CN101029148A - Process of reclaimed rubber by improved high-temperature dynamic desulfurization - Google Patents

Process of reclaimed rubber by improved high-temperature dynamic desulfurization Download PDF

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Publication number
CN101029148A
CN101029148A CNA2007100486594A CN200710048659A CN101029148A CN 101029148 A CN101029148 A CN 101029148A CN A2007100486594 A CNA2007100486594 A CN A2007100486594A CN 200710048659 A CN200710048659 A CN 200710048659A CN 101029148 A CN101029148 A CN 101029148A
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desulfurization
reclaimed rubber
parts
activators
tar
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CN100447187C (en
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吴富明
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HAIYAN RUBBER CO Ltd LONGCHANG SICHUAN
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HAIYAN RUBBER CO Ltd LONGCHANG SICHUAN
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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

Abstract

An improved process for producing reclaimed rubber by high-temperature dynamic desulfurization is carried out by taking tyre rubber powder and chemical auxiliary as raw materials, desulfurizing at 220-250degree for 120-160mins, milling at 0.95MPa to 1.65MPa, filtering, refining and forming. It improves desulfurizing formula and process and is more efficient.

Description

Improved high-temperature dynamic desulfurization is produced the novel process of reclaimed rubber
Technical field
The present invention relates to the reclaiming method of the reclaiming method, particularly scrap tire rubber of waste or used vulcanized rubber.
Background technology
With waste and used rubber tyre or rubber overshoes and other the multiple waste rubber goods technique for regenerated rubber that is raw material, generally comprise following steps: rubber powder produces that (junked tire is through cleaning, chopping, magnetic separation, screening, fiber separation, after removing the irony and filamentary material in the tire, obtain 10-30 purpose rubber powder), desulfurization, kneading, filtration, refining, forming process make the reclaimed rubber finished product.Wherein, committed step is a desulfurization process, the sulphur in the rubber is removed, to recover the original mechanical property of rubber.And the factor one that influences desulfurization be with adding auxiliary chemicals composition and content relevant, the 2nd, be subjected to the influence of factors such as the processing condition of desulfurization operations such as temperature, pressure.Application number is 95111197.3 and is called that the Chinese patent literature of " regenerated rubber for fined tyre and production technique thereof " has following open: the content that each component is formed in the desulfurization process is (weight percent): Stockholm tar 8-14, activator 460,829 or 420 accounts for 0.2-0.7, rosin accounts for 1.4-2.2, turps, kautschin or two set alkene account for 0.5-2.0, and surplus is the old tire rubber powder.Desulfurization operations is carried out in digester, and desulfurization temperature is 200-210 ℃, and desulfurization pressure is 1.6-1.9MPa, and desulfurization time is 120-180 minute.According to the document, this prescription and technology have reduced presses the refining number of times, has shortened the production cycle, and the reclaimed rubber quality of output reaches and surpasses national standard (GB/T13460-92).Though the desulfurization temperature of this technology increases than general technology (150-170 ℃),, also there is the possibility of raising in desulfurization temperature theoretically, and the extrusion rate of sulphur is still waiting further raising in the waste rubber powder.
Secondly, existing technique for regenerated rubber one is oil process production, the production cost height, and quality is low; The 2nd, water/oil method production, Quality Cost is better than oil process production, but damage ratio is bigger; The 3rd, dynamic desulfurization, the production unit that it adopts usually has two kinds: a kind of is oil heating digester, and another kind is the electrically heated digester.This method quality product is higher, pollutes but still exist.Still there is environmental pollution problems in the discharging of waste vapour in its sulfur removal technology process.At the pollution problem of desulfurization waste steam exhausting, application number is 96116907.9 and is called " process of technique transformation for producing reclaimed rubber by dynamic desulfating " and discloses a cover waste vapour treatment unit: mainly the cooling tank that is joined by order, the swollen bucket that rises, spray bucket are formed.The steam drain of many dynamic digesters connects into a molectron by pipe.The spray bucket is communicated with sewage lagoon.After lowering the temperature to waste vapour, this technology adopting water spray mode to handle.Organic removal effect is still undesirable in the waste vapour, secondly, does not have technical measures to realize the recycling of ingredient in the waste vapour as oil, combustible gas.
Summary of the invention
The purpose of this invention is to provide the novel process that the higher improved high-temperature dynamic desulfurization of a kind of new formulation, desulfuration efficiency is produced reclaimed rubber.
Purpose of the present invention is realized by following technical scheme: a kind of improved high-temperature dynamic desulfurization is produced the novel process of reclaimed rubber, comprise with the tire glue powder being raw material, be equipped with auxiliary chemicals through desulfurization, kneading, filter, refining, forming process makes the reclaimed rubber finished product, tire glue powder in 1000 weight parts in the desulfurization process is a benchmark, the add-on of producing the auxiliary chemicals of tyre surface footwear material reclaimed rubber is: 104~148 parts in solid coal tar, 9~28 parts of rosin, 6~23 parts of 820 resin additives, 3~22 parts of coal-tar pitch, 0.3~0.9 part in 450 activators, 3~7 parts in 420 activators (can add 0.02~0.08 part of reodorant as required); The add-on of the auxiliary chemicals of production high-performance reclaimed rubber is: 104~148 parts in solid coal tar, 9~28 parts of rosin, 6~23 parts of 820 resin additives, 3~9 parts of Stockholm tars, 6~19 parts of kautschins; 2~4 parts in 420 activators; In the desulfurization process, tire glue powder and auxiliary chemicals are added in the digester by above-mentioned prescription, under 220~250 ℃ desulfurization temperature, material in the jar is constantly stirred, vapor pressure rose to 1.65MPa by initial 0.95MPa in jar, finished desulfurization operations through 120~160 minutes.
Also have the off gas treatment operation: the waste gas in the digester is introduced tubular heater exchhanger by pipeline and is cooled off after the reducing valve decompression, carry out gas-liquid separation through the centrifugal gas-liquid separating device again, isolated inflammable gas causes boiler through pipeline and acts as a fuel and burn, isolated liquid carries out oily water separation through water-and-oil separator again, isolated oil is as the reuse raw material, and isolated water carries out entering septic tank after the anaerobic treatment.
Exploration and repetition test through enterprise technology personnel and two more than ten years of worker, in production practice and test, update and perfect, finally determined sulfur removal technology prescription of the present invention, promptly on existing desulfurization component basis, increased solid coal tar and 820 resin additives and adjusted each component ratio.Secondly, behind the compositional refinements, the corresponding desulfurization temperature that improved has effectively improved the removal efficiency of sulphur in the waste rubber powder.After testing, every index of tread reclaimed rubber reaches and is better than the top grade product standard of the national standard (GB/T13460-92) of existing regenerated rubber.As, each index detects as follows: moisture content 1.10~1.20% (top grade product standard is 1.20%, and qualified is 1.20%), (top grade product standard is 10% to ash 9.00~10.00%, qualified is 15%), two ketone extracts 20.00% (top grade product standard is 20%, and qualified is 28%), (top grade product standard is 9.5MPa to tensile strength 9.5MPa, qualified is 6MPa), tensile yield is greater than 390% (top grade product 390%, qualified is 320%), mooney viscosity 65 (top grade product standard is 70, and qualified is 80).
Embodiment
Novel process of the present invention, comprise with the tire glue powder being raw material, be equipped with auxiliary chemicals and make the reclaimed rubber finished product through desulfurization, kneading, filtration, refining, forming process, tire glue powder in 1000 weight parts in the desulfurization process is a benchmark, and the add-on of producing the auxiliary chemicals of tyre surface footwear material reclaimed rubber is: 104~148 parts in solid coal tar, 9~28 parts of rosin, 6~23 parts of 820 resin additives, 3~22 parts of coal-tar pitch, 0.3~0.9 part in 450 activators, 3~7 parts in 420 activators; The add-on of the auxiliary chemicals of production high-performance reclaimed rubber is: 104~148 parts in solid coal tar, 9~28 parts of rosin, 6~23 parts of 820 resin additives, 3~9 parts of Stockholm tars, 6~19 parts of kautschins; 2~4 parts in 420 activators; In the desulfurization process, tire glue powder and auxiliary chemicals are added in the digester by above-mentioned prescription, under 220~250 ℃ desulfurization temperature, material in the jar is constantly stirred, vapor pressure rose to 1.65MPa by initial 0.95MPa in jar, finished desulfurization operations through 120~160 minutes.Temperature in the digester is obtained the digester indirect heating by high temperature heat conductive oil.
Embodiment 1:
Tire glue powder and auxiliary chemicals prescription following (weight part, together following): tire glue powder 1000, solid coal tar 104.Rosin 9,820 resin additives 6, coal-tar pitch 3,450 activators 0.3,420 activator 3; By above-mentioned prescription material is added in the digester, digester adopts the high temperature heat conductive oil indirect heating, and 220 ℃ of desulfurization temperatures during desulfurization, constantly stir material in the jar, and desulfurization pressure is initially 0.95MPa, and resulting pressure is 1.65MPa, desulfurization time 140 minutes.The quality of reclaimed rubber reaches the GB primary standard.
Embodiment 2:
Tire glue powder and auxiliary chemicals prescription following (weight part, together following): tire glue powder 1000, solid coal tar 148.Rosin 28,820 resin additives 23, coal-tar pitch 22,450 activators 0.9,420 activator 7; 230 ℃ of desulfurization temperatures, desulfurization time 150 minutes.The reclaimed rubber quality reaches GB top grade standard.Moisture content, ash, three indexs of mooney viscosity are a little more than top grade product standard.
Embodiment 3:
Tire glue powder and auxiliary chemicals prescription following (weight part, together following): tire glue powder 1000, solid coal tar 120.Rosin 12,820 resin additives 12, coal-tar pitch 8,450 activators 0.5,420 activator 4; 240 ℃ of desulfurization temperatures, desulfurization time 150 minutes.The reclaimed rubber quality reaches GB top grade standard.
Embodiment 4:
Tire glue powder and auxiliary chemicals prescription following (weight part, together following): tire glue powder 1000, solid coal tar 130, rosin 20,820 resin additives 18, coal-tar pitch 14,450 activators 0.7,420 activator 6; 235 ℃ of desulfurization temperatures, desulfurization time 160 minutes.The reclaimed rubber quality reaches GB top grade standard.
Embodiment 5:
Tire glue powder and auxiliary chemicals prescription following (weight part, together following): tire glue powder 1000, solid coal tar 104, rosin 9,820 resin additives 6, Stockholm tar 3, kautschin 6,420 activators 2,245 ℃ of desulfurization temperatures, desulfurization time 160 minutes.The reclaimed rubber quality reaches GB top grade standard.
Embodiment 6:
Tire glue powder and auxiliary chemicals prescription following (weight part, together following): tire glue powder 1000, solid coal tar 148, rosin 28,820 resin additives 23, Stockholm tar 9, kautschin 19,420 activators 4,250 ℃ of desulfurization temperatures, desulfurization time 145 minutes.The reclaimed rubber quality reaches GB top grade standard.
Embodiment 7:
Tire glue powder and auxiliary chemicals prescription following (weight part, together following): tire glue powder 1000, solid coal tar 124, rosin 12,820 resin additives 14, Stockholm tar 6, kautschin 12,420 activators 3,260 ℃ of desulfurization temperatures, desulfurization time 150 minutes.The reclaimed rubber quality reaches GB top grade standard.
Embodiment 8:
Tire glue powder and auxiliary chemicals prescription following (weight part, together following): tire glue powder 1000, solid coal tar 136, rosin 22,820 resin additives 20, Stockholm tar 7, kautschin 15,420 activators 3,240 ℃ of desulfurization temperatures, desulfurization time 160 minutes.The reclaimed rubber quality reaches GB top grade standard.
The off gas treatment operation is as follows: the waste gas in the digester is introduced tubular heater exchhanger by pipeline and is cooled off after the reducing valve decompression, carry out gas-liquid separation through the centrifugal gas-liquid separating device again, isolated inflammable gas causes boiler through pipeline and acts as a fuel and burn, isolated liquid carries out oily water separation through water-and-oil separator again, isolated oil is as the reuse raw material, and isolated water carries out entering septic tank after the anaerobic treatment.
Inflammable gas in the waste vapour burns in boiler, and wherein organic components becomes water and carbonic acid gas, simultaneously, has maximally utilised its heat energy.Oil after the oily water separation has also carried out recovery and reuse, and the water after the separation can not pollute environment after the anaerobeization processing.
The waste vapour treatment effect of this waste disposal plant is good, has both eliminated the environmental pollution of waste vapour, and the energy has been saved in comprehensive utilization again, has favorable social and economic benefits.

Claims (10)

1, a kind of novel process of improved high-temperature dynamic desulfurization production reclaimed rubber, comprise with the tire glue powder being raw material, be equipped with auxiliary chemicals and make the reclaimed rubber finished product through desulfurization, kneading, filtration, refining, forming process, it is characterized in that: the tire glue powder in 1000 weight parts in the described desulfurization process is a benchmark, the add-on of producing the auxiliary chemicals of tyre surface footwear material reclaimed rubber is: 104~148 parts in solid coal tar, 9~28 parts of rosin, 6~23 parts of 820 resin additives, 3~22 parts of coal-tar pitch, 0.3~0.9 part in 450 activators, 3~7 parts in 420 activators; The add-on of the auxiliary chemicals of production high-performance reclaimed rubber is: 104~148 parts in solid coal tar, 9~28 parts of rosin, 6~23 parts of 820 resin additives, 3~9 parts of Stockholm tars, 6~19 parts of kautschins; 2~4 parts in 420 activators; In the desulfurization process, tire glue powder and auxiliary chemicals are added in the digester by above-mentioned prescription, under 220~250 ℃ desulfurization temperature, material in the jar is constantly stirred, vapor pressure rose to 1.65MPa by initial 0.95MPa in jar, finished desulfurization operations through 120~160 minutes.
2, the novel process that reclaimed rubber is produced in dynamic desulfurization according to the described improved high temperature of claim 1, it is characterized in that: the add-on of described auxiliary chemicals is: solid coal tar 104.Rosin 9,820 resin additives 6, coal-tar pitch 3,450 activators 0.3,420 activator 3; Described desulfurization temperature is 220 ℃, desulfurization time 140 minutes.
3, the novel process that reclaimed rubber is produced in dynamic desulfurization according to the described improved high temperature of claim 1, it is characterized in that: the add-on of described auxiliary chemicals is: solid coal tar 148.Rosin 28,820 resin additives 23, coal-tar pitch 22,450 activators 0.9,420 activator 7; Described desulfurization temperature is 230 ℃, desulfurization time 150 minutes.
4, the novel process that reclaimed rubber is produced in dynamic desulfurization according to the described improved high temperature of claim 1, it is characterized in that: the add-on of described auxiliary chemicals is: solid coal tar 120.Rosin 12,820 resin additives 12, coal-tar pitch 8,450 activators 0.5,420 activator 4; Described desulfurization temperature is 240 ℃, desulfurization time 150 minutes.
5, the novel process that reclaimed rubber is produced in dynamic desulfurization according to the described improved high temperature of claim 1, it is characterized in that: the add-on of described auxiliary chemicals is: solid coal tar 130, rosin 20,820 resin additives 18, coal-tar pitch 14,450 activators 0.7,420 activator 6; Described desulfurization temperature is 235 ℃, desulfurization time 160 minutes.
6, the novel process that reclaimed rubber is produced in dynamic desulfurization according to the described improved high temperature of claim 1, it is characterized in that: the add-on of described auxiliary chemicals is: solid coal tar 104, rosin 9,820 resin additives 6, Stockholm tar 3, kautschin 6,420 activators 2; Described desulfurization temperature is 245 ℃, desulfurization time 160 minutes.
7, the novel process that reclaimed rubber is produced in dynamic desulfurization according to the described improved high temperature of claim 1, it is characterized in that: the add-on of described auxiliary chemicals is: solid coal tar 148, rosin 28,820 resin additives 23, Stockholm tar 9, kautschin 19,420 activators 4; Described desulfurization temperature is 250 ℃, desulfurization time 145 minutes.
8, the novel process that reclaimed rubber is produced in dynamic desulfurization according to the described improved high temperature of claim 1, it is characterized in that: the add-on of described auxiliary chemicals is: solid coal tar 124, rosin 12,820 resin additives 14, Stockholm tar 6, kautschin 12,420 activators 3; Described desulfurization temperature is 260 ℃, desulfurization time 150 minutes.
9, the novel process that reclaimed rubber is produced in dynamic desulfurization according to the described improved high temperature of claim 1, it is characterized in that: the add-on of described auxiliary chemicals is: solid coal tar 136, rosin 22,820 resin additives 20, Stockholm tar 7, kautschin 15,420 activators 3; Described desulfurization temperature is 260 ℃, desulfurization time 160 minutes.
10, the novel process that reclaimed rubber is produced in dynamic desulfurization according to the described improved high temperature of the arbitrary claim of claim 1-9, it is characterized in that: also have the off gas treatment operation: the waste gas in the digester is introduced tubular heater exchhanger by pipeline and is cooled off after the reducing valve decompression, carry out gas-liquid separation through the centrifugal gas-liquid separating device again, isolated inflammable gas causes boiler through pipeline and acts as a fuel and burn, isolated liquid carries out oily water separation through water-and-oil separator again, isolated oil is as the reuse raw material, and isolated water carries out entering septic tank after the anaerobic treatment.
CNB2007100486594A 2007-03-19 2007-03-19 Process of reclaimed rubber by improved high-temperature dynamic desulfurization Expired - Fee Related CN100447187C (en)

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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101633744B (en) * 2009-08-27 2011-05-18 福建环科化工橡胶集团有限公司 Method for preparing environment-friendly white fine renewable rubber
JP2012512284A (en) * 2008-12-18 2012-05-31 タイアン ジンシャン ラバー インダストリー カンパニー リミテッド Automated rubber powder plasticizing process and apparatus
CN102492168A (en) * 2011-12-08 2012-06-13 四川省隆昌海燕橡胶有限公司 Preparation method of super reclaimed rubber
CN101906217B (en) * 2009-06-08 2012-07-25 福建环科集团三明市高科橡胶有限公司 Environment-friendly high-quality tyre reclaimed rubber manufacturing method
CN102936356A (en) * 2012-11-12 2013-02-20 江苏东旭科技有限公司 Method for processing regenerated rubber
CN103131043A (en) * 2011-11-22 2013-06-05 山西省平遥聚贤橡胶有限公司 Device for producing reduction rubber by using waste tyres
CN104526897A (en) * 2015-01-19 2015-04-22 莒县东盛橡胶有限公司 Automated linkage production device for reclaimed rubber refining process
CN104861200A (en) * 2015-05-12 2015-08-26 徐枫祥 Rubber plasticizing steam heating continuous desulfurization device and process
CN105330924A (en) * 2015-11-06 2016-02-17 界首市宇鑫橡胶有限公司 Rubber shoe vamp made from junked tire
CN108912431A (en) * 2018-06-08 2018-11-30 四川省隆昌海燕橡胶有限公司 A kind of flexible damping technique for regenerated rubber

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CN1145295A (en) * 1995-09-13 1997-03-19 南通市回力橡胶实业总公司 Regenerated rubber for fined tyre and its prodn. tech.
CN1250621C (en) * 2003-10-30 2006-04-12 盛国兴 Odorless tyre made from regenerated rubber and preparation method
CN100390228C (en) * 2005-01-21 2008-05-28 孔德威 Method for preparing fire-resistant anti-skid rubber plate

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2012512284A (en) * 2008-12-18 2012-05-31 タイアン ジンシャン ラバー インダストリー カンパニー リミテッド Automated rubber powder plasticizing process and apparatus
CN101906217B (en) * 2009-06-08 2012-07-25 福建环科集团三明市高科橡胶有限公司 Environment-friendly high-quality tyre reclaimed rubber manufacturing method
CN101633744B (en) * 2009-08-27 2011-05-18 福建环科化工橡胶集团有限公司 Method for preparing environment-friendly white fine renewable rubber
CN103131043A (en) * 2011-11-22 2013-06-05 山西省平遥聚贤橡胶有限公司 Device for producing reduction rubber by using waste tyres
CN103131043B (en) * 2011-11-22 2015-07-29 山西省平遥聚贤橡胶有限公司 Damaged tire is utilized to produce the equipment of reduced rubber
CN102492168A (en) * 2011-12-08 2012-06-13 四川省隆昌海燕橡胶有限公司 Preparation method of super reclaimed rubber
CN102936356A (en) * 2012-11-12 2013-02-20 江苏东旭科技有限公司 Method for processing regenerated rubber
CN104526897A (en) * 2015-01-19 2015-04-22 莒县东盛橡胶有限公司 Automated linkage production device for reclaimed rubber refining process
CN104526897B (en) * 2015-01-19 2016-07-06 莒县东盛橡胶有限公司 Reclaimed rubber refining process automatization linkage process units
CN104861200A (en) * 2015-05-12 2015-08-26 徐枫祥 Rubber plasticizing steam heating continuous desulfurization device and process
CN105330924A (en) * 2015-11-06 2016-02-17 界首市宇鑫橡胶有限公司 Rubber shoe vamp made from junked tire
CN108912431A (en) * 2018-06-08 2018-11-30 四川省隆昌海燕橡胶有限公司 A kind of flexible damping technique for regenerated rubber

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