CN108373557B - Preparation method of high-performance regenerated rubber - Google Patents
Preparation method of high-performance regenerated rubber Download PDFInfo
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- CN108373557B CN108373557B CN201711478000.2A CN201711478000A CN108373557B CN 108373557 B CN108373557 B CN 108373557B CN 201711478000 A CN201711478000 A CN 201711478000A CN 108373557 B CN108373557 B CN 108373557B
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L17/00—Compositions of reclaimed rubber
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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
- C08J11/16—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 by treatment with inorganic material
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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
- C08J11/18—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 by treatment with organic material
- C08J11/22—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 by treatment with organic material by treatment with organic oxygen-containing compounds
- C08J11/26—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 by treatment with organic material by treatment with organic oxygen-containing compounds containing carboxylic acid groups, their anhydrides or esters
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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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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/03—Polymer mixtures characterised by other features containing three or more polymers in a blend
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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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- Life Sciences & Earth Sciences (AREA)
- Sustainable Development (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Tires In General (AREA)
- Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)
Abstract
The invention discloses a preparation method of high-performance regenerated rubber, which comprises the following steps: and (3) putting the rubber powder, the softener, the activator, the antioxidant, the modifier and the modified nano montmorillonite into a stirring device provided with a microwave device, stirring, and reacting to obtain the high-performance regenerated rubber. The addition of the nano montmorillonite increases the friction force between colloidal particles, so that the mixing is more sufficient, and meanwhile, due to the existence of the coupling agent, the modified nano montmorillonite can be more uniformly dispersed in the packing layer of the reclaimed rubber. Due to the special lamellar structure of the nano-montmorillonite, the nano-montmorillonite uniformly dispersed in the rubber greatly improves the processing property of the rubber. Secondly, in the vulcanization process of the rubber powder, because ZDA is highly hydroxyl-philic, a hydroxyl-metal ion complex can be formed, the dispersion of the modified nano montmorillonite in the colloid is greatly enhanced, and the service performance of the vulcanized rubber is increased. Therefore, the high-performance reclaimed rubber prepared by the invention has the characteristics of good processability and high strength.
Description
Technical Field
The invention relates to the technical field of material forming processing, in particular to a preparation method of high-performance regenerated rubber.
Background
The main sources of the waste rubber are the production of products such as scrapped tires, rubber tubes, rubber belts, soles, industrial rubber sundries, materials of rubber factories and the like. In recent years, about 100 million tons of waste rubber are generated in China every year, the waste rubber products are not fully utilized, some places use the waste rubber as fuel to be burnt together with coal, so that serious secondary pollution and resource waste are caused, the recovery of the waste rubber not only expands the rubber raw material source and reduces the production cost, but also can protect the environment.
At present, most of vulcanized rubber recovery processes adopt a mechanochemical method, disulfides such as diphenyl disulfide, dibenzyl disulfide and the like are added into waste rubber, the regenerants not only cause harm to the environment, but also can cause part of C-C bonds to be broken when being heated due to the fact that the regenerants contain active sulfur, and the performance of the obtained regenerated rubber is unstable, so that how to stably and efficiently recycle the waste rubber is the development direction of the future rubber industry.
Disclosure of Invention
The invention mainly aims to provide a preparation method of high-performance reclaimed rubber, which has the characteristics of good processability and high strength.
In order to achieve the above purposes, the technical scheme adopted by the invention is as follows:
the invention provides a preparation method of high-performance regenerated rubber, which comprises the following steps: putting 80-120 parts by weight of rubber powder, 6-10 parts by weight of softener, 2-5 parts by weight of activator, 1-3 parts by weight of antioxidant, 2-5 parts by weight of modifier and 6-10 parts by weight of modified nano montmorillonite into a stirring device provided with a microwave device, stirring, and reacting to obtain the high-performance regenerated rubber, wherein the softener is a mixture of naphthenic oil and coumarone resin, the activator is modified stearic acid, and the modifier is zinc diacrylate.
Preferably, the rubber powder is prepared according to the following method: cleaning, airing and grinding waste rubber tires to obtain tread crude rubber powder; and carrying out magnetic separation and iron removal on the tread crude rubber powder for the first time, screening, crushing, and carrying out magnetic separation and iron removal for the second time to obtain rubber powder.
Preferably, the weight ratio of naphthenic oil to coumarone resin is 3: 2.
Preferably, the modified stearic acid is prepared according to the following method: dissolving 8-12 parts by weight of stearic acid in absolute ethyl alcohol, heating and stirring for 10-30min, adding a small amount of coupling agent KH-560 and 4-6 parts by weight of aluminum oxide powder after the stearic acid is fully mixed, reacting for 40-60min, filtering and drying to obtain the modified stearic acid.
Preferably, the heating temperature is 60 ℃.
Preferably, the antioxidant is N-phenyl-N-cyclohexyl-p-phenylenediamine.
Preferably, the modified nano-montmorillonite is prepared according to the following method: dissolving 1 weight part of coupling agent in absolute ethyl alcohol, heating and stirring for 10-15min at 60 ℃, adding 8 weight parts of nano montmorillonite, stirring, reacting for 30-50min, filtering, and drying to obtain the modified nano montmorillonite.
Preferably, the heating temperature is 60 ℃.
Preferably, the stirring time is 40-50 min.
Preferably, the rotational speed of the stirring device is 40 to 60 rpm.
The invention provides a preparation method of high-performance regenerated rubber, which comprises the following steps: putting 80-120 parts by weight of rubber powder, 6-10 parts by weight of softener, 2-5 parts by weight of activator, 1-3 parts by weight of antioxidant, 2-5 parts by weight of modifier and 6-10 parts by weight of modified nano montmorillonite into a stirring device provided with a microwave device, stirring, and reacting to obtain the high-performance regenerated rubber, wherein the softener is a mixture of naphthenic oil and coumarone resin, the activator is modified stearic acid, and the modifier is zinc diacrylate. Compared with the prior art, the addition of the nano montmorillonite increases the friction force between colloidal particles, so that the mixing is more sufficient, and meanwhile, due to the existence of the coupling agent, the modified nano montmorillonite can be more uniformly dispersed in the packing layer of the reclaimed rubber. In addition, due to the special lamellar structure of the nano montmorillonite, the nano montmorillonite uniformly dispersed in the rubber greatly improves the processing performance of the rubber. Secondly, in the vulcanization process of the prepared rubber powder, because ZDA is highly hydroxyl-philic, a hydroxyl-metal ion complex can be formed, the dispersion of the modified nano montmorillonite in the colloid is greatly enhanced, and the service performance of the vulcanized rubber is increased. Therefore, the high-performance reclaimed rubber prepared by the invention has the characteristics of good processability and high strength.
Detailed Description
The following description is presented to disclose the invention so as to enable any person skilled in the art to practice the invention. The preferred embodiments in the following description are given by way of example only, and other obvious variations will occur to those skilled in the art.
The invention provides a preparation method of high-performance regenerated rubber, which comprises the following steps: putting 80-120 parts by weight of rubber powder, 6-10 parts by weight of softener, 2-5 parts by weight of activator, 1-3 parts by weight of antioxidant, 2-5 parts by weight of modifier and 6-10 parts by weight of modified nano montmorillonite into a stirring device provided with a microwave device, stirring, and reacting to obtain the high-performance regenerated rubber, wherein the softener is a mixture of naphthenic oil and coumarone resin, the activator is modified stearic acid, and the modifier is zinc diacrylate.
The invention adopts a microwave stirring desulfurization method to recycle the regenerated rubber, and the energy provided by the microwave can cut off the C-S bond under the premise of not cutting off the main chain of the rubber at a certain temperature, thereby playing the role of desulfurization. The common microwave desulfurization technology has the advantages that the temperature cannot be accurately controlled, so that the impact temperature or temperature fluctuation in the microwave desulfurization process causes poor machining performance of the regenerated rubber.
Preferably, the rubber powder is prepared by the following method: cleaning, airing and grinding waste rubber tires to obtain tread crude rubber powder; and carrying out magnetic separation and iron removal on the tread crude rubber powder for the first time, screening, crushing, and carrying out magnetic separation and iron removal for the second time to obtain rubber powder.
Preferably, the weight ratio of naphthenic oil to coumarone resin is 3: 2.
Preferably, the modified stearic acid is prepared by the following method: dissolving 8-12 parts by weight of stearic acid in absolute ethyl alcohol, heating and stirring for 10-30min, adding a small amount of coupling agent KH-560 and 4-6 parts by weight of aluminum oxide powder after the stearic acid is fully mixed, reacting for 40-60min, filtering and drying to obtain the modified stearic acid. Preferably, the heating temperature is 60 ℃.
Preferably, the antioxidant is N-phenyl-N-cyclohexyl-p-phenylenediamine.
The addition of the nano montmorillonite increases the friction force between colloidal particles, so that the mixing is more sufficient, meanwhile, due to the existence of the coupling agent, the modified nano montmorillonite can be more uniformly dispersed in the packing layer of the reclaimed rubber, and in addition, due to the special lamellar structure of the nano montmorillonite, the nano montmorillonite uniformly dispersed in the rubber greatly improves the processing performance of the rubber.
The modified nano montmorillonite is used as the filler, and the C-C main chain is unstable after the C-S bond is broken due to the addition of the filler, so that the mechanical processing performance is poor.
As a preferred scheme, the modified nano montmorillonite is prepared according to the following method: dissolving 1 weight part of coupling agent in absolute ethyl alcohol, heating and stirring for 10-15min at 60 ℃, adding 8 weight parts of nano montmorillonite, stirring, reacting for 30-50min, filtering, and drying to obtain the modified nano montmorillonite. Preferably, the heating temperature is 60 ℃.
In the vulcanization process of the prepared rubber powder, because ZDA is highly hydroxyl-philic, a hydroxyl-metal ion complex can be formed, the dispersion of the filler in the colloid is greatly enhanced, and the service performance of the vulcanized rubber is increased.
In the preparation process of the high-performance regenerated rubber, the stirring time is preferably 40-50min, and the rotating speed of the stirring equipment is preferably 40-60 rpm.
According to the scheme, the friction force between colloidal particles is increased by adding the nano montmorillonite, so that the mixing is more sufficient, meanwhile, due to the existence of the coupling agent, the modified nano montmorillonite can be more uniformly dispersed in the packing layer of the reclaimed rubber, and in addition, due to the special lamellar structure of the nano montmorillonite, the nano montmorillonite uniformly dispersed in the rubber greatly improves the processing performance of the rubber. Secondly, in the vulcanization process of the prepared rubber powder, because ZDA is highly hydroxyl-philic, a hydroxyl-metal ion complex can be formed, so that the dispersion of the filler in the colloid is greatly enhanced, and the service performance of the vulcanized rubber is increased. Therefore, the high-performance reclaimed rubber prepared by the invention has the characteristics of good processability and high strength.
For further understanding of the present invention, the following embodiments are provided to illustrate the technical solutions of the present invention in detail, and the scope of the present invention is not limited by the following embodiments.
The raw materials and chemical reagents adopted in the embodiment of the invention are all commercially available.
The softener is a mixture of common commercially available naphthenic oil and coumarone resin in a ratio of 3: 2;
the activating agent is modified stearic acid;
the antioxidant is a common commercial antioxidant 4010 (N-phenyl-N-cyclohexyl-p-phenylenediamine);
the coupling agent is KH-560;
the additive is modified nano montmorillonite;
the modifier is zinc diacrylate ZDA (chemically pure) purchased from AlfaAesar.
Example 1
Dissolving 10 parts by weight of stearic acid in 100ml of absolute ethyl alcohol, fully heating and stirring for 10-30min at the heating temperature of 60 ℃, adding a small amount of coupling agent KH-560 and 5 parts by weight of aluminum oxide powder after fully mixing the stearic acid, reacting for 40-60min, filtering and drying after complete reaction to obtain the modified stearic acid.
Dissolving 1 weight part of coupling agent in 100ml of absolute ethyl alcohol, fully heating and stirring for 10-15min at the heating temperature of 60 ℃, adding 8 weight parts of nano-montmorillonite, fully stirring and reacting for 30-50min, filtering and drying after complete reaction to obtain the modified nano-montmorillonite.
Cleaning the waste rubber tires for 10-20min, drying after cleaning, grinding the dried waste rubber tires on a machine table, and collecting tread crude rubber powder.
And carrying out magnetic separation and iron removal on the tread coarse powder to obtain screened tread coarse powder.
And (3) crushing the screened tread coarse powder by a crusher (40-60 meshes), carrying out secondary magnetic separation and iron removal, and packaging the rubber powder.
100 parts by weight of rubber powder, 10 parts by weight of softener, 5 parts by weight of activator, 2 parts by weight of antioxidant, 2 parts by weight of modifier and 10 parts by weight of modified nano montmorillonite are put into a stirring device provided with a microwave device, fully stirred for 45min at the rotating speed of 40-60 r/min, and sucked into a charging hopper by an air suction device for packaging after the stirring is finished.
The tensile strength was 18MPa, the ash content was 12%, the elongation at break was 550%, and the 15-day Mooney change (. DELTA.ML) was 2.
Example 2
Dissolving 10 parts by weight of stearic acid in 100ml of absolute ethyl alcohol, fully heating and stirring for 10-30min at the heating temperature of 60 ℃, adding a small amount of coupling agent KH-560 and 5 parts by weight of aluminum oxide powder after fully mixing the stearic acid, reacting for 40-60min, filtering and drying after complete reaction to obtain the modified stearic acid.
Dissolving 1 weight part of coupling agent in 100ml of absolute ethyl alcohol, fully heating and stirring for 10-15min at the heating temperature of 60 ℃, adding 8 weight parts of nano-montmorillonite, fully stirring and reacting for 30-50min, filtering and drying after complete reaction to obtain the modified nano-montmorillonite.
Cleaning the waste rubber tires for 10-20min, drying after cleaning, grinding the dried waste rubber tires on a machine table, and collecting tread crude rubber powder.
And carrying out magnetic separation and iron removal on the tread coarse powder to obtain screened tread coarse powder.
And (3) crushing the screened tread coarse powder by a crusher (40-60 meshes), carrying out secondary magnetic separation and iron removal, and packaging the rubber powder.
100 parts by weight of rubber powder, 8 parts by weight of softener, 3 parts by weight of activator, 1 part by weight of antioxidant and 8 parts by weight of modified nano montmorillonite of 3 parts by weight of modifier are put into a stirring device provided with a microwave device, fully stirred for 45min at the rotating speed of 40-60 r/min, and sucked into a charging hopper by an air suction device for packaging after the stirring is finished.
The tensile strength was measured to be 15MPa, the ash content was measured to be 10%, the elongation at break was measured to be 500%, and the 15-day Mooney change (. DELTA.ML) was measured to be 1.
Example 3
Dissolving 10 parts by weight of stearic acid in 100ml of absolute ethyl alcohol, fully heating and stirring for 10-30min at the heating temperature of 60 ℃, adding a small amount of coupling agent KH-560 and 5 parts by weight of aluminum oxide powder after fully mixing the stearic acid, reacting for 40-60min, filtering and drying after complete reaction to obtain the modified stearic acid.
Dissolving 1 weight part of coupling agent in 100ml of absolute ethyl alcohol, fully heating and stirring for 10-15min at the heating temperature of 60 ℃, adding 8 weight parts of nano-montmorillonite, fully stirring and reacting for 30-50min, filtering and drying after complete reaction to obtain the modified nano-montmorillonite.
Cleaning the waste rubber tires for 10-20min, drying after cleaning, grinding the dried waste rubber tires on a machine table, and collecting tread crude rubber powder.
And carrying out magnetic separation and iron removal on the tread coarse powder to obtain screened tread coarse powder.
And (3) crushing the screened tread coarse powder by a crusher (40-60 meshes), carrying out secondary magnetic separation and iron removal, and packaging the rubber powder.
100 parts by weight of rubber powder, 6 parts by weight of softener, 2 parts by weight of activator, 1 part by weight of antioxidant, 5 parts by weight of modifier and 6 parts by weight of modified nano montmorillonite are put into a stirring device provided with a microwave device, fully stirred for 45min at the rotating speed of 40-60 r/min, and sucked into a charging hopper by an air suction device for packaging after the stirring is finished.
The tensile strength was measured to be 13MPa, the ash content was measured to be 16%, the elongation at break was measured to be 440%, and the 15-day Mooney change (. DELTA.ML) was measured to be 7.
Comparative example
The preparation procedure of example 1 was used, and the raw materials and properties used are shown in Table 1.
TABLE 1 raw materials and results of performance tests for comparative examples of the present invention
The foregoing shows and describes the general principles, essential features, and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are merely illustrative of the principles of the invention, but that various changes and modifications may be made without departing from the spirit and scope of the invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (1)
1. The preparation method of the high-performance reclaimed rubber is characterized by comprising the following steps of:
putting 80-120 parts by weight of rubber powder, 6-10 parts by weight of softener, 2-5 parts by weight of activator, 1-3 parts by weight of antioxidant, 2-5 parts by weight of modifier and 6-10 parts by weight of modified nano-montmorillonite into a stirring device provided with a microwave device, stirring, reacting to obtain high-performance regenerated rubber,
the softener is a mixture of naphthenic oil and coumarone resin,
the activating agent is modified stearic acid, and the activating agent is modified stearic acid,
the modifier is zinc diacrylate, and the modifier is zinc diacrylate,
the weight ratio of naphthenic oil to coumarone resin is 3:2,
the antioxidant is N-phenyl-N-cyclohexyl-p-phenylenediamine,
the modified nano montmorillonite is prepared by the following method:
dissolving 1 weight part of coupling agent in absolute ethyl alcohol, heating and stirring for 10-15min at 60 ℃, adding 8 weight parts of nano montmorillonite, stirring, reacting for 30-50min, filtering, drying to obtain modified nano montmorillonite,
the rubber powder is prepared by the following method:
cleaning, airing and grinding waste rubber tires to obtain tread crude rubber powder;
the tread crude rubber powder is subjected to magnetic separation for the first time to remove iron, screening and crushing, and magnetic separation for the second time to remove iron, so as to obtain rubber powder,
the modified stearic acid is prepared by the following method:
dissolving 8-12 parts by weight of stearic acid in absolute ethyl alcohol, heating and stirring for 10-30min, adding a small amount of coupling agent KH-560 and 4-6 parts by weight of aluminum oxide powder after the stearic acid is fully mixed, reacting for 40-60min, filtering, drying to obtain modified stearic acid,
the rotating speed of the stirring equipment is 40-60 rpm.
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| CN111995838B (en) * | 2020-07-17 | 2022-11-08 | 中北大学 | Regenerated ABS/HIPS blending material modified by ionic crosslinking and preparation method thereof |
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| CN103435843A (en) * | 2013-08-29 | 2013-12-11 | 中胶橡胶资源再生（青岛）有限公司 | Reclaiming agent, reclaimed rubber prepared therefrom, and preparation method of reclaimed rubber |
| CN105254919A (en) * | 2015-11-10 | 2016-01-20 | 徐州工业职业技术学院 | Method for preparing environment-friendly high-strength tire reclaimed rubber through microwaves |
| CN105295148A (en) * | 2015-10-28 | 2016-02-03 | 贵州安泰再生资源科技有限公司 | Method for preparing reclaimed rubber through waste tire |
| CN105418964A (en) * | 2015-12-28 | 2016-03-23 | 天津海泰环保科技发展有限公司 | Microwave catalytic activation rubber powder composition and preparation method therefor |
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| CN101045799A (en) * | 2007-04-17 | 2007-10-03 | 福建省晋江市陈埭江头茂泰橡塑厂 | Preparation method of reclaimed rubber using microwave desulfurization method |
| CN103435843A (en) * | 2013-08-29 | 2013-12-11 | 中胶橡胶资源再生（青岛）有限公司 | Reclaiming agent, reclaimed rubber prepared therefrom, and preparation method of reclaimed rubber |
| CN105295148A (en) * | 2015-10-28 | 2016-02-03 | 贵州安泰再生资源科技有限公司 | Method for preparing reclaimed rubber through waste tire |
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