CN107868274A - A kind of preparation method of reclaimed rubber - Google Patents
A kind of preparation method of reclaimed rubber Download PDFInfo
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- CN107868274A CN107868274A CN201711420571.0A CN201711420571A CN107868274A CN 107868274 A CN107868274 A CN 107868274A CN 201711420571 A CN201711420571 A CN 201711420571A CN 107868274 A CN107868274 A CN 107868274A
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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
- 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
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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
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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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- Chemical & Material Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
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- Health & Medical Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Polymers & Plastics (AREA)
- Organic Chemistry (AREA)
- Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)
Abstract
The present invention relates to a kind of preparation method of reclaimed rubber, scrap rubber is crushed successively, filtering separation, desulfurization and refining, obtain the reclaimed rubber, the desulfurized step is specially：The coupling agents of KH 570 of scrap rubber after the filtering separation of 100 parts by weight, the rosin softening agent of 10 15 parts by weight, the regeneration activators of G 680 of 23 parts by weight, the activators of RX 680 of 23 parts by weight, the zinc oxide activator of 35 parts by weight and 13 parts by weight are mixed, desulfurization process is carried out under conditions of pressure is 20 30MPa, temperature is 220 320 DEG C, the time of the desulfurization process is 55 60min, then carries out refinement step.The preparation method of the reclaimed rubber of the present invention, which has, ensures the advantages of Mooney viscosity is stable.
Description
Technical field
The present invention relates to rubber-moulding technology, more particularly to a kind of preparation method of reclaimed rubber.
Background technology
Reclaimed rubber be leftover bits cured in being produced using rubber as Raw material processing into, have certain plasticity,
The rubber that can be reused, abbreviation reclaimed rubber.Different by scrap rubber used, reclaimed rubber is divided into cover tire class, inner tube of a tyre class and rubber overshoes class etc..
Reclaimed rubber partly can be used for rubber instead of rubber, to save rubber and carbon black, be also beneficial to improve processing
Some performances of performance and rubber.Regenerative process is scrap rubber in plasticizer (softening agent and activator), oxygen, heat and mechanical shear
Make the moieties chain of vulcanization rubber and the process of crosslinking points fracture under the comprehensive function cut.Softening agent plays expansion and plasticising is made
With conventional has coal tar, pine tar, petroleum line softener, cracked residue.Activator can shorten the recovery time, reduce softening
Agent dosage.Conventional activator is aromatic mercaptans and its zinc salt and aromatic disulfides.Reclaimed rubber production process includes powder
3 processes of broken, regeneration (desulfurization) and refining.Technique mainly has oil process (open steam static method), water/oil method (cooking process), high temperature
Dynamic desulfurization, extruding process, method of chemical treatment, microwave method etc..The manufacture method for the reclaimed rubber that China primarily now applies has oil
Method, water/oil method and high-temperature dynamic desulfurization manufacture reclaimed rubber.
The preparation method of reclaimed rubber of the prior art, for the reclaimed rubber that it is prepared during storage, reclaimed rubber is daily
3 to 4 Mooney points are raised, rises to more than 180 within one month, the problem of Mooney viscosity is unstable be present, subsequent technique performance can be triggered
Difference, it is kneaded the problem of pressure is not in blocks.
The content of the invention
The technical problems to be solved by the invention are：A kind of preparation method of the stable reclaimed rubber of Mooney viscosity is provided.
In order to solve the above-mentioned technical problem, the technical solution adopted by the present invention is：
A kind of preparation method of reclaimed rubber, scrap rubber is crushed successively, filtering separation, desulfurization and refining, obtain institute
Reclaimed rubber is stated, the desulfurized step is specially：By scrap rubber, the rosin of 10-15 parts by weight after the filtering separation of 100 parts by weight
Softening agent, the G-680 regeneration activators of 2-3 parts by weight, the RX-680 activators of 2-3 parts by weight, the zinc oxide of 3-5 parts by weight are lived
The KH-570 coupling agents of agent and 1-3 parts by weight mix, and enter under conditions of pressure is 20-30MPa, temperature is 220-320 DEG C
Row desulfurization process, the time of the desulfurization process is 55-60min, then carries out refinement step.
The beneficial effects of the present invention are：
The raw material of above-mentioned parts by weight is designed, G-680 regeneration activators, RX-680 activators and zinc oxide activator are compounded
Using the composite regenerated activator of effect, and above-mentioned specific weight ratio is designed, composite regenerated activator softens with above-mentioned rosin
After agent, coupling agent are used cooperatively, it can divide living radical in dynamic sweetening process, this high mars free radical can hinder
Only high molecular polymer thermal oxide speed, and can make the desulfurization time of vulcanized rubber powder shorten 8-9 times, and Simultaneous Stabilization vulcanizate divides greatly
The structure of son.The high mars free radical of cracking out, plays a part of acceptor, it with vulcanizate macromolecular in sulfide linkage knot
Close, and then accelerate the cracking destructive process of vulcanized rubber structure, the polymerization once again between rubber molecular chain is prevented, so as to effectively improve
The plasticity of product, reach the purpose of vulcanized rubber powder desulfurization regeneration, the disconnected fracture process of rubber macromolecule chain can be accelerated, had simultaneously
Effect prevent fracture macromolecular further in conjunction with chance, there is provided excellent anti-destructive under hot oxygen environment.So as to be effectively accomplished
The regeneration of waste old；And then, it is ensured that Mooney viscosity is stable.
Embodiment
To describe the technology contents of the present invention, the objects and the effects in detail, it is explained below in conjunction with embodiment.
The design of most critical of the present invention is：G-680 regeneration activators, RX-680 activators and zinc oxide activator are answered
Composite regenerated activator is acted on using, and design the composite regenerated activator and above-mentioned rosin softening agent, coupling agent cooperation to make
With.
The present invention provides a kind of preparation method of reclaimed rubber, scrap rubber is crushed successively, filtering separation, desulfurization and essence
Refining, obtains the reclaimed rubber, the desulfurized step is specially：By the scrap rubber after the filtering separation of 100 parts by weight, 10-15 weights
Measure the rosin softening agent of part, the G-680 regeneration activators of 2-3 parts by weight, the RX-680 activators of 2-3 parts by weight, 3-5 parts by weight
Zinc oxide activator and 1-3 parts by weight KH-570 coupling agents mixing, in pressure be 20-30MPa, temperature be 220-320 DEG C
Under conditions of carry out desulfurization process, the time of the desulfurization process is 55-60min, then carries out refinement step.
It was found from foregoing description, the beneficial effects of the present invention are：
The raw material of above-mentioned parts by weight is designed, G-680 regeneration activators, RX-680 activators and zinc oxide activator are compounded
Using the composite regenerated activator of effect, and above-mentioned specific weight ratio is designed, composite regenerated activator softens with above-mentioned rosin
After agent, coupling agent are used cooperatively, it can divide living radical in dynamic sweetening process, this high mars free radical can hinder
Only high molecular polymer thermal oxide speed, and can make the desulfurization time of vulcanized rubber powder shorten 8-9 times, and Simultaneous Stabilization vulcanizate divides greatly
The structure of son.The high mars free radical of cracking out, plays a part of acceptor, it with vulcanizate macromolecular in sulfide linkage knot
Close, and then accelerate the cracking destructive process of vulcanized rubber structure, the polymerization once again between rubber molecular chain is prevented, so as to effectively improve
The plasticity of product, reach the purpose of vulcanized rubber powder desulfurization regeneration, the disconnected fracture process of rubber macromolecule chain can be accelerated, had simultaneously
Effect prevent fracture macromolecular further in conjunction with chance, there is provided excellent anti-destructive under hot oxygen environment.So as to be effectively accomplished
The regeneration of waste old；And then, it is ensured that Mooney viscosity is stable.
Further, by scrap rubber, rosin softening agent, dipentene regeneration activator, triethylene tetramine softening agent and three second
Hydramine regeneration activator is mixed in digester.
Further, the total content and rosin of the G-680 regeneration activators, RX-680 activators and zinc oxide activator
The ratio of the content of softening agent is (0.8-1):1.
Seen from the above description, it is preferred that G-680 regeneration activators, RX-680 activators and zinc oxide activator it is total
The ratio of content and the content of rosin softening agent is (0.8-1):1, it can further obtain higher tensile strength.
Further, the pressure of the desulfurization process is 25MPa, and temperature is 260 DEG C.
Seen from the above description, it is preferred that the pressure and temperature of above-mentioned desulfurization process can be used, when further shortening desulfurization
Between.
Further, the pulverising step is specially：Waste Crumb rubber is broken to 15-25 mesh sizes.
Seen from the above description, the pulverized size of above-mentioned scrap rubber can improve the physical and mechanical properties of reclaimed rubber, and can
Further help to improve tensile strength (increase rate 1-1.5MPa).
Embodiments of the invention one are：
The preparation method of the reclaimed rubber of the present embodiment, scrap rubber is crushed successively, filtering separation, desulfurization and refining,
The reclaimed rubber is obtained, the desulfurized step is specially：By scrap rubber after the filterings of 100 parts by weight separation, 10 parts by weight
The zinc oxide activation of rosin softening agent, the G-680 regeneration activators of 2 parts by weight, the RX-680 activators of 2 parts by weight, 3 parts by weight
The KH-570 coupling agents of agent and 1 parts by weight are mixed in digester, under conditions of pressure is 20MPa, temperature is 220 DEG C
Desulfurization process is carried out, the time of the desulfurization process is 55min, then carries out refinement step.The pulverising step is specially：Will
Waste Crumb rubber is broken to 15 mesh sizes.
Embodiments of the invention two are：
The preparation method of the reclaimed rubber of the present embodiment, scrap rubber is crushed successively, filtering separation, desulfurization and refining,
The reclaimed rubber is obtained, the desulfurized step is specially：By scrap rubber after the filterings of 100 parts by weight separation, 15 parts by weight
The zinc oxide activation of rosin softening agent, the G-680 regeneration activators of 3 parts by weight, the RX-680 activators of 3 parts by weight, 5 parts by weight
The KH-570 coupling agents of agent and 3 parts by weight are mixed in digester, under conditions of pressure is 30MPa, temperature is 320 DEG C
Desulfurization process is carried out, the time of the desulfurization process is 60min, then carries out refinement step.The pulverising step is specially：Will
Waste Crumb rubber is broken to 25 mesh sizes.
Embodiments of the invention three are：
The preparation method of the reclaimed rubber of the present embodiment, scrap rubber is crushed successively, filtering separation, desulfurization and refining,
The reclaimed rubber is obtained, the desulfurized step is specially：By the scrap rubber after the filtering separation of 100 parts by weight, 10.5 parts by weight
Rosin softening agent, the G-680 regeneration activators of 2.9 parts by weight, the RX-680 activators of 2.9 parts by weight, the oxygen of 4.7 parts by weight
The KH-570 coupling agents for changing zinc activator and 2 parts by weight are mixed in digester, in pressure be 25MPa, temperature be 280 DEG C
Under conditions of carry out desulfurization process, the time of the desulfurization process is 58min, then carries out refinement step.The pulverising step
Specially：Waste Crumb rubber is broken to 20 mesh sizes.
Performance test
The reclaimed rubber that embodiment one to embodiment three is prepared successively according to《GB/T 13460-2008 reclaimed rubbers》
In standard respectively after preparation at 2 days, 3 days and 30 days carry out Mooney viscosity performance test.Above-mentioned GB/T 13460-2008 marks
The standard value of accurate Mooney viscosity (1+4) 100 is：≤85.
Measuring result is：
Mooney viscosity of the reclaimed rubber that embodiment one prepares respectively after preparation at 2 days, 3 days and 30 days is followed successively by
45.6、48.1、51.1。
Mooney viscosity of the reclaimed rubber that embodiment two prepares respectively after preparation at 2 days, 3 days and 30 days is followed successively by
46.6、48.1、50.1。
Mooney viscosity of the reclaimed rubber that embodiment three prepares respectively after preparation at 2 days, 3 days and 30 days is followed successively by
45.2、45.8、49.5。
In summary, the preparation method of reclaimed rubber provided by the invention, which has, ensures the advantages of Mooney viscosity is stable.
Embodiments of the invention are the foregoing is only, are not intended to limit the scope of the invention, it is every to utilize this hair
The equivalents that bright description is made, or the technical field of correlation is directly or indirectly used in, similarly it is included in this hair
In bright scope of patent protection.
Claims (5)
1. a kind of preparation method of reclaimed rubber, scrap rubber is crushed successively, filtering separation, desulfurization and refining, described in acquisition
Reclaimed rubber, it is characterised in that the desulfurized step is specially：By the scrap rubber after the filtering separation of 100 parts by weight, 10-15 weights
Measure the rosin softening agent of part, the G-680 regeneration activators of 2-3 parts by weight, the RX-680 activators of 2-3 parts by weight, 3-5 parts by weight
Zinc oxide activator and 1-3 parts by weight KH-570 coupling agents mixing, in pressure be 20-30MPa, temperature be 220-320 DEG C
Under conditions of carry out desulfurization process, the time of the desulfurization process is 55-60min, then carries out refinement step.
2. the preparation method of reclaimed rubber according to claim 1, it is characterised in that by scrap rubber, rosin softening agent, double penta
Alkene regeneration activator, triethylene tetramine softening agent and triethanolamine regeneration activator are mixed in digester.
3. the preparation method of reclaimed rubber according to claim 1, it is characterised in that the G-680 regeneration activators, RX-
The total content of 680 activators and zinc oxide activator and the ratio of the content of rosin softening agent are (0.8-1):1.
4. the preparation method of reclaimed rubber according to claim 1, it is characterised in that the pressure of the desulfurization process is
25MPa, temperature are 260 DEG C.
5. the preparation method of reclaimed rubber according to claim 1, it is characterised in that the pulverising step is specially：Will be useless
Rubber pulverizing is to 15-25 mesh sizes.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711420571.0A CN107868274A (en) | 2017-12-25 | 2017-12-25 | A kind of preparation method of reclaimed rubber |
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| CN201711420571.0A CN107868274A (en) | 2017-12-25 | 2017-12-25 | A kind of preparation method of reclaimed rubber |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109796625A (en) * | 2018-12-28 | 2019-05-24 | 南京绿金人橡塑高科有限公司 | A kind of environmental friendly regenerated dose and preparation method thereof for rubber regeneration |
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| CN102634062A (en) * | 2012-04-28 | 2012-08-15 | 徐州工业职业技术学院 | Method for preparing high-tenacity reclaimed rubber by adding coupling agent |
| CN103937059A (en) * | 2014-04-10 | 2014-07-23 | 青岛通力橡胶科技有限公司 | Environment-friendly reclaimed rubber with high tenacity and stable Mooney viscosity and preparation method thereof |
| CN104672489A (en) * | 2013-11-29 | 2015-06-03 | 招远市东晟橡胶制品有限公司 | Waste rubber desulfurization technology |
| CN104890165A (en) * | 2015-05-13 | 2015-09-09 | 福建省邵武市恒晖橡胶再生有限公司 | Regenerated rubber formula test method, and regenerated rubber desulphurization machine |
-
2017
- 2017-12-25 CN CN201711420571.0A patent/CN107868274A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102634062A (en) * | 2012-04-28 | 2012-08-15 | 徐州工业职业技术学院 | Method for preparing high-tenacity reclaimed rubber by adding coupling agent |
| CN104672489A (en) * | 2013-11-29 | 2015-06-03 | 招远市东晟橡胶制品有限公司 | Waste rubber desulfurization technology |
| CN103937059A (en) * | 2014-04-10 | 2014-07-23 | 青岛通力橡胶科技有限公司 | Environment-friendly reclaimed rubber with high tenacity and stable Mooney viscosity and preparation method thereof |
| CN104890165A (en) * | 2015-05-13 | 2015-09-09 | 福建省邵武市恒晖橡胶再生有限公司 | Regenerated rubber formula test method, and regenerated rubber desulphurization machine |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109796625A (en) * | 2018-12-28 | 2019-05-24 | 南京绿金人橡塑高科有限公司 | A kind of environmental friendly regenerated dose and preparation method thereof for rubber regeneration |
| CN109796625B (en) * | 2018-12-28 | 2021-11-16 | 南京绿金人橡塑高科有限公司 | Environment-friendly regenerant for rubber regeneration and preparation method thereof |
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