CN113337002B - Environment-friendly waste rubber regenerant and preparation method thereof - Google Patents

Environment-friendly waste rubber regenerant and preparation method thereof Download PDF

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Publication number
CN113337002B
CN113337002B CN202110631758.5A CN202110631758A CN113337002B CN 113337002 B CN113337002 B CN 113337002B CN 202110631758 A CN202110631758 A CN 202110631758A CN 113337002 B CN113337002 B CN 113337002B
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parts
environment
waste rubber
stirring
rubber
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CN113337002A (en
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常明丰
刘志玲
张艺行
裴建中
张久鹏
熊锐
朱玉芳
熊建波
范志宏
刘虎军
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Taizhou Dongdian Rubber & Plastic Co ltd
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Changan University
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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
    • C08J11/28—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 compounds containing nitrogen, sulfur or phosphorus
    • 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
    • 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
    • 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
    • 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
    • C08J2319/00—Characterised by the use of rubbers not provided for in groups C08J2307/00 - C08J2317/00
    • 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

Abstract

The invention belongs to the technical field of waste rubber regeneration, and provides an environment-friendly waste rubber regenerant and a preparation method thereof, wherein the regenerant consists of an activator, a softener and a tackifier which are uniformly mixed; the weight portions of the components are as follows: 10-25 parts of activating agent, 60-80 parts of softening agent and 10-15 parts of adhesion promoter; the activator is prepared from octadecylamine, deodorized distillate, stearic acid and an accelerator NS in mass ratio: 2 to 5:5 to 11.25:1 to 4: and 2 to 7.5 percent of the components are evenly mixed. The activating agent, the softening agent and the adhesion promoter adopted by the invention are applied to the regeneration of the waste rubber, so that the odor is small, the emission of toxic gas in the rubber regeneration process is reduced, the swelling property of the rubber is good, the stability is good and the plasticizing effect is good when the activating agent, the softening agent and the adhesion promoter are applied to the regeneration of the waste rubber; the polycyclic aromatic hydrocarbon meets the technical requirements of domestic and foreign environmental protection, has good mechanical properties, simple preparation process, easy control of products, no pollution in the preparation process and is beneficial to large-scale industrial production and application.

Description

Environment-friendly waste rubber regenerant and preparation method thereof
Technical Field
The invention belongs to the technical field of waste rubber regeneration, and particularly relates to an environment-friendly waste rubber regenerant and a preparation method thereof.
Background
With the rapid development of modern industry, the rubber industry is rapidly developed, and the method is widely applied to the fields of tires, soles, latex products and the like, the consumption of rubber is continuously increased, the situation of shortage of rubber resources is aggravated, and simultaneously, a large amount of generated waste rubber also aggravates the pollution to the environment, so that the effective treatment and comprehensive utilization of the waste rubber are not only beneficial to environmental protection, but also can regenerate precious rubber resources. China is the largest waste rubber producer, wherein the total amount of the waste tire rubber is more than 70% of the total amount of the waste rubber. According to the data, in 2020, the number of used tires in China is about 12.65 hundred million, and the number of waste tires reaches 3.80 hundred million. In general, these scrap tire rubbers are discarded, landfilled or incinerated in large quantities, which not only results in a large occupation of land resources, but also creates serious environmental problems. The recycling of the waste wheel rubber can realize the recycling of the waste rubber and reduce the adverse effect of the waste rubber on the environment. Therefore, the method for recycling the waste tire rubber has important significance for long-term healthy development of the rubber industry in China.
Waste rubber belongs to thermosetting polymer materials, is insoluble under conventional conditions and is difficult to degrade under natural conditions, and reclaimed rubber is regenerated rubber in waste rubber and plays an important role in a raw rubber formula system as a filler. The addition of reclaimed rubber can reduce physical and mechanical properties of the raw rubber, such as tensile strength, modulus, tear strength and the like, but can provide characteristics which are not available for the raw rubber. On one hand, the mixing time can be shortened, and the energy consumption of the sizing material in the mixing process can be reduced; secondly, the feeding speed is higher in the extrusion or calendering process, and when the reclaimed rubber is contained in the rubber compound, the problems of extrusion expansion and calendering shrinkage can be avoided; thirdly, during vulcanization, the reclaimed rubber can play a role in ageing resistance, and the effect is better than that of adding the anti-ageing agent. Therefore, the recovery and regeneration of the waste rubber have good economic benefit and environmental protection benefit, and have wide application prospect and great development potential. If the method can be based on the existing waste rubber regeneration technology, comprehensive and deep research is conducted from the aspects of manufacturability, environmental protection, economy and the like, or some promising new regeneration technologies are further perfected, a method capable of truly and effectively recycling the waste rubber is sought, an updated and advanced technology is created, and the progress of the waste rubber regeneration technology and the development of the reclaimed rubber industry are greatly promoted. The regeneration of the waste rubber is that the waste rubber damages the reticular crosslinked structure of the waste rubber under the conditions of heat, mechanical force and the like, so that the rubber has certain plasticity and processability again. The rubber regeneration method is classified into physical regeneration, chemical regeneration, biological regeneration, etc. At present, the comprehensive utilization of the two or more methods for regenerating the waste rubber becomes a common choice.
The regeneration of waste rubber is realized by a mechanochemical method in the waste rubber regeneration industry, namely, a certain amount of regenerant is added under the conditions of medium and high temperature (more than 200 ℃) and high pressure (2-4 MPa), so that the regenerant acts on sulfur-containing bonds such as monosulfur bonds, disulfide bonds and the like in the waste rubber, and meanwhile, shearing force is applied to the rubber, so that the desulfurization regeneration of the waste rubber is realized. Although the method can obtain the reclaimed rubber with excellent mechanical properties and processing properties, the energy consumption in the preparation process is high, and the processing aids such as the regenerant, the anti-aging agent and the like added in the regeneration process are easy to release a large amount of toxic and harmful gases under the high-temperature condition, so that the environment is polluted. At present, most of the traditional regenerants are prepared by mixing sulfide activators (420, 480, mercaptan and the like), non-environment-friendly softeners (coal tar, aromatic hydrocarbon and the like) and the like in a certain proportion, and most of the regenerants have the defects of high toxicity, bad smell and the like, and reclaimed rubber produced by using the regenerants has the defects of high smell, high content of harmful substances, easy yellowing and difficulty in meeting the technical requirements of current production environment protection. For example: the activators in the traditional regenerants are mostly sulfides such as mercaptan, thiophenol and the like containing mercapto structures, and have excellent regenerability, but have toxicity and chemical reaction in the regeneration process to generate a large amount of toxic and harmful gases (H) 2 S、SO 2 Etc.) seriously harms the environment and the health of practitioners; the softener coal tar, aromatic hydrocarbon oil and the like have good cost performance and good regeneration effect, but have higher types and contents of harmful components, contain a large amount of polycyclic aromatic hydrocarbon and contain cancerogenic substances such as benzopyrene, and do not accord with the regeneration industry of the rubber at home and abroadThe environmental protection technical requirement of raw rubber severely restricts the application of reclaimed rubber in the field of rubber products.
Disclosure of Invention
The invention aims to provide an environment-friendly waste rubber regenerant with small smell, no toxicity, small pollution and good regeneration effect, and also provides a preparation method of the environment-friendly waste rubber regenerant with simple process and low cost, aiming at the defects of large smell, toxicity, high pollution and the like of the existing rubber regenerant.
The invention aims at providing an environment-friendly waste rubber regenerant, which consists of an activator, a softener and a tackifier which are uniformly mixed; the weight portions of the components are as follows: 10-25 parts of activating agent, 60-80 parts of softening agent and 10-15 parts of adhesion promoter; the activator is prepared from octadecylamine, deodorized distillate, stearic acid and an accelerator NS in mass ratio: 2 to 5:5 to 11.25:1 to 2.5:2 to 7.5 are evenly mixed.
Preferably, the deodorized distillate is one or more of soybean oil deodorized distillate, rapeseed oil deodorized distillate and linseed oil deodorized distillate.
Preferably, the softener is one or more of waste silicone oil, swill-cooked dirty oil and rice bran oil.
Preferably, the adhesion promoter is one or a combination of more than one of waste epoxidized soybean oil, waste epoxidized linseed oil and rosin.
The second purpose of the invention is to provide a preparation method of the environment-friendly waste rubber regenerant, which comprises the following steps:
s1, weighing all raw material components for preparing the regenerant according to a proportion; mixing the components of the softener according to the proportion, and uniformly stirring to obtain a mixture;
s2, heating the mixture in the step S1, sequentially adding an activating agent and a tackifier into the mixture, and stirring and dispersing at the constant temperature of 110-130 ℃ to obtain a mixed product;
and S3, uniformly mixing and stirring the mixed product in the step S2, and cooling to room temperature to obtain the environment-friendly waste rubber regenerant.
Preferably, in S1, the stirring speed is 500-1000 r/min, and the stirring time is 10-30 min.
Preferably, in S2, the heating temperature is 100 to 150 ℃.
Preferably, in S2, the stirring speed is 700-1300 r/min, and the stirring time is 10-30 min.
Compared with the prior art, the invention has the beneficial effects that:
1. the regenerant prepared from the activator component is applied to the regeneration of waste rubber, has small smell, reduces the emission of toxic gas in the rubber regeneration process, and is green, safe and good in effect.
2. The softener component adopted by the invention has good swelling property and low volatility to rubber; the adhesion promoter component has good stability and good plasticizing effect when applied to the regeneration of waste rubber. The regenerated rubber produced by the prepared regenerated agent has low volatility, small smell and good mechanical property, and meets the domestic and foreign environmental protection technical requirements through the interaction among the activating agent, the softening agent and the adhesion promoter.
3. The regenerant prepared by the invention provides an effective way for recycling waste grease, and has the advantages of wide raw material sources, low cost, environmental protection, small smell, safety and innocuity; the preparation process is simple, the product is easy to control, the preparation process is pollution-free, the storage is easy, the price is low, and the preparation process is favorable for large-scale industrial production and application.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described in the following in conjunction with the embodiments of the present invention, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
It should be noted that the technical terms used in the present invention are only for describing specific embodiments, and are not intended to limit the scope of the present invention, and various raw materials, reagents, instruments and equipment used in the following embodiments of the present invention may be purchased commercially or prepared by existing methods unless otherwise specifically described. In the examples of the present invention, 1 part by weight means 1g.
Example 1
The environment-friendly waste rubber regenerant is prepared by weighing the following main raw materials:
2 parts of octadecylamine, 2.5 parts of soybean oil deodorization distillate, 2.5 parts of rapeseed oil deodorization distillate, 1 part of stearic acid, 2 parts of accelerator NS, 40 parts of swill-cooked dirty oil, 40 parts of rice bran oil, 5 parts of waste epoxidized soybean oil and 5 parts of waste epoxidized linseed oil.
The preparation process of the environment-friendly waste rubber regenerant comprises the following steps: (1) Weighing 2 parts of octadecylamine, 2.5 parts of soybean oil deodorization distillate, 2.5 parts of rapeseed oil deodorization distillate, 1 part of stearic acid and 2 parts of accelerator NS, mixing, and stirring at a stirring rate of 1000r/min for 10min to obtain a softener mixture; (2) Heating the softener mixture to 110 ℃, sequentially heating 40 parts of swill-cooked dirty oil, 40 parts of rice bran oil, 5 parts of waste epoxidized soybean oil and 5 parts of waste epoxidized linseed oil into the softener mixture, heating to 120 ℃, keeping the temperature constant, and stirring and dispersing for 10min at the stirring rate of 800r/min to obtain a mixed product; (3) And then adjusting the stirring speed to 1000r/min, stirring the obtained mixed product for 10min, and naturally cooling to room temperature to obtain the environment-friendly waste rubber regenerant.
Example 2
The environment-friendly waste rubber regenerant is prepared by weighing the following main raw materials:
3 parts of octadecylamine, 3.375 parts of soybean oil deodorization distillate, 3.375 parts of rapeseed oil deodorization distillate, 2.25 parts of stearic acid, 5 parts of accelerator NS, 50 parts of swill-cooked dirty oil, 25 parts of waste silicone oil, 5 parts of waste epoxidized soybean oil and 5 parts of waste epoxidized linseed oil.
The preparation process of the environment-friendly waste rubber regenerant comprises the following steps: (1) Weighing and mixing 3 parts of octadecylamine, 3.375 parts of soybean oil deodorization distillate, 3.375 parts of rapeseed oil deodorization distillate, 2.25 parts of stearic acid and 5 parts of accelerator NS, and stirring at a stirring rate of 800r/min for 15min to obtain a softener mixture; (2) Heating the softener mixture to 120 ℃, sequentially heating 50 parts of swill-cooked dirty oil, 25 parts of waste silicone oil, 5 parts of waste epoxidized soybean oil and 5 parts of waste epoxidized linseed oil into the softener mixture, and stirring and dispersing for 15min at the constant temperature of 120 ℃ at the stirring rate of 900r/min to obtain a mixed product; (3) And then adjusting the stirring speed to 1500r/min, stirring the obtained mixed product for 15min, and naturally cooling to room temperature to obtain the environment-friendly waste rubber regenerant.
Example 3
The environment-friendly waste rubber regenerant is prepared by weighing the following main raw materials:
4 parts of octadecylamine, 4 parts of soybean oil deodorization distillate, 4 parts of rapeseed oil deodorization distillate, 4 parts of stearic acid, 4 parts of accelerator NS, 50 parts of rice bran oil, 25 parts of waste silicone oil, 5 parts of waste epoxidized soybean oil and 5 parts of rosin.
The preparation process of the environment-friendly waste rubber regenerant comprises the following steps: (1) 4 parts of octadecylamine, 4 parts of soybean oil deodorization distillate, 4 parts of rapeseed oil deodorization distillate, 4 parts of stearic acid and 4 parts of accelerator NS, and stirring for 30min at a stirring rate of 500r/min to obtain a softener mixture; (2) Heating the softener mixture to 130 ℃, sequentially heating 50 parts of rice bran oil, 25 parts of waste silicone oil, 5 parts of waste epoxidized soybean oil and 5 parts of rosin into the softener mixture, cooling to 120 ℃, keeping the temperature constant, and stirring and dispersing for 15min at the stirring rate of 900r/min to obtain a mixed product; (3) And then adjusting the stirring speed to 1500r/min, stirring the obtained mixed product for 15min, and naturally cooling to room temperature to obtain the environment-friendly waste rubber regenerant.
Example 4
The environment-friendly waste rubber regenerant is prepared by weighing the following main raw materials:
5 parts of octadecylamine, 5.625 parts of soybean oil deodorization distillate, 5.625 parts of rapeseed oil deodorization distillate, 2.5 parts of stearic acid, 6.25 parts of accelerator NS, 65 parts of swill-cooked dirty oil and 10 parts of waste epoxidized soybean oil.
The preparation process of the environment-friendly waste rubber regenerant comprises the following steps: (1) 5 parts of octadecylamine, 5.625 parts of soybean oil deodorization distillate, 5.625 parts of rapeseed oil deodorization distillate, 2.5 parts of stearic acid and 6.25 parts of accelerator NS are mixed, and stirred for 15min at a stirring rate of 600r/min to obtain a softener mixture; (2) Heating the softener mixture to 140 ℃, sequentially heating 65 parts of swill-cooked dirty oil and 10 parts of waste epoxidized soybean oil into the softener mixture, cooling to 110 ℃, keeping the constant temperature, and stirring and dispersing for 20min at the stirring rate of 1000r/min to obtain a mixed product; (3) And then adjusting the stirring speed to 2000r/min, stirring the obtained mixed product for 20min, and naturally cooling to room temperature to obtain the environment-friendly waste rubber regenerant.
Example 5
The environment-friendly waste rubber regenerant is prepared by weighing the following main raw materials:
5 parts of octadecylamine, 5 parts of soybean oil deodorization distillate, 5 parts of rapeseed oil deodorization distillate, 2.5 parts of stearic acid, 7.5 parts of accelerator NS, 60 parts of waste silicone oil and 15 parts of waste epoxy linseed oil.
The preparation process of the environment-friendly waste rubber regenerant comprises the following steps: (1) 5 parts of octadecylamine, 5 parts of soybean oil deodorization distillate, 5 parts of rapeseed oil deodorization distillate, 2.5 parts of stearic acid and 7.5 parts of accelerator NS are mixed and stirred for 15min at a stirring rate of 800r/min to obtain a softener mixture; (2) Heating the softener mixture to 150 ℃, sequentially heating 60 parts of waste silicone oil and 15 parts of waste epoxy linseed oil into the softener mixture, cooling to 120 ℃, keeping the temperature constant, and stirring and dispersing for 25min at the stirring rate of 1100r/min to obtain a mixed product; (3) And then adjusting the stirring speed to 2500r/min, stirring the obtained mixed product for 25min, and naturally cooling to room temperature to obtain the environment-friendly waste rubber regenerant.
Example 6
The environment-friendly waste rubber regenerant is prepared by weighing the following main raw materials:
2 parts of octadecylamine, 2.5 parts of soybean oil deodorization distillate, 2.5 parts of rapeseed oil deodorization distillate, 1 part of stearic acid, 2 parts of accelerator NS, 40 parts of swill-cooked dirty oil, 40 parts of rice bran oil, 5 parts of waste epoxidized soybean oil and 5 parts of waste epoxidized linseed oil.
The preparation process of the environment-friendly waste rubber regenerant comprises the following steps: (1) Weighing 2 parts of octadecylamine, 2.5 parts of soybean oil deodorization distillate, 2.5 parts of rapeseed oil deodorization distillate, 1 part of stearic acid and 2 parts of accelerator NS, mixing, and stirring at a stirring rate of 1000r/min for 10min to obtain a softener mixture; (2) Heating the softener mixture to 150 ℃, sequentially heating 40 parts of swill-cooked dirty oil, 40 parts of rice bran oil, 5 parts of waste epoxidized soybean oil and 5 parts of waste epoxidized linseed oil into the softener mixture, cooling to 120 ℃, keeping the temperature constant, and stirring and dispersing for 30min at the stirring rate of 700r/min to obtain a mixed product; (3) And then adjusting the stirring speed to 1000r/min, stirring the obtained mixed product for 30min, and naturally cooling to room temperature to obtain the environment-friendly waste rubber regenerant.
Example 7
The environment-friendly waste rubber regenerant is prepared by weighing the following main raw materials:
3 parts of octadecylamine, 3.375 parts of soybean oil deodorization distillate, 3.375 parts of rapeseed oil deodorization distillate, 2.25 parts of stearic acid, 3 parts of accelerator NS, 45 parts of swill-cooked dirty oil, 15 parts of waste silicone oil, 15 parts of rice bran oil, 5 parts of waste epoxidized soybean oil and 5 parts of waste epoxidized linseed oil.
The preparation process of the environment-friendly waste rubber regenerant comprises the following steps: (1) Weighing and mixing 3 parts of octadecylamine, 3.375 parts of soybean oil deodorization distillate, 3.375 parts of rapeseed oil deodorization distillate, 2.25 parts of stearic acid and 3 parts of accelerator NS, and stirring at a stirring rate of 800r/min for 15min to obtain a softener mixture; (2) Heating the softener mixture to 120 ℃, sequentially heating 30 parts of swill-cooked dirty oil, 30 parts of waste silicone oil, 5 parts of waste epoxidized soybean oil and 5 parts of waste epoxidized linseed oil into the softener mixture, heating to 130 ℃ and keeping constant temperature, and stirring and dispersing for 10min at a stirring rate of 1300r/min to obtain a mixed product; (3) And then adjusting the stirring speed to 3000r/min, stirring the obtained mixed product for 10min, and naturally cooling to room temperature to obtain the environment-friendly waste rubber regenerant.
Example 8
The environment-friendly waste rubber regenerant is prepared by weighing the following main raw materials:
5 parts of octadecylamine, 5 parts of soybean oil deodorization distillate, 5 parts of rapeseed oil deodorization distillate, 2.5 parts of stearic acid, 7.5 parts of accelerator NS, 60 parts of waste silicone oil and 15 parts of waste epoxy linseed oil.
The preparation process of the environment-friendly waste rubber regenerant comprises the following steps: (1) 5 parts of octadecylamine, 5 parts of soybean oil deodorization distillate, 5 parts of rapeseed oil deodorization distillate, 2.5 parts of stearic acid and 7.5 parts of accelerator NS are mixed and stirred for 20min at a stirring rate of 700r/min to obtain a softener mixture; (2) Heating the softener mixture to 130 ℃, sequentially heating 60 parts of waste silicone oil and 15 parts of waste epoxy linseed oil into the softener mixture, cooling to 120 ℃, keeping the temperature constant, and stirring and dispersing for 15min at the stirring rate of 1100r/min to obtain a mixed product; (3) And then adjusting the stirring speed to 2000r/min, stirring the obtained mixed product for 20min, and naturally cooling to room temperature to obtain the environment-friendly waste rubber regenerant.
Comparative example 1
(1) Weighing 2 parts of octadecylamine, 2.5 parts of soybean oil deodorization distillate, 2.5 parts of rapeseed oil deodorization distillate, 1 part of stearic acid and 2 parts of accelerator NS, mixing, and stirring at a stirring rate of 1000r/min for 10min to obtain a softener mixture; (2) Heating the softener mixture to 110 ℃, sequentially heating 80 parts of aromatic oil, 5 parts of waste epoxidized soybean oil and 5 parts of waste epoxidized linseed oil into the softener mixture, heating to 120 ℃, keeping the temperature constant, and stirring and dispersing for 10min at the stirring rate of 800r/min to obtain a mixed product; (3) And then adjusting the stirring speed to 1000r/min, stirring the obtained mixed product for 10min, and naturally cooling to room temperature to obtain the environment-friendly waste rubber regenerant.
Comparative example 2
(1) Weighing and mixing 3 parts of octadecylamine, 3.375 parts of soybean oil deodorization distillate, 3.375 parts of rapeseed oil deodorization distillate, 2.25 parts of stearic acid and 5 parts of accelerator NS, and stirring at a stirring rate of 800r/min for 15min to obtain a softener mixture; (2) Heating the softener mixture to 120 ℃, sequentially heating 75 parts of aromatic oil, 5 parts of waste epoxidized soybean oil and 5 parts of waste epoxidized linseed oil into the softener mixture, and stirring and dispersing for 15min at the constant temperature of 120 ℃ at the stirring rate of 900r/min to obtain a mixed product; (3) And then adjusting the stirring speed to 1500r/min, stirring the obtained mixed product for 15min, and naturally cooling to room temperature to obtain the environment-friendly waste rubber regenerant.
Comparative example 3
(1) 5 parts of octadecylamine, 5 parts of soybean oil deodorization distillate, 5 parts of rapeseed oil deodorization distillate, 2.5 parts of stearic acid and 7.5 parts of accelerator NS are mixed and stirred for 15min at a stirring rate of 800r/min to obtain a softener mixture; (2) Heating the softener mixture to 150 ℃, sequentially heating 60 parts of aromatic oil and 15 parts of waste epoxy linseed oil into the softener mixture, cooling to 120 ℃, keeping the temperature constant, and stirring and dispersing for 25min at the stirring rate of 1100r/min to obtain a mixed product; (3) And then adjusting the stirring speed to 2500r/min, stirring the obtained mixed product for 25min, and naturally cooling to room temperature to obtain the environment-friendly waste rubber regenerant.
The regenerants prepared in examples 1 to 8 and comparative examples 1 to 3 were added to the same type of waste rubber, and the preparation method thereof was as follows: (1) Adding the waste tire rubber powder and the regenerant into a high-speed mixer according to the mass ratio of 100:15 for premixing for 10min, wherein the high-speed mixer is set at the temperature of 100 ℃ and the speed of 1500r/min; (2) Adding the premix into an internal mixer with the volume of 2L, setting the rotating speed to be 32r/min, keeping the regeneration temperature to be 200 ℃, and cooling the discharged material to room temperature after keeping for 15min, wherein the regenerated material is reclaimed rubber; (3) The premix exiting the internal mixer was subjected to a thin-pass plastication on an open mill, followed by the addition of the other components in steps, wherein the premix: vulcanization accelerator TBBS: znO: stearic acid: the mass ratio of the sulfur is 300:2.4:7.5:1.0:3.5, mixing uniformly, and then slicing; (4) vulcanization test piece: vulcanizing the mixed rubber material in a flat vulcanizing machine through a die, wherein the vulcanizing temperature is 165 ℃, the vulcanizing time is 20min, the pressure is 10-13 MPa, and the performance test is performed after the vulcanized test piece is parked for 24 hours.
The prepared rubber product is tested, and the test comprises whether the tensile strength, the elongation at break performance reference GB/T528-2009, the Mooney viscosity reference GB/T1232.1-2000, the polycyclic aromatic hydrocarbon content (8 items) reference HG/T3837-2008 and the reclaimed rubber environmental protection requirement meet the technical requirements of the domestic and foreign rubber product environmental protection regulations. The performance standard of the reclaimed rubber produced by the reclaiming agent is GB/T13460-2016 reclaimed rubber (tire reclaimed rubber R-TW) national standard technical requirement; the reclaimed rubber performance test was prepared as in table 1 using the reclaimed agents prepared in examples 1 to 8 and comparative examples 1 to 3.
TABLE 1 Performance test of reclaimed rubber prepared using the regenerates prepared in examples 1 to 8 and comparative examples 1 to 3
Figure BDA0003103946050000091
Figure BDA0003103946050000101
As shown by the test results in Table 1, compared with the reclaimed rubber prepared by adding aromatic oil as a softener, the reclaimed rubber prepared by adding aromatic oil as a softener has extremely high content of the reclaimed rubber ring aromatic hydrocarbon, which indicates that the reclaimed rubber ring aromatic hydrocarbon prepared by adding aromatic oil as a softener has high content of harmful substances, high toxicity and bad smell, and the polycyclic aromatic hydrocarbon contains cancerogenic substances such as benzopyrene.
It should be noted that, when numerical ranges are referred to in the present invention, it should be understood that two endpoints of each numerical range and any numerical value between the two endpoints are optional, and because the adopted step method is the same as the embodiment, in order to prevent redundancy, the present invention describes a preferred embodiment. While preferred embodiments of the present invention have been described, additional variations and modifications in those embodiments may occur to those skilled in the art once they learn of the basic inventive concepts. It is therefore intended that the following claims be interpreted as including the preferred embodiments and all such alterations and modifications as fall within the scope of the invention.
It will be apparent to those skilled in the art that various modifications and variations can be made to the present invention without departing from the spirit or scope of the invention. Thus, it is intended that the present invention also include such modifications and alterations insofar as they come within the scope of the appended claims or the equivalents thereof.

Claims (7)

1. An environment-friendly waste rubber regenerating agent is characterized by comprising an activating agent, a softening agent and a tackifier which are uniformly mixed; the weight portions of the components are as follows: 10-25 parts of activating agent, 60-80 parts of softening agent and 10-15 parts of adhesion promoter; the activator is prepared from octadecylamine, deodorized distillate, stearic acid and an accelerator NS in mass ratio: 2 to 5:5 to 11.25:1 to 4:2 to 7.5 are evenly mixed;
the deodorized distillate is one or more of soybean oil deodorized distillate, rapeseed oil deodorized distillate and linseed oil deodorized distillate;
the softener is one or a combination of more than one of waste silicone oil, swill-cooked dirty oil and rice bran oil.
2. The environment-friendly waste rubber regenerant according to claim 1, wherein the adhesion promoter is one or a combination of more of waste epoxidized soybean oil, waste epoxidized linseed oil and rosin.
3. The method for preparing the environment-friendly waste rubber regenerant as claimed in claim 1, which is characterized by comprising the following steps:
s1, weighing all raw material components for preparing the regenerant according to a proportion; mixing the components of the softener according to the proportion, and uniformly stirring to obtain a mixture;
s2, heating the mixture in the step S1, sequentially adding an activating agent and a tackifier into the mixture, and stirring and dispersing at the constant temperature of 110-130 ℃ to obtain a mixed product;
and S3, uniformly mixing and stirring the mixed product in the step S2, and cooling to room temperature to obtain the environment-friendly waste rubber regenerant.
4. The method for preparing the environment-friendly waste rubber regenerant according to claim 3, wherein in S1, the stirring speed is 500-1000 r/min and the stirring time is 10-30 min.
5. The method for preparing an environment-friendly waste rubber regenerant according to claim 4, wherein in S2, the heating temperature is 100-150 ℃.
6. The method for preparing the environment-friendly waste rubber regenerant according to claim 5, wherein in S2, the stirring speed is 700-1300 r/min and the stirring time is 10-30 min.
7. The method for preparing the environment-friendly waste rubber regenerant according to claim 6, wherein in S3, the stirring speed is 1000-3000 r/min, and the stirring time is 10-30 min.
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Publication number Priority date Publication date Assignee Title
CN102250396A (en) * 2010-05-21 2011-11-23 徐建雄 Reclaimed rubber process method special for high-temperature steam method
CN102807692A (en) * 2012-08-29 2012-12-05 莱芜市福泉橡胶有限公司 Softener for producing regenerated rubber
CN103044736A (en) * 2012-12-21 2013-04-17 焦作市弘瑞橡胶有限责任公司 Method for producing rubber auxiliaries
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