CN103483654A - Reprocessing method for recycling and reusing flame-retardant rubber - Google Patents
Reprocessing method for recycling and reusing flame-retardant rubber Download PDFInfo
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- CN103483654A CN103483654A CN201310430316.XA CN201310430316A CN103483654A CN 103483654 A CN103483654 A CN 103483654A CN 201310430316 A CN201310430316 A CN 201310430316A CN 103483654 A CN103483654 A CN 103483654A
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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
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- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
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- Y02W30/62—Plastics recycling; Rubber recycling
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Abstract
The invention belongs to the field of chemistry, and particularly relates to a reprocessing method for recycling and reusing flame-retardant rubber, which is used for preparing and producing rubber products by using waste tire rubber pyrolysis. The method comprises the following processes such as cleaning waste tire rubber to remove impurities, preparing catalyst, carrying out primary pyrolysis and secondary pyrolysis on the waste tire rubber, and after being mixed with various assistants, adopting products obtained after pyrolysis for processing rubber products again. According to the invention, two-stage pyrolysis is performed on the recycled waste tire rubber by using a catalyst, in each stage pyrolysis, the temperature and the pyrolysis time can be controlled strictly, not only can sufficient pyrolysis be ensured, but also equipment internal coking, which is caused by over temperature and has influences to pyrolysis product quality, can be avoided, products obtained can be directly added with various assistants, new rubber products can be produced, the effect of waste utilization is reached, environment protection is ensured, and resources are saved.
Description
Technical field
The invention belongs to chemical field, what be specifically related to is to utilize the waste rubber cracking preparation to produce the process for subsequent treatment of a kind of recycling flame retardant rubber of rubber item.
Background technology
As everyone knows, rubber, because it has the characteristics such as splendid high temperature resistant, low temperature resistant, corrosion-resistant, electrical isolation and nontoxic, fire-retardant, stable chemical nature, is just obtaining applying more and more widely in social every profession and trade.To after waste rubber cracking, by further processing, put in the production of rubber item; this has not only processed the industrial refuses such as a large amount of waste olds that modern society produces; alleviate environmental pollution, and provide new approach for solving day by day serious energy dilemma now.At present, although the various technique relevant with waste rubber cracking is arranged
With equipment, be in the news, but, great majority are abundant in order to guarantee waste rubber cracking, the cracking temperature adopted is all higher, thereby the inflammable gas that makes final cracking produce is more, and oil is less, cause oil yield low, Pintsch process also easily causes the device interior coking, reduction of service life, increases production energy consumption; If the reduction cracking temperature, make cracking not thorough, adhere to impurity on the carbon black of gained more, make the carbon black quality descend.
Summary of the invention
For the deficiency existed on prior art, the invention provides the process for subsequent treatment of a kind of recycling flame retardant rubber that a kind of cracking is abundant, quality better, can recycle.
To achieve these goals, the present invention realizes by the following technical solutions:
A kind of process for subsequent treatment of recycling flame retardant rubber, it comprises the steps,
1) to waste old cleaned, impurity elimination;
2) preparation of catalyzer, described catalyzer comprises that the composition of following parts by weight forms: silico-aluminate 35-55 part, activated alumina 10-30 part, zinc oxide 15-25 part, atlapulgite 10-30 part mix;
3) by step 2) after the waste old that cleans up with step 1) of the catalyzer of gained mixes in the ratio of 2-5:1000, send into pyrolyzer and carry out the one-level cracking;
4) the one-level cracking complete after the solid product of gained directly enter the secondary pyrolyzer and carry out the secondary cracking, the splitting gas that the one-level cracking produces is together discharged with the splitting gas of secondary cracking generation;
5) the secondary cracking complete after the solid matter of gained through screening, pulverize, standby after uniform particles;
6) composition by weight forms: the product that takes 4-6 part step 5) gained, 40-60 part reclaimed rubber, 8-10 part protective agent, 1-2 part promotor, 1.5-2 part ferric oxide, 2-5 part tackiness agent, 5-20 part thickening material, 5-10 part toughner, 20-25 part nano flame retardant mixture, 5-9 part quartz sand, mix, molded processing method moulding rubber item;
The preparation method of described nano flame retardant recombiner is:
(1) silicon hydroxyapatite, red phosphorus, Attapulgite, hydrotalcite, polynite, titanium dioxide, calcite, kaolin are mixed according to the mass fraction proportioning of 25-35:15-20:10-15: 10-15:8-10:8-10:7-8:5-7, join in the mixing solutions of 200 parts of methyl-sulphoxides (DMSO) and 50 parts of methyl alcohol, in 65 ℃, stir 60 hours, filter, and wash and remove excessive methyl-sulphoxide (DMSO) for 3 times with the hot ethanol of 60 ℃ of temperature, put into vacuum drying oven, dry 24 hours of 60 ℃ of temperature, grinding is sieved, and obtains the modified flame-retardant mixture one time;
(2), 1 part of modified flame-retardant mixture, 10 parts of Potassium ethanoates and 25 parts of distilled water are mixed, in temperature 50 C, stir more than 10 hours, in 30 ℃ of temperature, first under ultrasonic electric power 350W condition, disperse 2.5 hours, and then disperse 3 hours under ultrasonic electric power 250W condition.Filter, and wash 3 times with distillation, 80 ℃ of vacuum-drying 24 hours, grinding is sieved, and obtains twice-modified fire-retardant mixture;
(3), above-mentioned 1 part of twice-modified fire-retardant mixture is disperseed to 40min at the 600W power ultrasonic, be heated to 90 ℃ with constant temperature heating device, and stir (1200r/min) 60 minutes with mechanical stirrer; Obtain the nano flame retardant mixture.
Above-mentioned recycling elastomeric material, in its described step 4), the solid product that the one-level cracking completes gained enters the opposite direction to the solid product motion in the secondary cracking process and passes into water vapor.
Above-mentioned recycling elastomeric material, the described one-level cracking temperature of its step 3) is 380-410 ℃, pyrolysis time is 15-30 minute.
Above-mentioned recycling elastomeric material, the temperature of the described secondary cracking of its step 4) is 450-500 ℃, pyrolysis time is 10-15 minute.
Beneficial effect:
The present invention utilizes catalyzer to carry out the two-stage cracking to the waste old reclaimed; temperature and pyrolysis time are strictly controlled in every one-level cracking; both guaranteed sufficient cracking; avoided again, because excess Temperature causes the device interior coking, affecting the quality of split product, resulting product directly adds multiple auxiliary agent; can make new rubber item again; reach the effect of utilization of waste material, protected environment, saved resource.Fire retardant prepared by the present invention is not halogen-containing, organism, and asepsis environment-protecting, have a extensive future; The present invention carries out twice-modified, such benefit: increase the reactive behavior point, improve modified effect; In the time of modification, can steam again except the moisture in system, dry and modification is carried out simultaneously, has improved working efficiency; Have a large amount of physics and chemistry planar water in nano silicone hydroxyapatite, Attapulgite, polynite, kaolin etc. self micropore, at high temperature produce water vapor, blocking-up oxygen, absorb heat, reaches multiple fire-retardant effect; Powerful absorption property can effectively improve the synergy of several fire retardants, stops and is raise by the fire retardant matter temperature, has improved flame retarding efficiency; The aboundresources such as silicon hydroxyapatite, Attapulgite, polynite, kaolin, greatly reduce the industrial cost of fire retardant, and also the Application and Development for attapulgite provides a new way; The present invention adopts the solution method ultrasonic wave to disperse and the mechanical high-speed agitator stirs, make fire retardant separately component reached the nano level dispersion in solution, effectively avoided the natural oxidation to matrix material, thereby made matrix material there is better mechanical property.The oxygen index of matrix material is 39.
Embodiment
For technique means, creation characteristic that the present invention is realized, reach purpose and effect is easy to understand, below in conjunction with embodiment, further set forth the present invention.
The invention provides a kind of process for subsequent treatment of recycling flame retardant rubber, its implementation process comprises the steps,
1) to waste old cleaned, impurity elimination;
2) preparation of catalyzer, described catalyzer comprises that the composition of following parts by weight forms: 40 parts of silico-aluminates, 30 parts of activated aluminas, 20 parts, zinc oxide, 25 parts of atlapulgites mix rear standby;
3) by step 2) after the waste old that cleans up with step 1) of the catalyzer of gained mixes in the ratio of 3:1000, to send into pyrolyzer and carry out the one-level cracking, the one-level cracking temperature is 390 ℃, pyrolysis time is 30 minutes;
4) the one-level cracking complete after the solid product of gained directly enter the secondary pyrolyzer and carry out the secondary cracking, the temperature of secondary cracking is 480 ℃, pyrolysis time is 15 minutes, the splitting gas that the one-level cracking produces is together discharged with the splitting gas of secondary cracking generation;
5) the secondary cracking complete after the solid matter of gained through screening, pulverize, standby after uniform particles;
6) composition by weight forms: the product that takes 4-6 part step 5) gained, 40-60 part reclaimed rubber, 8-10 part protective agent, 1-2 part promotor, 1.5-2 part ferric oxide, 2-5 part tackiness agent, 5-20 part thickening material, 5-10 part toughner, 20-25 part nano flame retardant mixture, 5-9 part quartz sand, mix, molded processing method moulding rubber item;
The preparation method of described nano flame retardant recombiner is:
(1) silicon hydroxyapatite, red phosphorus, Attapulgite, hydrotalcite, polynite, titanium dioxide, calcite, kaolin are mixed according to the mass fraction proportioning of 25-35:15-20:10-15: 10-15:8-10:8-10:7-8:5-7, join in the mixing solutions of 200 parts of methyl-sulphoxides (DMSO) and 50 parts of methyl alcohol, in 65 ℃, stir 60 hours, filter, and wash and remove excessive methyl-sulphoxide (DMSO) for 3 times with the hot ethanol of 60 ℃ of temperature, put into vacuum drying oven, dry 24 hours of 60 ℃ of temperature, grinding is sieved, and obtains the modified flame-retardant mixture one time;
(2), 1 part of modified flame-retardant mixture, 10 parts of Potassium ethanoates and 25 parts of distilled water are mixed, in temperature 50 C, stir more than 10 hours, in 30 ℃ of temperature, first under ultrasonic electric power 350W condition, disperse 2.5 hours, and then disperse 3 hours under ultrasonic electric power 250W condition.Filter, and wash 3 times with distillation, 80 ℃ of vacuum-drying 24 hours, grinding is sieved, and obtains twice-modified fire-retardant mixture;
(3), above-mentioned 1 part of twice-modified fire-retardant mixture is disperseed to 40min at the 600W power ultrasonic, be heated to 90 ℃ with constant temperature heating device, and stir (1200r/min) 60 minutes with mechanical stirrer; Obtain the nano flame retardant mixture.
As further improvement, in described step 4), the solid product that the one-level cracking completes gained enters the opposite direction to the solid product motion in the secondary cracking process and passes into water vapor, be beneficial to cracking process fully fully.Fire retardant prepared by the present invention is not halogen-containing, organism, and asepsis environment-protecting, have a extensive future; The present invention carries out twice-modified, such benefit: increase the reactive behavior point, improve modified effect; In the time of modification, can steam again except the moisture in system, dry and modification is carried out simultaneously, has improved working efficiency; Have a large amount of physics and chemistry planar water in nano silicone hydroxyapatite, Attapulgite, polynite, kaolin etc. self micropore, at high temperature produce water vapor, blocking-up oxygen, absorb heat, reaches multiple fire-retardant effect; Powerful absorption property can effectively improve the synergy of several fire retardants, stops and is raise by the fire retardant matter temperature, has improved flame retarding efficiency; The aboundresources such as silicon hydroxyapatite, Attapulgite, polynite, kaolin, greatly reduce the industrial cost of fire retardant, and also the Application and Development for attapulgite provides a new way; The present invention adopts the solution method ultrasonic wave to disperse and the mechanical high-speed agitator stirs, make fire retardant separately component reached the nano level dispersion in solution, effectively avoided the natural oxidation to matrix material, thereby made matrix material there is better mechanical property.
Above demonstration and described ultimate principle of the present invention and principal character and advantage of the present invention.The technician of the industry should understand; the present invention is not restricted to the described embodiments; that in above-described embodiment and specification sheets, describes just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention.The claimed scope of the present invention is defined by appending claims and equivalent thereof.
Claims (5)
1. the process for subsequent treatment of a recycling flame retardant rubber, is characterized in that, comprise the steps,
1) to waste old cleaned, impurity elimination;
2) preparation of catalyzer, described catalyzer comprises that the composition of following parts by weight forms: silico-aluminate 35-55 part, activated alumina 10-30 part, zinc oxide 15-25 part, atlapulgite 10-30 part mix;
3) by step 2) after the waste old that cleans up with step 1) of the catalyzer of gained mixes in the ratio of 2-5:1000, send into pyrolyzer and carry out the one-level cracking;
4) the one-level cracking complete after the solid product of gained directly enter the secondary pyrolyzer and carry out the secondary cracking, the splitting gas that the one-level cracking produces is together discharged with the splitting gas of secondary cracking generation;
5) the secondary cracking complete after the solid matter of gained through screening, pulverize, standby after uniform particles;
6) composition by weight forms: the product that takes 4-6 part step 5) gained, 40-60 part reclaimed rubber, 8-10 part protective agent, 1-2 part promotor, 1.5-2 part ferric oxide, 2-5 part tackiness agent, 5-20 part thickening material, 5-10 part toughner, 20-25 part nano flame retardant mixture, 5-9 part quartz sand, mix, molded processing method moulding rubber item;
The preparation method of described nano flame retardant recombiner is:
(1) silicon hydroxyapatite, red phosphorus, Attapulgite, hydrotalcite, polynite, titanium dioxide, calcite, kaolin are mixed according to the mass fraction proportioning of 25-35:15-20:10-15: 10-15:8-10:8-10:7-8:5-7, join in the mixing solutions of 200 parts of methyl-sulphoxides (DMSO) and 50 parts of methyl alcohol, in 65 ℃, stir 60 hours, filter, and wash and remove excessive methyl-sulphoxide (DMSO) for 3 times with the hot ethanol of 60 ℃ of temperature, put into vacuum drying oven, dry 24 hours of 60 ℃ of temperature, grinding is sieved, and obtains the modified flame-retardant mixture one time;
(2), 1 part of modified flame-retardant mixture, 10 parts of Potassium ethanoates and 25 parts of distilled water are mixed, in temperature 50 C, stir more than 10 hours, in 30 ℃ of temperature, first under ultrasonic electric power 350W condition, disperse 2.5 hours, and then disperse 3 hours under ultrasonic electric power 250W condition.
2. filter, and wash 3 times with distillation, 80 ℃ of vacuum-drying 24 hours, grinding is sieved, and obtains twice-modified fire-retardant mixture;
(3), above-mentioned 1 part of twice-modified fire-retardant mixture is disperseed to 40min at the 600W power ultrasonic, be heated to 90 ℃ with constant temperature heating device, and stir (1200r/min) 60 minutes with mechanical stirrer; Obtain the nano flame retardant mixture.
3. according to the described recycling elastomeric material of claim 1, it is characterized in that: in described step 4), the solid product that the one-level cracking completes gained enters the opposite direction to the solid product motion in the secondary cracking process and passes into water vapor.
4. according to the described recycling elastomeric material of claim 1 or 2, it is characterized in that: the described one-level cracking temperature of step 3) is 380-410 ℃, and pyrolysis time is 15-30 minute.
5. according to the described recycling elastomeric material of claim 1 or 2, it is characterized in that: the temperature of the described secondary cracking of step 4) is 450-500 ℃, and pyrolysis time is 10-15 minute.
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| CN201310430316.XA CN103483654B (en) | 2013-09-22 | 2013-09-22 | A kind of process for subsequent treatment of recycling flame retardant rubber |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106543476A (en) * | 2016-12-08 | 2017-03-29 | 肇庆学院 | A kind of composite for PVC heat stabilizer and preparation method thereof |
| WO2019084978A1 (en) * | 2017-11-06 | 2019-05-09 | 常熟三爱富振氟新材料有限公司 | Production system for vinylidene fluoride |
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|---|---|---|---|---|
| CN1443798A (en) * | 2002-03-12 | 2003-09-24 | 上海绿人生态经济科技有限公司 | Rubber tire containing pyrolyzed carbon black |
| WO2008074188A1 (en) * | 2006-12-20 | 2008-06-26 | Bin Niu | A pyrolysis process for waste and old rubber |
| CN102002141A (en) * | 2010-11-19 | 2011-04-06 | 安徽大学 | Preparation method of polyurethane-nano kaolin composite material |
| CN102898701A (en) * | 2012-09-04 | 2013-01-30 | 青岛保利康新材料有限公司 | Recyclable rubber material |
| CN103045283A (en) * | 2012-10-31 | 2013-04-17 | 牛晓璐 | Continuous cracking process of waste rubber and device thereof |
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2013
- 2013-09-22 CN CN201310430316.XA patent/CN103483654B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1443798A (en) * | 2002-03-12 | 2003-09-24 | 上海绿人生态经济科技有限公司 | Rubber tire containing pyrolyzed carbon black |
| WO2008074188A1 (en) * | 2006-12-20 | 2008-06-26 | Bin Niu | A pyrolysis process for waste and old rubber |
| CN102002141A (en) * | 2010-11-19 | 2011-04-06 | 安徽大学 | Preparation method of polyurethane-nano kaolin composite material |
| CN102898701A (en) * | 2012-09-04 | 2013-01-30 | 青岛保利康新材料有限公司 | Recyclable rubber material |
| CN103045283A (en) * | 2012-10-31 | 2013-04-17 | 牛晓璐 | Continuous cracking process of waste rubber and device thereof |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106543476A (en) * | 2016-12-08 | 2017-03-29 | 肇庆学院 | A kind of composite for PVC heat stabilizer and preparation method thereof |
| CN106543476B (en) * | 2016-12-08 | 2019-01-04 | 肇庆学院 | A kind of composite material and preparation method for PVC heat stabilizer |
| WO2019084978A1 (en) * | 2017-11-06 | 2019-05-09 | 常熟三爱富振氟新材料有限公司 | Production system for vinylidene fluoride |
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Address after: 215138 No. 1 Zhangtangbangxiang, Yangchenghu Town, Xiangcheng District, Suzhou City, Jiangsu Province Patentee after: Suzhou Xiangyuan New Materials Co., Ltd. Address before: 215100 Jiangsu, Xiangcheng District Yang Cheng lake town (Hunan City) figure ten Village Patentee before: Suzhou Xiangyuan Speical Fine Chemical Co., Ltd. |
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