CN108373557A - A kind of preparation method of high-performance reclaimed rubber - Google Patents

A kind of preparation method of high-performance reclaimed rubber Download PDF

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Publication number
CN108373557A
CN108373557A CN201711478000.2A CN201711478000A CN108373557A CN 108373557 A CN108373557 A CN 108373557A CN 201711478000 A CN201711478000 A CN 201711478000A CN 108373557 A CN108373557 A CN 108373557A
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weight
rubber
parts
preparation method
characterized
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CN201711478000.2A
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Chinese (zh)
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CN108373557B (en
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孔永胜
孔荣坤
杨登盛
许琦
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天台坤荣橡胶有限公司
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    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L17/00Compositions of reclaimed rubber
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G
    • C08J11/00Recovery or working-up of waste materials
    • C08J11/04Recovery or working-up of waste materials of polymers
    • C08J11/10Recovery or working-up of waste materials of polymers by chemically breaking down the molecular chains of polymers or breaking of crosslinks, e.g. devulcanisation
    • C08J11/16Recovery 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
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G
    • C08J11/00Recovery or working-up of waste materials
    • C08J11/04Recovery or working-up of waste materials of polymers
    • C08J11/10Recovery or working-up of waste materials of polymers by chemically breaking down the molecular chains of polymers or breaking of crosslinks, e.g. devulcanisation
    • C08J11/18Recovery 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
    • C08J11/22Recovery 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
    • C08J11/26Recovery 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
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08JWORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G
    • C08J2317/00Characterised by the use of reclaimed rubber
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08KUse of inorganic or non-macromolecular organic substances as compounding ingredients
    • C08K2201/00Specific properties of additives
    • C08K2201/011Nanostructured additives
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08LCOMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L2205/00Polymer mixtures characterised by other features
    • C08L2205/03Polymer mixtures characterised by other features containing three or more polymers in a blend
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02WCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
    • Y02W30/00Technologies for solid waste management
    • Y02W30/50Reuse, recycling or recovery technologies
    • Y02W30/62Plastics recycling

Abstract

The invention discloses a kind of preparation methods of high-performance reclaimed rubber, including:Rubber powder, softening agent, activator, antioxidant, modifying agent, modified nano montmorillonite are put into the mixing plant equipped with microwave device, stirs, high-performance reclaimed rubber is obtained after reaction.The addition of nano imvite increases the frictional force between micelle, makes to be more fully mixed, simultaneously as the presence of coupling agent, modified nano imvite can more uniformly disperse in the packing layer of reclaimed rubber.Due to the special lamellar structure of nano imvite, it is dispersed in the processing performance that nano imvite in rubber substantially increases rubber.Second, rubber powder, since ZDA is the close hydroxyl of height, can form hydroxy metal ion complex compound, greatly reinforce modified nano montmorillonite and disperseed in colloid, increase the performance of vulcanizate in sulfidation.Therefore, the high-performance reclaimed rubber that prepared by the present invention has the characteristics that processing performance is good, intensity is high.

Description

A kind of preparation method of high-performance reclaimed rubber

Technical field

The present invention relates to material forming processing technology field more particularly to a kind of preparation methods of high-performance reclaimed rubber.

Background technology

The main source of waste old is the tire scrapped, sebific duct, adhesive tape, sole, industrial glue sundries and rubber plant The production of the products such as material.In recent years, China about generates 1,000,000 tons of scrap rubber rubber every year, these waste and old rubber products all do not have It is fully utilized, waste old is mixed burning by some places, causes serious secondary pollution and money The recycling of the waste in source, waste old not only expands rubber raw materials source, reduces production cost, and can be with environmental protection.

The recovery process of vulcanizate mostly uses greatly mechanochemical reaction at present, and disulphide is added in waste old, and such as two Vulcanize hexichol, dibenzyl disulfide etc., these regenerative agents can not only cause damages to environment, since it contains active sulphur, when being heated Part C-C keys can be made to be broken, obtained reclaimed rubber performance is unstable, therefore, how to recycle to stability and high efficiency waste and old rubber Glue is the developing direction of the following rubber industry.

Invention content

The main purpose of the present invention is to provide a kind of preparation method of high-performance reclaimed rubber, good with processing performance, The high feature of intensity.

To achieve the above objectives, the technical solution adopted by the present invention is:

The present invention provides a kind of preparation method of high-performance reclaimed rubber, includes the following steps:80-120 parts by weight rubbers Rubber powder body, 6-10 parts by weight softening agent, 2-5 parts by weight activator, 1-3 parts by weight antioxidant, part by weight modified dose of 2-5,6-10 Part by weight modified nano imvite is put into the mixing plant equipped with microwave device, stirring, and high-performance regeneration rubber is obtained after reaction Glue, the softening agent are the mixture of naphthenic oil and coumarone indene resin, and the activator is modified stearic acid, and the modifying agent is Dizinc acrylate resin.

Preferably, the rubber powder is prepared as follows:Waste and used rubber tyre is cleaned, dry, is ground, is obtained The thick rubber powder of tyre surface;It by the thick rubber powder first time iron removal by magnetic separation of the tyre surface, screens, crushes, second of iron removal by magnetic separation obtains rubber powder Body.

Preferably, the weight ratio of the naphthenic oil and coumarone indene resin is 3:2.

Preferably, the modified stearic acid is prepared as follows:8-12 parts by weight stearic acid is dissolved in absolute ethyl alcohol In, a small amount of coupling agent KH-560 and 4-6 parts by weight of alumina powder is added in heating stirring 10-30min after stearic acid is sufficiently mixed End, reacts 40-60min, and filtering, drying obtain modified stearic acid.

Preferably, heating temperature is 60 DEG C.

Preferably, the antioxidant is N- phenyl N-cyclohexyl p-phenylenediamine.

Preferably, the modified nano montmorillonite is prepared as follows:1 parts by weight coupling agent is taken to be dissolved in absolute ethyl alcohol In, heating stirring 10-15min, heating temperature is 60 DEG C, and 8 parts by weight nano imvites are added, and 30-50min, mistake are reacted in stirring Filter, it is dry, obtain modified nano montmorillonite.

Preferably, heating temperature is 60 DEG C.

Preferably, mixing time 40-50min.

Preferably, the rotating speed of mixing plant is 40-60 revs/min.

The present invention provides a kind of preparation method of high-performance reclaimed rubber, includes the following steps:80-120 parts by weight rubbers Rubber powder body, 6-10 parts by weight softening agent, 2-5 parts by weight activator, 1-3 parts by weight antioxidant, part by weight modified dose of 2-5,6-10 Part by weight modified nano imvite is put into the mixing plant equipped with microwave device, stirring, and high-performance regeneration rubber is obtained after reaction Glue, the softening agent are the mixture of naphthenic oil and coumarone indene resin, and the activator is modified stearic acid, and the modifying agent is Dizinc acrylate resin.Compared with prior art, the addition of nano imvite increases the frictional force between micelle in the present invention so that Be more fully mixed, simultaneously as the presence of coupling agent, modified nano imvite can reclaimed rubber packing layer it is more uniform Dispersion.In addition, due to the special lamellar structure of nano imvite, it is dispersed in nano imvite in rubber and substantially increases The processing performance of rubber.Second, the obtained rubber powder that obtains, can be with shape since ZDA is the close hydroxyl of height in sulfidation It at hydroxyl-metal ion complex, has greatly reinforced modified nano montmorillonite and has disperseed in colloid, increased the use of vulcanizate Performance.Therefore, the high-performance reclaimed rubber that prepared by the present invention has the characteristics that processing performance is good, intensity is high.

Specific implementation mode

It is described below for disclosing the present invention so that those skilled in the art can realize the present invention.It is excellent in being described below Embodiment is selected to be only used as illustrating, it may occur to persons skilled in the art that other obvious modifications.

The present invention provides a kind of preparation method of high-performance reclaimed rubber, includes the following steps:80-120 parts by weight rubbers Rubber powder body, 6-10 parts by weight softening agent, 2-5 parts by weight activator, 1-3 parts by weight antioxidant, part by weight modified dose of 2-5,6-10 Part by weight modified nano imvite is put into the mixing plant equipped with microwave device, stirring, and high-performance regeneration rubber is obtained after reaction Glue, the softening agent are the mixture of naphthenic oil and coumarone indene resin, and the activator is modified stearic acid, and the modifying agent is Dizinc acrylate resin.

The present invention recycles reclaimed rubber using microwave stirring desulphurization method, and at a certain temperature, microwave carries The energy of confession can cut off C-S keys under the premise of not cutting off rubber backbone, play the role of desulfurization.Common microwave desulfurization skill Art causes microwave desulfurization in the process due to blunt temperature or temperature fluctuation, causes reclaimed rubber since temperature can not accurately control Machining property is poor, and the present invention is stearic acid modified by activator, and alumina powder is added, and one is played while activation Fixed accumulation of heat effect, that is, ensure that the stabilization of temperature, also reduce energy consumption to a certain extent.

Preferably, the rubber powder is prepared as follows:Waste and used rubber tyre is cleaned, dry, is ground Mill, obtains the thick rubber powder of tyre surface;It by the thick rubber powder first time iron removal by magnetic separation of the tyre surface, screens, crushes, second of iron removal by magnetic separation obtains To rubber powder.

Preferably, the weight ratio of the naphthenic oil and coumarone indene resin is 3:2.

Preferably, the modified stearic acid is prepared as follows:8-12 parts by weight stearic acid is dissolved in nothing In water-ethanol, a small amount of coupling agent KH-560 and 4-6 parts by weight oxygen is added in heating stirring 10-30min after stearic acid is sufficiently mixed Change aluminium powder, react 40-60min, filtering, drying obtain modified stearic acid.Preferably, heating temperature is 60 DEG C.

Preferably, the antioxidant is N- phenyl N-cyclohexyl p-phenylenediamine.

The addition of nano imvite increases the frictional force between micelle so that is more fully mixed, simultaneously as coupling The presence of agent, modified nano imvite can more uniformly disperse in the packing layer of reclaimed rubber, in addition, due to nano imvite Special lamellar structure, be dispersed in the processing performance that nano imvite in rubber substantially increases rubber.

The present invention using modified nano montmorillonite as filler, waste old due to filler addition, after interrupting C-S keys, Cause C-C main chains unstable, to which machining property is deteriorated.

Preferably, the modified nano montmorillonite is prepared as follows:1 parts by weight coupling agent will be taken to be dissolved in In absolute ethyl alcohol, heating stirring 10-15min, heating temperature is 60 DEG C, and 8 parts by weight nano imvites are added, and 30- is reacted in stirring 50min is filtered, dry, obtains modified nano montmorillonite.Preferably, heating temperature is 60 DEG C.

The obtained rubber powder that obtains, since ZDA is the close hydroxyl of height, can form hydroxyl-metal ion in sulfidation Complex compound has greatly reinforced filler and has disperseed in colloid, increases the performance of vulcanizate.

In the preparation process of high-performance reclaimed rubber, mixing time is preferably 40-50min, and the rotating speed of mixing plant is excellent It is selected as 40-60 revs/min.

From above scheme as can be seen that in the present invention addition of nano imvite increase the frictional force between micelle, make Must be more fully mixed, simultaneously as the presence of coupling agent, modified nano imvite can reclaimed rubber packing layer it is more equal Even dispersion is dispersed in nano imvite in rubber and greatly improves in addition, due to the special lamellar structure of nano imvite The processing performance of rubber.Second, the obtained rubber powder that obtains, since ZDA is the close hydroxyl of height, can be formed in sulfidation Hydroxyl-metal ion complex has greatly reinforced filler and has disperseed in colloid, increases the performance of vulcanizate.Therefore, originally High-performance reclaimed rubber prepared by invention has the characteristics that processing performance is good, intensity is high.

For a further understanding of the present invention, technical solution provided by the invention is carried out specifically with reference to embodiment Bright, protection scope of the present invention is not limited by the following examples.

Raw material and chemical reagent used in the embodiment of the present invention are purchased in market.

The softening agent is the mixture of common commercially available naphthenic oil and coumarone indene resin, ratio 3:2;

The activator is modified stearic acid;

The antioxidant is common commercially available antioxidant 4010 (N- phenyl N-cyclohexyls p-phenylenediamine);

The coupling agent is KH-560;

The additive is modified nano montmorillonite;

The modifying agent is that dizinc acrylate resin ZDA (chemistry is pure) is purchased from AlfaAesar.

Embodiment 1

10 parts by weight stearic acid are taken to be dissolved in 100ml absolute ethyl alcohols, abundant heating stirring 10-30min, heating temperature 60 DEG C, a small amount of coupling agent KH-560 and 5 parts by weight of alumina powder are added after stearic acid is sufficiently mixed, reacts 40-60min, instead It should the completely rear obtained modified stearic acid of filtration drying.

1 parts by weight coupling agent is taken to be dissolved in 100ml absolute ethyl alcohols, abundant heating stirring 10-15min, heating temperature is 60 DEG C, 8 parts by weight nano imvites are added, are sufficiently stirred reaction 30-50min, filtration drying is made modified Nano and covers and takes off after the reaction was complete Soil.

Waste and used rubber tyre is subjected to cleaning 10-20min, it is to be cleaned it is clean after dry, the waste and used rubber tyre that will be dried In board top bevel, and collect the thick rubber powder of tyre surface.

Tyre surface coarse powder carries out the tyre surface coarse powder after iron removal by magnetic separation is screened.

Tyre surface coarse powder after screening pulverizer is crushed into (40-60 mesh), is packaged rubber powder after carrying out secondary iron removal by magnetic separation.

100 parts by weight of rubber powder, 10 parts by weight of softening agent, 5 parts by weight of activator, 2 parts by weight of antioxidant, 2 weight of modifying agent Amount part, 10 parts by weight of modified nano montmorillonite are put into the mixing plant equipped with microwave device, are sufficiently stirred 45min, rotating speed is 40-60 revs/min, after by air intake device sucking charging hopper carry out packing packaging.

Detect its tensile strength be 18MPa, ash content 12%, the elongation at break variation of Mooney on the 550%, 15 (△ ML) It is 2.

Embodiment 2

10 parts by weight stearic acid are taken to be dissolved in 100ml absolute ethyl alcohols, abundant heating stirring 10-30min, heating temperature 60 DEG C, a small amount of coupling agent KH-560 and 5 parts by weight of alumina powder are added after stearic acid is sufficiently mixed, reacts 40-60min, instead It should the completely rear obtained modified stearic acid of filtration drying.

1 parts by weight coupling agent is taken to be dissolved in 100ml absolute ethyl alcohols, abundant heating stirring 10-15min, heating temperature is 60 DEG C, 8 parts by weight nano imvites are added, are sufficiently stirred reaction 30-50min, filtration drying is made modified Nano and covers and takes off after the reaction was complete Soil.

Waste and used rubber tyre is subjected to cleaning 10-20min, it is to be cleaned it is clean after dry, the waste and used rubber tyre that will be dried In board top bevel, and collect the thick rubber powder of tyre surface.

Tyre surface coarse powder carries out the tyre surface coarse powder after iron removal by magnetic separation is screened.

Tyre surface coarse powder after screening pulverizer is crushed into (40-60 mesh), is packaged rubber powder after carrying out secondary iron removal by magnetic separation.

100 parts by weight of rubber powder, 8 parts by weight of softening agent, 3 parts by weight of activator, 1 parts by weight of antioxidant, 3 weight of modifying agent Part 8 parts by weight of modified nano montmorillonite are put into the mixing plant equipped with microwave device, are sufficiently stirred 45min, rotating speed 40-60 Rev/min, after by air intake device sucking charging hopper carry out packing packaging.

Detect its tensile strength be 15MPa, ash content 10%, the elongation at break variation of Mooney on the 500%, 15 (△ ML) It is 1.

Embodiment 3

10 parts by weight stearic acid are taken to be dissolved in 100ml absolute ethyl alcohols, abundant heating stirring 10-30min, heating temperature 60 DEG C, a small amount of coupling agent KH-560 and 5 parts by weight of alumina powder are added after stearic acid is sufficiently mixed, reacts 40-60min, instead It should the completely rear obtained modified stearic acid of filtration drying.

1 parts by weight coupling agent is taken to be dissolved in 100ml absolute ethyl alcohols, abundant heating stirring 10-15min, heating temperature is 60 DEG C, 8 parts by weight nano imvites are added, are sufficiently stirred reaction 30-50min, filtration drying is made modified Nano and covers and takes off after the reaction was complete Soil.

Waste and used rubber tyre is subjected to cleaning 10-20min, it is to be cleaned it is clean after dry, the waste and used rubber tyre that will be dried In board top bevel, and collect the thick rubber powder of tyre surface.

Tyre surface coarse powder carries out the tyre surface coarse powder after iron removal by magnetic separation is screened.

Tyre surface coarse powder after screening pulverizer is crushed into (40-60 mesh), is packaged rubber powder after carrying out secondary iron removal by magnetic separation.

100 parts by weight of rubber powder, 6 parts by weight of softening agent, 2 parts by weight of activator, 1 parts by weight of antioxidant, 5 weight of modifying agent Part, 6 parts by weight of modified nano montmorillonite are put into the mixing plant equipped with microwave device, are sufficiently stirred 45min, rotating speed 40- 60 revs/min, after by air intake device sucking charging hopper carry out packing packaging.

Detect its tensile strength be 13MPa, ash content 16%, the elongation at break variation of Mooney on the 440%, 15 (△ ML) It is 7.

Comparative example

Using the preparation method of embodiment 1, the raw material and performance of use are as shown in table 1.

The raw material and the performance test results that 1 comparative example of the present invention of table uses

The basic principles, main features and advantages of the present invention have been shown and described above.The technology of the industry Personnel are it should be appreciated that the present invention is not limited to the above embodiments, and what is described in the above embodiment and the description is only the present invention Principle, various changes and improvements may be made to the invention without departing from the spirit and scope of the present invention, these variation and Improvement is both fallen in the range of claimed invention.The present invention claims protection domain by appended claims and its Equivalent defines.

Claims (10)

1. a kind of preparation method of high-performance reclaimed rubber, which is characterized in that include the following steps:
80-120 parts by weight of rubber powder, 6-10 parts by weight softening agent, 2-5 parts by weight activator, 1-3 parts by weight antioxidant, Part by weight modified dose of 2-5, the part by weight modified nano imvites of 6-10 are put into the mixing plant equipped with microwave device, stirring, instead Should after obtain high-performance reclaimed rubber,
The softening agent is the mixture of naphthenic oil and coumarone indene resin,
The activator is modified stearic acid,
The modifying agent is dizinc acrylate resin.
2. preparation method according to claim 1, which is characterized in that the rubber powder is prepared as follows:
Waste and used rubber tyre is cleaned, dry, is ground, the thick rubber powder of tyre surface is obtained;
It by the thick rubber powder first time iron removal by magnetic separation of the tyre surface, screens, crushes, second of iron removal by magnetic separation obtains rubber powder.
3. preparation method according to claim 1, which is characterized in that the weight ratio of the naphthenic oil and coumarone indene resin is 3:2。
4. preparation method according to claim 1, which is characterized in that the modified stearic acid is prepared as follows:
8-12 parts by weight stearic acid is dissolved in absolute ethyl alcohol, heating stirring 10-30min is added after stearic acid is sufficiently mixed A small amount of coupling agent KH-560 and 4-6 parts by weight of alumina powder, reacts 40-60min, and filtering, drying obtain modified stearic acid.
5. preparation method according to claim 4, which is characterized in that heating temperature is 60 DEG C.
6. preparation method according to claim 1, which is characterized in that the antioxidant is N- phenyl N-cyclohexyls pair Phenylenediamine.
7. preparation method according to claim 1, which is characterized in that the modified nano montmorillonite is made as follows It is standby:
1 parts by weight coupling agent is taken to be dissolved in absolute ethyl alcohol, heating stirring 10-15min, heating temperature is 60 DEG C, and 8 parts by weight are added 30-50min is reacted in nano imvite, stirring, filters, dry, obtains modified nano montmorillonite.
8. preparation method according to claim 7, which is characterized in that heating temperature is 60 DEG C.
9. preparation method according to claim 1, which is characterized in that mixing time 40-50min.
10. preparation method according to claim 1, which is characterized in that the rotating speed of mixing plant is 40-60 revs/min.
CN201711478000.2A 2017-12-29 2017-12-29 Preparation method of high-performance regenerated rubber CN108373557B (en)

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