the following steps: 1) Putting waste ethylene-propylene rubber into an open mill at normal temperature, crushing by thin pass for 30 times to obtain waste ethylene-propylene rubber powder; 2) Pre-processing of chlorinated polyethylene CM-3000 master batch: 30 g of paraffin oil,
1.5 g of tribasic lead sulfate and 1.5 g of dibasic lead phosphite are evenly added into powdered chlorinated polyethylene CM-3000 30 g on an open mill to prepare 63 g of chlorinatéd/501593 polyethylene CM-3000 master batch; 3) Weighing 300 g of waste ethylene-propylene rubber powder and putting it into an open mill with a roll distance of 0.2 mm, adding 63 g of powdered chlorinated polyethylene CM-3000 masterbatch, 6 g of regenerative activator 510, 15 g of stearic acid (SA) and 15 g of zinc oxide according to a certain proportion, and rolling it through the open mill for 10 times, so that all components are uniformly dispersed in the waste ethylene-propylene rubber powder to prepare mixed rubber; 4) Putting the mixed rubber powder into a desulfurization tank, and performing desulfurization according to the regeneration temperature of 205°Cand the regeneration time of minutes to prepare desulfurized rubber powder; 5) After regeneration, the desulfurized rubber powder is quickly cooled to 60°C or below, park at room temperature for more than 4 hours to be refined, 6) Adjust the roller distance of the mill to 0.1 mm, refine the desulfurized rubber powder at low temperature until the surface of the film is smooth and uniform to obtain refined reclaimed rubber, take part of the refined reclaimed rubber and park it for 24 hours, and then test the Mooney viscosity of the rubber; 7) Add sulfur Sg 4.5 g, accelerator M 1.5 g and accelerator TMTD 3.0 g to the remaining refined reclaimed rubber, mix evenly, then park for 16 hours, then vulcanize, and test the performance of vulcanized test pieces after parking for 24 hours. See Table 1 for the test performance.
Table 1 Effects of modifier CM and paraffin oil on processing technology and mechanical properties of ethylene-propylene reclaimed rubber Regenerated Rubber GB/T _ 13460-2008 “action REACH ethylene-pr FUR Example 2 Example 3 opylene ; egulation | Example 1 he 7 ; Project (EC) No Modifier Modifier Modifier reclaimed CM-7130(12. | CM-3000(10.0) rubber 1907/2006 CM-3000(5. ; ; ; Detection ; 0)/ Paraffin / Paraffin softening Registration, 0)/ Paraffin performance Evaluation oil (5.0) Hydrocarbon Hydrocarbon agent 4 SE ’ Oil (5.0) Oil (5.0) Paraffin uthorisation Co Hydrocarbo and Restriction n oil (10.0) of Chemicals ‘ REACH-2009
Regeneration Regeneratio Regeneration Regenerati Regeneratio LU501593 activator n activator activator on activator n activator 510(2.0) 510(2.0) 510(2.0) 510(2.0) 510(2.0) /ISA(2.0) /ISA(2.0) /SA(2.0) Tensile strength >5.5 8.33 7.50 7.86 /MPa Elongation at >260 334.00 409.00 396.00 300 break/% ~ ’ ’ ; Mooney viscosity ML100 <65 30.34 26.26 36.48 “C(1+4) Total content of 18 polycyclic aromatic <200 149.72 129.41 138.36 5371.31 hydrocarbons /mg/kg/ GC-MS analysis Note: Example regeneration temperature/time: 210+5‘C/20 min.
Table 2 Effect of regeneration process conditions on processing technology and mechanical properties of ethylene-propylene reclaimed rubber Example 1 _ Process Temperature/time Traditional De ‘ dition of regeneration temperature/time etectiqn ° 210+5°C/20 A ; performanès ( / (280+5°C/60 min) min) Tensile strength Pre | us | ue Elongation at Mooney viscosity ML100°C 30.34 60.15 (1+4) Total content of 18 polycyclic aromatic hydrocarbons 149.72 5371.31 /mg/kg/ GC-MS analysis

Claims (6)

  1. CLAIMS LU501593
    1. A Method for producing environment-friendly high-quality ethylene-propylene reclaimed rubber by temperature reduction and desulfurization, characterized by comprising the following raw materials in parts by mass: Waste ethylene propylene rubber 100 Regeneration activator 510 2.0 Stearic acid (SA) 3.0-5.0 Paraffin oil 5.0-10.0 Chlorinated polyethylene rubber CM 5.0-12.0 Tribasic lead sulfate 0.5 Dibasic lead phosphite 0.5 Zinc oxide 5.0 Accelerant TMTD 1.0 Accelerant M 0.5 Sulfur Sg 1.5 the mass ratio of regenerative activator 510 to stearic acid (SA) in the composite regenerative activator is 1:1; the preparation method comprises the following steps: 1) putting waste ethylene-propylene rubber into an open mill at normal temperature, crushing by thin pass for 30 times to obtain waste ethylene-propylene rubber powder; 2) pre-processing of chlorinated polyethylene CM masterbatch: evenly adding paraffin oil, tribasic lead sulfate and dibasic lead phosphite into powdered chlorinated polyethylene CM on an open mill to prepare chlorinated polyethylene CM masterbatch; 3) weighing waste ethylene-propylene rubber powder and putting it into an open mill with a roll distance of 0.2 mm, adding powdered chlorinated polyethylene CM masterbatch, regeneration activator 510, stearic acid (SA) and zinc oxide according to a certain proportion, and rolling through the open mill for 10 times, so that all components are uniformly dispersed in the waste ethylene-propylene rubber powder to prepare mixed rubber powder;
    4) putting the mixed rubber powder into a desulfurization tank, and desulfurizatid#/501593 according to desulfurization regeneration conditions to prepare desulfurized rubber powder; the desulfurization temperature is 210+£5°C and the regeneration time is 15+5 min; 5) after regeneration, quickly cooling the desulfurized rubber powder to 60°C or below, and parking at room temperature for more than 4 hours to be refined, 6) adjusting the roller distance of the mill to 0.1 mm, refining the desulfurized rubber powder at low temperature until the surface of the film is smooth and uniform to obtain refined reclaimed rubber, taking part of the refined reclaimed rubber and park it for 24 hours, and then testing the mooney viscosity of the rubber; 7) adding sulfur Ss, accelerator M and accelerator TMTD into the remaining refined reclaimed rubber, mixing evenly, and then parking for 16 hours before vulcanization, and then testing the performance of vulcanized test pieces after parking for 24 hours.
    2. The method for producing environment-friendly high-quality ethylene-propylene reclaimed rubber by temperature reduction and desulfurization according to claim 1, characterized in that the composite regenerative activator is made of regenerative activator 510 and stearic acid (SA) in any proportion.
    3. The method for producing environment-friendly high-quality ethylene-propylene reclaimed rubber by temperature reduction and desulfurization according to claim 2, characterized in that in the composite regenerative activator, the mass ratio of regenerative activator 510 to stearic acid (SA) is 1:1.
    4. The method for producing environment-friendly high-quality ethylene-propylene reclaimed rubber by temperature reduction and desulfurization according to claim 1, characterized in that the chlorinated polyethylene rubber CM is 10-15 parts.
    5. The method for producing environment-friendly high-quality ethylene-propylene reclaimed rubber by temperature reduction and desulfurization according to claim 1, characterized in that the paraffin oil is 5-10 parts.
    6. The method for producing environment-friendly high-quality ethylene-propylene reclaimed rubber by temperature reduction and desulfurization according to claim 1, characterized in that the desulfurization regeneration condition refers to the regeneration temperature of 210+5°C and the regeneration time of 1545 min.
LU501593A 2022-03-04 2022-03-04 Method for Producing Environment-friendly High-quality Ethylene-propylene Reclaimed Rubber by Temperature Reduction and Desulfurization LU501593B1 (en)

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