CN101824173A - Microwave modified rubber powder of waste tire and preparation method thereof - Google Patents

Microwave modified rubber powder of waste tire and preparation method thereof Download PDF

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Publication number
CN101824173A
CN101824173A CN201010132572A CN201010132572A CN101824173A CN 101824173 A CN101824173 A CN 101824173A CN 201010132572 A CN201010132572 A CN 201010132572A CN 201010132572 A CN201010132572 A CN 201010132572A CN 101824173 A CN101824173 A CN 101824173A
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China
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powder
waste
microwave
rubber
tyre rubber
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CN201010132572A
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CN101824173B (en
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万昆
余国贤
周瑞雪
路平
李忠铭
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Jianghan University
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Jianghan University
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    • 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; Rubber recycling

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  • Separation, Recovery Or Treatment Of Waste Materials Containing Plastics (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

The invention provides microwave modified rubber powder of a waste tire and a preparation method of the modified rubber powder. The method comprises the following steps: heating 2-14 parts by weight of heavy distillate to 90-130 DEG C, and maintaining the temperature stable; adding 84-97.8 parts by weight of rubber powder of the waste tire and 0.2-2 part(s) by weight of additive into the mixture, and mixing well; and heating the mixture through microwave irradiation, thereby obtaining the microwave modified rubber powder of the waste tire. The invention adopts the rubber powder of the waste tire as the raw material, and solves the problem of over high temperature in modification of the rubber powder of the waste tire through microwave desulfurization under the effect of the additive and the heavy distillate, thereby preventing the rubber powder from excessively aging and agglomeration during microwave desulfurization. The invention also realizes the desulfurization and recycling of the rubber powder of the waste tire, thereby not only saving the cost of the rubber powder, but also reducing the environmental pollution. In addition, since only microwave heating is needed, the invention has the advantages of simple process and high practicality.

Description

A kind of waste-tyre rubber-powder of using microwave modification and preparation method thereof
Technical field
The present invention relates to a kind of waste-tyre rubber-powder, particularly a kind of waste-tyre rubber-powder with microwave modification the invention still further relates to this preparation method who uses the waste-tyre rubber-powder of microwave modification.
Background technology
The burden of China's junked tire with every year about 6,500 ten thousand make us surprised speed increment, will reach 200,000,000 at present, and recovery utilization rate has only 30%.China is a rubber applications big country, and the year consumption of rubber ranks first in the world.And meanwhile, China is again the serious deficient country of a rubber sources, and 60% of year consumption all needs import, and does not have the method for basic solution in the short period of time.Therefore the regeneration of waste rubber goods has quite positive meaning.2006, Chinese rubber powder output reached 300,000 tons, has increased by 50% than the last year.Though compare with the tire output of quick growth, though reclaimed rubber of China and rubber powder have replenished a part of rubber sources, but China remains the big natural rubber of the first in the world importer for many years, natural rubber dependence on import more than 70%, rubber industry safety and even national security have been subjected to serious challenge.Therefore, China presses for from tire demand big country and moves towards tire recycle power.
Application number is that 200710008844.0 patent document discloses the method that a kind of microwave exposure prepares reclaimed rubber: with the waste old material pulverize waste rubber powder, cross the 5-200 mesh sieve; Waste rubber powder is considered to be worth doing and impurity with the electromagnetic method de-iron; With the microwave desulfurization jar of packing into of the waste rubber powder behind de-iron bits and the impurity, the adding Rubber Softener is pressed mass ratio, waste rubber powder: Rubber Softener=100: 0-15; The microwave heating desulfurization, 140~300 ℃ of Heating temperatures; After desulfurization is finished, be cooled to below 150 ℃, roller is produced sheet.This method requires desulfurization temperature up to 230 ℃ usually, and for lower boiling Rubber Softener, the microwave exposure system needs pressurized vessel, and this preparation to equipment requires very high, and energy consumption strengthens simultaneously.The comparatively general way of method of microwave current irradiation rubber powder modified is with rubber powder microwave exposure modification under air atmosphere, and Zhi Bei modified glue powder surface properties is difficult to control like this, and rubber powder was aging severe after system temperature was higher than 100 ℃, poor-performing.And microwave exposure rubber powder under the air atmosphere, although technology is simple, the dusty gas quantity discharged is big, ground rubber is of poor quality.
Summary of the invention
The objective of the invention is at above-mentioned deficiency provide a kind of lower-cost, preparation technology is simple, and the caking that can not wear out with the waste-tyre rubber-powder of microwave modification.
Another object of the present invention provides this preparation method who uses the waste-tyre rubber-powder of microwave modification.
A kind of waste-tyre rubber-powder with microwave modification, it is mixed with by the following raw materials in parts by weight number and forms: waste-tyre rubber-powder 84-97.8 part, heavy distillate 2-14 part, auxiliary agent 0.2-2 part.
The particle diameter of described waste-tyre rubber-powder is the 5-100 order.
3. the waste-tyre rubber-powder with microwave modification according to claim 1, it is characterized in that: the particle diameter of described waste-tyre rubber-powder is the 10-40 order.
Described auxiliary agent is one or more the mixture in sulphur, the agent of shortization of rubber.
Described heavy distillate is a kind of in long residuum, fluid catalytic cracking decant oil or the lubricating oil.
A kind of preparation method who uses the waste-tyre rubber-powder of microwave modification, its step comprises:
1) be that holding temperature was stable after the heavy distillate of 2-14 part was heated to 90-130 ℃ with parts by weight;
2) adding parts by weight in the mixture in step 1) is that the waste-tyre rubber-powder and parts by weight of 84-97.8 part are the auxiliary agent of 0.2-2 part, mixes then;
3) with step 2) in mixture promptly obtain waste-tyre rubber-powder in microwave exposure heating with microwave modification.
The particle diameter of described waste-tyre rubber-powder is the 5-100 order; Described auxiliary agent is one or more the mixture in sulphur, the agent of shortization of rubber; Described heavy distillate is a kind of in long residuum, fluid catalytic cracking decant oil or the lubricating oil.
Mixture temperature is controlled at 150-180 ℃ in the described step 3).
Microwave frequency is 915 or 2450MHz in the described step 3).
Microwave irradiation time is 3-10 minute in the described step 3).
The present invention is a raw material with the waste-tyre rubber-powder, is aided with the effect of auxiliary agent and heavy distillate, has solved the too high problem of temperature in the process of microwave desulfurization modified waste tire glue powder, thereby has prevented rubber powder overaging and caking in the microwave desulfurization process.The present invention makes the waste-tyre rubber-powder can the desulfurization regeneration recycle, not only can save the cost of rubber powder, and can reduce environmental pollution.The present invention only needs microwave heating to get final product, and technology is simple, has very strong practicality.
Embodiment
Below in conjunction with specific embodiment the present invention is described:
Embodiment 1
It is stable that parts by weight are that 14 parts heavy distillate is heated to 90 ℃ and holding temperature, and described heavy distillate is a long residuum.Adding particle diameter then is that 5 order parts by weight are that 84 parts waste-tyre rubber-powder, the auxiliary agent sulphur that parts by weight are 2 parts mix.Be effect 3 minutes under the microwave exposure of 915MHz again with said mixture, and the material system temperature is controlled at 180 ℃, promptly obtains waste-tyre rubber-powder sample 1 with microwave modification in microwave frequency.
Embodiment 2
It is stable that parts by weight are that 8 parts heavy distillate is heated to 130 ℃ and holding temperature, and described heavy distillate is a fluid catalytic cracking decant oil.Adding particle diameter then is that 20 order parts by weight are that 91.6 parts waste-tyre rubber-powder, the auxiliary agent di-mercaptobenzothiazolby that parts by weight are 0.4 part mix.Be effect 10 minutes under the microwave exposure of 915MHz again with said mixture, and the material system temperature is controlled at 170, promptly obtains waste-tyre rubber-powder sample 2 with microwave modification in microwave frequency.
Embodiment 3
With parts by weight be 7 parts heavy distillate be heated to 100 and holding temperature stable, described heavy distillate be the lubricating oil from reduced pressure distillate production.Adding particle diameter then is that 40 order parts by weight are that 92.2 parts waste-tyre rubber-powder, the auxiliary agent polyalkylbenzene phenol disulphide that parts by weight are 0.8 part mix.Be effect 5 minutes under the microwave exposure of 915MH z again with said mixture, and the material system temperature is controlled at 180 ℃, promptly obtains waste-tyre rubber-powder sample 3 with microwave modification in microwave frequency.
Embodiment 4
It is stable that parts by weight are that 8 parts heavy distillate is heated to 110 ℃ and holding temperature, and described heavy distillate is that oil is extracted in furfural treatment out.Adding particle diameter then is that 60 order parts by weight are that 90 parts waste-tyre rubber-powder, the auxiliary agent triethylene tetramine that parts by weight are 1 part mix.Be effect 6 minutes under the microwave exposure of 2450MHz again with said mixture, and the material system temperature is controlled at 160 ℃, obtains waste-tyre rubber-powder sample 4 with microwave modification in microwave frequency.
Embodiment 5
It is stable that parts by weight are that 2 parts heavy distillate is heated to 120 ℃ and holding temperature, and described heavy distillate is that phenol treating is extracted oil out.Adding particle diameter then is that 100 order parts by weight are that 97.8 parts waste-tyre rubber-powder, the auxiliary agent thiuram disulphide that parts by weight are 0.2 part mix.Be effect 5 minutes under the microwave exposure of 2450MHz again with said mixture, and the material system temperature is controlled at 150 ℃, promptly obtains waste-tyre rubber-powder sample 5 with microwave modification in microwave frequency.
Embodiment 6
It is stable that parts by weight are that 11.4 parts heavy distillate is heated to 100 ℃ and holding temperature, and described heavy distillate is the refining oil of extracting out of N-Methyl pyrrolidone.Adding particle diameter then is that 20 order parts by weight are that 88 parts waste-tyre rubber-powder, the auxiliary agent sulphenamide that parts by weight are 0.6 part mix.Be effect 5 minutes under the microwave exposure of 2450MHz again with said mixture, and the material system temperature is controlled at 160 ℃, promptly obtains waste-tyre rubber-powder sample 6 with microwave modification in microwave frequency.
Embodiment 7
It is stable that parts by weight are that 11.4 parts heavy distillate is heated to 100 ℃ and holding temperature, and described heavy distillate is that oil is extracted in furfural treatment out.Adding particle diameter then is that 20 order parts by weight are that 88 parts waste-tyre rubber-powder, the auxiliary agent that parts by weight are 0.6 part mix, and described auxiliary agent is that parts by weight are the sulphur mixture that 0.6 part sulphenamide and parts by weight are 0.4 part.Be effect 5 minutes under the microwave exposure of 915MHz again with said mixture, and the material system temperature is controlled at 180 ℃, promptly obtains waste-tyre rubber-powder sample 7 with microwave modification in microwave frequency.
The waste-tyre rubber-powder sample 1-7 with microwave modification in the foregoing description cooperated with natural rubber test, measure performance with the waste-tyre rubber-powder of microwave modification according to standard GB/T 13460-2008, the pavement performance of the modifying asphalt that records is as shown in table 1.
Wherein the performance of natural rubber is: tensile strength 23.5Mpa; Elongation rate of tensile failure 1238%; Tear fracture intensity 115N/m.
Modified glue powder Tensile strength Mpa Elongation rate of tensile failure % Tear fracture intensity N/m The natural gum amount
Sample 1 ??15.2 ??802 ??81 ??0
Sample 1 ??16.8 ??931 ??91 ??10
Sample 1 ??19.2 ??1062 ??99 ??20
Sample 1 ??21.3 ??1193 ??109 ??30
Sample 2 ??17.1 ??889 ??88 ??0
Sample 3 ??15.9 ??853 ??84 ??0
Sample 4 ??17.9 ??921 ??95 ??0
Sample 5 ??17.5 ??917 ??89 ??0
Modified glue powder Tensile strength Mpa Elongation rate of tensile failure % Tear fracture intensity N/m The natural gum amount
Sample 6 ??17.7 ??904 ??91 ??0
Sample 7 ??17.7 ??914 ??93 ??0
Sample 7 ??18.8 ??961 ??94 ??10
Sample 7 ??20.2 ??1102 ??108 ??20
Sample 7 ??22.3 ??1213 ??113 ??30
The performance that table 1 uses the waste-tyre rubber-powder of microwave modification to cooperate with natural rubber
As seen from the above table, the key technical indexes of above-mentioned waste-tyre rubber-powder with microwave modification has reached among standard GB/T 13460-2008 the superfine requirement to whole tire reclaim rubber fully, if and were aided with a spot of natural rubber, the regenerated rubber performance that obtains would be better.Therefore, the present invention can be applied to actual production fully with the waste-tyre rubber-powder of microwave modification, has very strong practicality.

Claims (10)

1. waste-tyre rubber-powder with microwave modification, it is mixed with by the following raw materials in parts by weight number and forms: waste-tyre rubber-powder 84-97.8 part, heavy distillate 2-14 part, auxiliary agent 0.2-2 part.
2. the waste-tyre rubber-powder with microwave modification according to claim 1, it is characterized in that: the particle diameter of described waste-tyre rubber-powder is the 5-100 order.
3. the waste-tyre rubber-powder with microwave modification according to claim 1, it is characterized in that: the particle diameter of described waste-tyre rubber-powder is 10-40.
4. the waste-tyre rubber-powder with microwave modification according to claim 1 is characterized in that: described auxiliary agent is one or more the mixture in sulphur, the agent of shortization of rubber.
5. the waste-tyre rubber-powder with microwave modification according to claim 1 is characterized in that: described heavy distillate is a kind of in long residuum, fluid catalytic cracking decant oil or the lubricating oil.
6. preparation method with the waste-tyre rubber-powder of microwave modification, its step comprises:
1) be that holding temperature was stable after the heavy distillate of 2-14 part was heated to 90-130 ℃ with parts by weight;
2) adding parts by weight in the mixture in step 1) is that the waste-tyre rubber-powder and parts by weight of 84-97.8 part are the auxiliary agent of 0.2-2 part, mixes then;
3) with step 2) in mixture promptly obtain waste-tyre rubber-powder in microwave exposure heating with microwave modification.
7. the preparation method who uses the waste-tyre rubber-powder of microwave modification according to claim 6, it is characterized in that: the particle diameter of described waste-tyre rubber-powder is the 5-100 order; Described auxiliary agent is one or more the mixture in sulphur, the agent of shortization of rubber; Described heavy distillate is a kind of in long residuum, fluid catalytic cracking decant oil or the lubricating oil.
8. the preparation method who uses the waste-tyre rubber-powder of microwave modification according to claim 6, it is characterized in that: mixture temperature is controlled at 150-180 ℃ in the described step 3).
9. the preparation method of the waste-tyre rubber-powder with microwave modification according to claim 6 is characterized in that: microwave frequency is 915 or 2450MHz in the described step 3).
10. the preparation method who uses the waste-tyre rubber-powder of microwave modification according to claim 6, it is characterized in that: microwave irradiation time is 3-10 minute in the described step 3).
CN2010101325727A 2010-03-23 2010-03-23 Microwave modified rubber powder of waste tire and preparation method thereof Expired - Fee Related CN101824173B (en)

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Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102127246A (en) * 2010-12-13 2011-07-20 四川大学 Method for removing miscellaneous elements from waste high polymer material by using microwave irradiation
CN102815879A (en) * 2012-08-03 2012-12-12 绵阳锐洋新材料技术开发有限公司 Modification method of tire rubber powder, and application thereof in self-insulation partition wall building blocks
CN104723476A (en) * 2013-12-23 2015-06-24 宁夏恒源晟达橡胶制品有限公司 Method for producing rubber powder by utilization of waste tires
CN104845292A (en) * 2015-05-06 2015-08-19 安徽省佳艺休闲用品有限公司 Inflaming-retarding plastic container
CN105802269A (en) * 2016-06-15 2016-07-27 李孟平 Waste tire recycling method
CN107868272A (en) * 2017-11-22 2018-04-03 荣成市华诚橡胶有限公司 A kind of method for reclaiming waste old

Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1103350A (en) * 1993-12-02 1995-06-07 梅州市梅江嘉应橡塑厂 Method for desulfuration regeneration of waste rubber
CN1908042A (en) * 2006-08-29 2007-02-07 马如琦 Desulfurization method of rubber and apparatus thereof
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

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1103350A (en) * 1993-12-02 1995-06-07 梅州市梅江嘉应橡塑厂 Method for desulfuration regeneration of waste rubber
CN1908042A (en) * 2006-08-29 2007-02-07 马如琦 Desulfurization method of rubber and apparatus thereof
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

Cited By (8)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102127246A (en) * 2010-12-13 2011-07-20 四川大学 Method for removing miscellaneous elements from waste high polymer material by using microwave irradiation
CN102127246B (en) * 2010-12-13 2013-02-06 四川大学 Method for removing miscellaneous elements from waste high polymer material by using microwave irradiation
CN102815879A (en) * 2012-08-03 2012-12-12 绵阳锐洋新材料技术开发有限公司 Modification method of tire rubber powder, and application thereof in self-insulation partition wall building blocks
CN102815879B (en) * 2012-08-03 2014-03-26 绵阳锐洋新材料技术开发有限公司 Modification method of tire rubber powder, and application thereof in self-insulation partition wall building blocks
CN104723476A (en) * 2013-12-23 2015-06-24 宁夏恒源晟达橡胶制品有限公司 Method for producing rubber powder by utilization of waste tires
CN104845292A (en) * 2015-05-06 2015-08-19 安徽省佳艺休闲用品有限公司 Inflaming-retarding plastic container
CN105802269A (en) * 2016-06-15 2016-07-27 李孟平 Waste tire recycling method
CN107868272A (en) * 2017-11-22 2018-04-03 荣成市华诚橡胶有限公司 A kind of method for reclaiming waste old

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