CN101475693A - Preparation of modified coal pitch material - Google Patents
Preparation of modified coal pitch material Download PDFInfo
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- CN101475693A CN101475693A CNA2008102073181A CN200810207318A CN101475693A CN 101475693 A CN101475693 A CN 101475693A CN A2008102073181 A CNA2008102073181 A CN A2008102073181A CN 200810207318 A CN200810207318 A CN 200810207318A CN 101475693 A CN101475693 A CN 101475693A
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Abstract
The invention discloses a preparation method for a modified coal pitch material. The method comprises: firstly, heating coal pitch to be between 150 and 200 DEG C inside high-speed shearing equipment till the coal pitch flows completely; then, adding diluting agent in the coal pitch and stirring the mixture at a rotation speed between 1,000 and 3,000rpm for 5 to 20min; adding polymer in the coal pitch and stirring the mixture at a rotation speed between 4,000 and 8,000rpm for 20 to 120min; and finally, adding vulcanizing agent and keeping constant rotation speed and temperature during stirring the mixture for 20 to 120min, and obtaining a finished product of the modified coal pitch. The preparation method not only ensures that the physical property and storage stability of coal pitch can meet state specified standards on road pitch material, but also greatly reduces the content of carcinogenic substance benzpyrene in coal pitch to avoid environmental pollution; moreover, the preparation method is simple and ensures controllable reaction and process time without releasing irritating harmful gases; therefore, the method is suitable for industrial application.
Description
Technical field
The present invention relates to a kind of preparation method who is used for the modified coal pitch material of road pavement.
Background technology
Adopt coal-tar pitch to be of long duration as the road pavement material, but because coal-tar pitch matter is crisp, and contain more condensed-nuclei aromatics, wherein benzopyrene has carinogenicity, thereby at first uses from the Europe restriction in view of environmental protection requirement in nineteen nineties.In recent years, in short supply day by day along with petroleum resources, the development and use of coal-tar pitch have been trend of the times.But there is two large problems in coal-tar pitch as pavior, the one, can satisfy the needs of modern road pavement on the coal-tar pitch performance; The 2nd, in environment protection, whether meet the requirements, or can go up the possibility that reduces environmental pollution to greatest extent.At preceding problem, announced with existing many documents of the exploitation of coal-tar pitch and patent from the inferior grade road, as the general anthraxolite that uses of road pavement in last century, this pitch is that the mixture of medium temperature coal pitch and petroleum pitch is again through modification, thereby improve the method for its low temperature ductility, but this method is not the modification of coal-tar pitch on the pure meaning; For improving the low temperature ductility of coal-tar pitch, existing reported in literature and patent such as U.S. Pat 4008095 adopt medium temperature coal pitch and a large amount of aromatic hydrocarbon oil or coal processing byproduct washing oil interworking, prepare the preferable road coal-tar pitch of low-temperature performance; On this basis, Chinese patent CN 1342726A by add coking solvent oil, polymkeric substance, anti-aging agent through high temperature (more than 260 ℃) thus reaction reaches 6 hours prepares to satisfy and is similar to the oil matrix pitch, and softening temperature is less than 55 ℃, and this method is not considered performances such as coal-tar pitch high-temperature storage stability; Polyethylene and ethylene-vinyl acetate copolymer that Chinese patent CN1074458A discloses a kind of recovery are additive, and petroleum pitch is the method for raw material production modified coal pitch, but this method at be the method for waterproof roll; Canadian Patent 50372/14, U.S. Pat P5473000,6193793 have announced that polymkeric substance is as reclaiming plastics or modified rubber petroleum pitch or coal-tar pitch has improved its consistency by adding the 3rd component such as Ester, but these patents do not provide the data of relevant high-temperature storage stability, and do not provide its evaluation to environmental influence; " reduce in the coal-tar pitch 3 with polymeric reagent, the research of 4-benzopyrene " (Coal Chemical Industry, 2007,1:58-60) reported that coal-tar pitch adopts polymkeric substance to reduce the method for its carcinogens content through pyroreaction, but this method temperature is too high, causing polymkeric substance to improve performances such as coal-tar pitch intensity can reduce, and this method is not set forth the road use properties of modified coal pitch material.
Summary of the invention
Technical problem to be solved by this invention provides a kind of preparation method of modified coal pitch material, this method can reduce the content of carcinogens benzopyrene in the coal-tar pitch greatly, the modified coal pitch material of preparation can be used for road pavement, physicals and excellent storage stability.
Technical solution of the present invention: a kind of preparation method of modified coal pitch material, the steps include: in high-speed shearing equipment, coal-tar pitch to be heated to 150～200 ℃ to mobile fully, then thinner is added in the coal-tar pitch, the consumption of thinner is 10～90% of a pitch weight, stir 5～20min at rotating speed 1000～3000rpm, again polymkeric substance is added in the coal-tar pitch, the consumption of polymkeric substance is 1～10% of a pitch weight, stir 20～120min at rotating speed 4000～8000rpm, add vulcanizing agent again, the consumption of vulcanizing agent is 0.001～0.2% of a pitch weight, keep at last rotating speed and temperature-resistant stirring 20～120min get final product the modified coal pitch finished product; Wherein, described thinner is selected from a kind of in coking solvent oil, the naphthenic oil or their mixture, described polymkeric substance is selected from a kind of or rubber-like in rubber-like, thermoplastic elastomer class, the plastics class, thermoplastic elastomer class, plastics class three's polymer blend, and described vulcanizing agent is selected from the mixture of dithiomorpholine or dithiomorpholine and sulphur.
Rubber-like in the described polymkeric substance be selected from natural rubber or synthetic cis-1,4-polybutadiene rubber, ethylene-propylene rubber(EPR), isoprene-isobutylene rubber, paracril, chloroprene rubber, styrene-butadiene rubber(SBR) one of them.
Thermoplastic elastomer class in the described polymkeric substance is selected from styrene-butadiene-styrene triblock copolymer or styrene-isoprene-phenylethene triblock copolymer.
Plastics class in the described polymkeric substance be selected from polyethylene, polypropylene or polystyrene one of them.
The consumption of described thinner is a bituminous 20～50%.
The consumption of described polymkeric substance is a bituminous 2～8%.
Rubber content was 10～90% when described polymkeric substance was rubber-like, thermoplastic elastomer class, plastics class three's a polymer blend.
Rubber content was 30～70% when described polymkeric substance was rubber-like, thermoplastic elastomer class, plastics class three's a polymer blend.
When described vulcanizing agent was the mixture of dithiomorpholine and sulphur, the weight proportion of dithiomorpholine and sulphur was 10.0～100.0:90.0～5.0.
The beneficial effect of the invention: the preparation method of modified coal pitch material of the present invention both can guarantee the physicals of coal-tar pitch and the road bituminous material index that package stability reaches China's regulation, can reduce the content of carcinogens benzopyrene in the coal-tar pitch again greatly, avoid contaminate environment, and the preparation method is simple, reaction and process period are controlled, can emit the pungency obnoxious flavour, be fit to industrial application.
Embodiment
Below by embodiment the present invention is described in further detail, the preparation method of modified coal pitch material of the present invention, in high-speed shearing equipment, coal-tar pitch is heated to 150～200 ℃ to mobile fully earlier, then thinner is added in the coal-tar pitch, stir 5～20min at rotating speed 1000～3000rpm, again polymkeric substance is added in the coal-tar pitch, stir 20～120min at rotating speed 4000～8000rpm, add vulcanizing agent again, keep rotating speed and temperature-resistant, stir 20～120min get final product the modified coal pitch finished product.The thinner of indication be meant coking solvent oil, naphthenic oil the two one or both of mixture; The polymkeric substance of rubber-like comprises natural rubber or synthetic rubber such as cis-1,4-polybutadiene rubber, ethylene-propylene rubber(EPR), isoprene-isobutylene rubber, paracril, chloroprene rubber, styrene-butadiene rubber(SBR); The thermoplastic elastomer base polymer comprises that styrene-butadiene-styrene triblock copolymer (SBS) or styrene-isoprene-phenylethene triblock copolymer (SIS) etc. contain the thermoplastic elastomer of unsaturated double-bond; The polymkeric substance of plastics class comprises polythene PE, polypropylene PP, polystyrene PS.The consumption of thinner is a bituminous 10～90% among the present invention, and optimum amount is 20～50%; The consumption of polymkeric substance is a bituminous 1～10%, and optimum amount is 2～8%; When polymkeric substance was rubber-like, thermoplastic elastomer class, plastics class three's polymer blend, rubber content was 10～90%, and optimum amount is 30～70%; The consumption of vulcanizing agent is a bituminous 0.001～0.2%, the vulcanizing agent dithiomorpholine can use separately, also can mix the back with sulphur and add use, when described vulcanizing agent was the mixture of dithiomorpholine and sulphur, the weight proportion of dithiomorpholine and sulphur was 10.0～100.0: 90.0～5.0.
Embodiment 1
With (the Shanghai Coke Plant production of 600g low temperature coal-tar pitch, 50 ℃ of softening temperatures, benzopyrene content 1.32%), container internal heating to the 180 ℃ coal-tar pitch of packing into is mobile fully, add coking solvent oil 60g then, start high-shear emulsion machine (BME-1001, Shanghai Weiyu Electromechanical Equipment Manufacture Co. Ltd. produces) stir 10min at rotating speed 2000rpm, add 15gSBS (trade mark 791H, yueyang, hunan petro-chemical corporation produces) again, rotating speed 5000rpm stirs 50min, in coal-tar pitch, mix fully to SBS, add the 0.8g dithiomorpholine again, controlled temperature and rotating speed are constant, mix 120min.Products obtained therefrom is modified coal pitch, and its performance is tested the requirement that touches the mark fully by China road bitumen standard GB/T4509, GB/T4508, GB/4507, and the content of carcinogens benzopyrene reduced by 40%, and the specific performance index sees Table embodiment 1 in 1.
Embodiment 2
(the Wuhan Iron and Steel Plant coke-oven plant produces with the 600g medium temperature coal pitch, 78 ℃ of softening temperatures, benzopyrene content 1.52%), container internal heating to the 180 ℃ coal-tar pitch of packing into is mobile fully, add thinner coking solvent oil 400g, naphthenic oil 200g then, start high-shear emulsion machine, rotating speed 2000rpm stirs 10min, add 15gSBS again, rotating speed 5000rpm stirs 50min, mixes fully in coal-tar pitch to SBS, adds the mixture of 0.6g dithiomorpholine and 0.3g sulphur again, controlled temperature and rotating speed mix 120min respectively at 180 ℃, 6000rpm.Products obtained therefrom is modified coal pitch, and its performance is tested the requirement that touches the mark fully by China road bitumen standard GB/T4509, GB/T4508, GB/4507, and the content of carcinogens benzopyrene reduced by 36.2%, and specific performance sees Table embodiment 2 in 1.
Embodiment 3
With 600g low temperature coal-tar pitch, container internal heating to the 180 ℃ coal-tar pitch of packing into is mobile fully, adds coking solvent oil 60g then, starts high-shear emulsion machine, rotating speed 2000rpm stirs 10min, add 20gSBR (trade mark 1500, Qilu Petrochemical company in Shandong produces) again, rotating speed 5000rpm stirs 50min, in coal-tar pitch, mix fully to SBR, add the mixture of 0.4g dithiomorpholine and 1g sulphur again, controlled temperature and rotating speed are constant, mix 120min.Products obtained therefrom is modified coal pitch, and its performance is tested the requirement that touches the mark fully by China road bitumen standard GB/T4509, GB/T4508, GB/4507, and the content of carcinogens benzopyrene reduced by 46%, and specific performance sees Table embodiment 3 in 1.
Embodiment 4
With 600g low temperature coal-tar pitch, container internal heating to the 180 ℃ coal-tar pitch of packing into is mobile fully, add coking solvent oil 60g then, start high-shear emulsion machine, rotating speed 2000rpm stirs 10min, the mixture (wherein SBR content is 30g) that adds 50gSBR, SIS, PE three again, rotating speed 5000rpm stirs 50min, mixes fully in coal-tar pitch to styrene-butadiene rubber(SBR), adds the mixture of 0.4g dithiomorpholine and 1g sulphur again, controlled temperature and rotating speed are constant, mix 120min.Products obtained therefrom is modified coal pitch, and its performance is tested the requirement that touches the mark fully by China road bitumen standard GB/T4509, GB/T4508, GB/4507, and the content of carcinogens benzopyrene reduced by 42%, and specific performance sees Table embodiment 4 in 1.
Embodiment 5
With 600g low temperature coal-tar pitch, container internal heating to the 180 ℃ coal-tar pitch of packing into is mobile fully, add coking solvent oil 60g then, start high-shear emulsion machine, rotating speed 2000rpm stirs 10min, the mixture (wherein BR content is 10g) that adds 50gBR, SIS, PS three again, rotating speed 5000rpm stirs 50min, mixes fully in coal-tar pitch to BR rubber, adds the mixture of 0.2g dithiomorpholine and 1g sulphur again, controlled temperature and rotating speed are constant, mix 120min.Products obtained therefrom is modified coal pitch, and its performance is tested the requirement that touches the mark fully by China road bitumen standard GB/T4509, GB/T4508, GB/4507, and the content of carcinogens benzopyrene reduced by 52%, and specific performance sees Table embodiment 5 in 1.
Embodiment 6
With 600g low temperature coal-tar pitch, container internal heating to the 180 ℃ coal-tar pitch of packing into is mobile fully, add coking solvent oil 60g and 2g sulphur then, start high-shear emulsion machine, rotating speed 4000rpm stirs 30min, the mixture (wherein BR content is 10g) that adds 20gBR, SBS, PS three again, rotating speed 5000rpm stirs 50min, mixes fully in coal-tar pitch to BR rubber, adds the mixture of 0.2g dithiomorpholine and 2g sulphur again, controlled temperature and rotating speed are constant, mix 120min.Products obtained therefrom is modified coal pitch, and its performance is tested the requirement that touches the mark fully by China road bitumen standard GB/T4509, GB/T4508, GB/4507, and the content of carcinogens benzopyrene reduced by 72%, and specific performance sees Table embodiment 6 in 1.
Table 1 modified coal pitch performance index
Described content only is the basic explanation of the present invention under conceiving, and according to any equivalent transformation that technical scheme of the present invention is done, all should belong to protection scope of the present invention.
Claims (9)
1. the preparation method of a modified coal pitch material, the steps include: in high-speed shearing equipment, coal-tar pitch to be heated to 150～200 ℃ to mobile fully, then thinner is added in the coal-tar pitch, the consumption of thinner is 10～90% of a pitch weight, stir 5～20min at rotating speed 1000～3000rpm, again polymkeric substance is added in the coal-tar pitch, the consumption of polymkeric substance is 1～10% of a pitch weight, stir 20～120min at rotating speed 4000～8000rpm, add vulcanizing agent again, the consumption of vulcanizing agent is 0.001～0.2% of a pitch weight, keep at last rotating speed and temperature-resistant stirring 20～120min get final product the modified coal pitch finished product; Wherein, described thinner is selected from a kind of in coking solvent oil, the naphthenic oil or their mixture, described polymkeric substance is selected from a kind of or rubber-like in rubber-like, thermoplastic elastomer class, the plastics class, thermoplastic elastomer class, plastics class three's polymer blend, and described vulcanizing agent is selected from the mixture of dithiomorpholine or dithiomorpholine and sulphur.
2. according to the preparation method of the described modified coal pitch material of claim 1, it is characterized in that: the rubber-like in the described polymkeric substance be selected from natural rubber or synthetic cis-1,4-polybutadiene rubber, ethylene-propylene rubber(EPR), isoprene-isobutylene rubber, paracril, chloroprene rubber, styrene-butadiene rubber(SBR) one of them.
3. according to the preparation method of the described modified coal pitch material of claim 1, it is characterized in that: the thermoplastic elastomer class in the described polymkeric substance is selected from styrene-butadiene-styrene triblock copolymer or styrene-isoprene-phenylethene triblock copolymer.
4. according to the preparation method of the described modified coal pitch material of claim 1, it is characterized in that: the plastics class in the described polymkeric substance be selected from polyethylene, polypropylene or polystyrene one of them.
5. according to the preparation method of the described modified coal pitch material of claim 1, it is characterized in that: the consumption of described thinner is a bituminous 20～50%.
6. according to the preparation method of the described modified coal pitch material of claim 1, it is characterized in that: the consumption of described polymkeric substance is a bituminous 2～8%.
7. according to the preparation method of the described modified coal pitch material of claim 1, it is characterized in that: rubber content was 10～90% when described polymkeric substance was rubber-like, thermoplastic elastomer class, plastics class three's a polymer blend.
8. according to the preparation method of the described modified coal pitch material of claim 7, it is characterized in that: rubber content was 30～70% when described polymkeric substance was rubber-like, thermoplastic elastomer class, plastics class three's a polymer blend.
9. according to the preparation method of the described modified coal pitch material of claim 1, it is characterized in that: when described vulcanizing agent was the mixture of dithiomorpholine and sulphur, the weight proportion of dithiomorpholine and sulphur was 10.0～100.0:90.0～5.0.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNA2008102073181A CN101475693A (en) | 2008-12-19 | 2008-12-19 | Preparation of modified coal pitch material |
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| CNA2008102073181A CN101475693A (en) | 2008-12-19 | 2008-12-19 | Preparation of modified coal pitch material |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101705003B (en) * | 2009-11-26 | 2011-05-04 | 济南开发区星火科学技术研究院 | Coal tar pitch for high-grade roads |
| CN102924935A (en) * | 2012-11-07 | 2013-02-13 | 中交第一公路勘察设计研究院有限公司 | Method used for modifying low-temperature coal tar asphalt into paving asphalt |
| CN110152347A (en) * | 2019-05-17 | 2019-08-23 | 太原科技大学 | A kind of method that coal liquefaction residue progress detoxification is modified |
| CN113149665A (en) * | 2021-04-08 | 2021-07-23 | 北京联合荣大工程材料股份有限公司 | Environment-friendly bonding agent and stemming for blast furnace |
-
2008
- 2008-12-19 CN CNA2008102073181A patent/CN101475693A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101705003B (en) * | 2009-11-26 | 2011-05-04 | 济南开发区星火科学技术研究院 | Coal tar pitch for high-grade roads |
| CN102924935A (en) * | 2012-11-07 | 2013-02-13 | 中交第一公路勘察设计研究院有限公司 | Method used for modifying low-temperature coal tar asphalt into paving asphalt |
| CN110152347A (en) * | 2019-05-17 | 2019-08-23 | 太原科技大学 | A kind of method that coal liquefaction residue progress detoxification is modified |
| CN113149665A (en) * | 2021-04-08 | 2021-07-23 | 北京联合荣大工程材料股份有限公司 | Environment-friendly bonding agent and stemming for blast furnace |
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Open date: 20090708 |