CN104032652B - A kind of method utilizing the extract of wax tailings to reclaim aged petroleum pitch - Google Patents

A kind of method utilizing the extract of wax tailings to reclaim aged petroleum pitch Download PDF

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Publication number
CN104032652B
CN104032652B CN201410271715.0A CN201410271715A CN104032652B CN 104032652 B CN104032652 B CN 104032652B CN 201410271715 A CN201410271715 A CN 201410271715A CN 104032652 B CN104032652 B CN 104032652B
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China
Prior art keywords
distillate
petroleum pitch
aged
distillation
pitch
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Expired - Fee Related
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CN201410271715.0A
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Chinese (zh)
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CN104032652A (en
Inventor
魏建明
张新功
杜峰
高明军
赵辉
李正
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Qingdao Hui Cheng Environmental Technology Co ltd
China University of Petroleum East China
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QINGDAO HUICHENG PETROCHEMICAL TECHNOLOGY Co Ltd
China University of Petroleum East China
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Abstract

The present invention relates to a kind of method utilizing the extract of wax tailings to reclaim aged petroleum pitch, concrete step is as follows: the preparation 1) being greater than the distillate of 300 DEG C; 2) solvent extraction; 3) preparation of bitumen regenerant; 4) regeneration of aged petroleum pitch.Advantage of the present invention is: the inventive method preparation technology is simple, easy to operate, and equipment requirements degree is low; Bitumen regenerant regeneration efficiency prepared by the present invention is high, ageing resistance is excellent.

Description

A kind of method utilizing the extract of wax tailings to reclaim aged petroleum pitch
Technical field
The present invention relates to building material technical field, particularly a kind of oil of the extraction for petroleum pitch regenerator, its preparation method and application thereof.
Background technology
Petroleum pitch road surface is in life-time service process, while the repeated action of vehicular load can be subject to, also can be subject to the impact of the natural causes such as sleet, temperature, sunlight, thus a series of physics, chemical transformation can be there is through certain time limit, occur hardening, become fragile, the phenomenon such as cracking, namely there occurs the aging of pitch.Carry out milling to aged asphalt road surface to abandon, then carrying out again making with new asphalt is means conventional in the past.The every annual meeting of this method produces a considerable amount of asphalt waste.If these discarded asphalts are mishandling, not only can take large-area stacking soil, cause the waste of Nonrenewable resources, and can objectionable impurities be discharged in stacking process, cause the destruction of the environment such as air, water body and soil.The method of carrying out regenerating waste asphalt by adding bitumen regenerant makes the recycling of this part waste resource become possibility.Bitumen regenerant is exactly add in waste and old or aged asphalt to make it recover the material of use properties.The focus that regeneration efficiency is high, the production development of the excellent regenerator of ageing resistance is asphalt-regenerating area research both at home and abroad at present.
Summary of the invention
For problems of the prior art, the object of this invention is to provide a kind of extraction for petroleum pitch regenerator oil, its preparation method and application thereof.
Concrete technical scheme is as follows:
Utilize the extract of wax tailings to reclaim a method for aged petroleum pitch, concrete step is as follows:
1) preparation of the distillate of 300 DEG C is greater than
Use true boiling point distillation instrument by wax tailings in residual voltage for carrying out underpressure distillation under about 10mmHg, 6 × 6mm stainless steel protruded packing is filled with in distillation column, be equivalent to 15-17 block number of theoretical plate, distillation obtains being less than the distillate of 300 DEG C and being greater than the distillate of 300 DEG C, reclaims respectively; Concrete steps are as follows:
(1) connect true boiling point distillation instrument, start vacuum pump, make residual voltage in true boiling point distillation instrument keep 10mmHg;
(2) thermal still and distillation column is added; Operate identical with air distillation;
(3) obtain being less than the distillate of 300 DEG C and being greater than the distillate of 300 DEG C; Be 10 ~ 15mmHg with tower top pressure reduction at the bottom of still, the speed of distillating is 3 ~ 5mLmin -1;
(4), when still temperature is close to 300 DEG C, stops all heating, unload electric furnace, accelerating cooling;
(5) when still temperature drop is to less than 150 DEG C, slowly put into air by blow-off valve, make residual voltage increase, then stop vacuum pump, continue to put into air, until system recovery normal pressure;
2) solvent extraction:
By solvent and step 1) distillate being greater than 300 DEG C that obtains is mixed to join in pulsed extraction column according to weight ratio 1: 1-6: 1 and carries out extracting, obtain extracting oil out and raffinating oil; Described solvent is: furfural, phenol or N-Methyl pyrrolidone;
3) preparation of bitumen regenerant:
By step 2) extraction prepared oil and AH-70 pitch mixes according to " hot asphalt regenerator " (SH/T0819-2010) petrochemical industry standard according to the weight ratio of 1: 9-9: 1, extraction oil and straight-run pitch AH-70 are in harmonious proportion by different ratios, prepare the bitumen regenerant meeting different viscosity grade.
4) regeneration of aged petroleum pitch:
(1) the useless compound that old asphalt pavement milling is got off is screened, then Separation and Recovery aged asphalt;
(2) aged asphalt petroleum pitch regenerator and step (1) reclaimed, according to the ratio Hybrid Heating of weight ratio 1: 1.2-1: 10, fully stirs.
Advantage of the present invention is: the inventive method preparation technology is simple, easy to operate, and equipment requirements degree is low; Bitumen regenerant regeneration efficiency prepared by the present invention is high, ageing resistance is excellent.
Accompanying drawing illustrates:
Fig. 1 is step 3 in embodiment 1) 60 DEG C of viscosity of regenerator sample and the curved line relation of extracting oil ratio example out.
Embodiment
Following examples, only for the present invention will be further described, are not for limiting the scope of the invention.
Embodiment 1
Wax tailings (from Qingdao refinery company coker) prepares the method for aged petroleum bitumen regenerant, and concrete step is as follows:
1) (method do not write exactly in detail in this step is the working method of true boiling point distillation instrument routine to be greater than the preparation of the distillate of 300 DEG C.)
Use true boiling point distillation instrument by wax tailings in residual voltage for carrying out underpressure distillation under about 10mmHg, 6 × 6mm stainless steel protruded packing is filled with in distillation column, be equivalent to 15-17 block number of theoretical plate, distillation obtains being less than the distillate of 300 DEG C and being greater than the distillate of 300 DEG C, reclaims respectively; Concrete steps are as follows:
(1) connect true boiling point distillation instrument, start vacuum pump, make residual voltage in true boiling point distillation instrument keep 10mmHg;
(2) thermal still and distillation column is added; Operate identical with air distillation;
(3) obtain being less than the distillate of 300 DEG C and being greater than the distillate of 300 DEG C; Be 10 ~ 15mmHg with tower top pressure reduction at the bottom of still, the speed of distillating is 3 ~ 5mLmin -1;
(4), when still temperature is close to 300 DEG C, stops all heating, unload electric furnace, accelerating cooling;
(5) when still temperature drop is to less than 150 DEG C, slowly put into air by blow-off valve, make residual voltage increase, then stop vacuum pump, continue to put into air, until system recovery normal pressure;
2) solvent extraction (method do not write exactly in detail in this step is the working method of pulsed extraction column routine):
By solvent and step 1) distillate being greater than 300 DEG C that obtains is mixed to join in pulsed extraction column according to weight ratio 1: 1-6: 1 and carries out extracting, obtain extracting oil out and raffinating oil; Described solvent is: furfural, phenol or N-Methyl pyrrolidone;
The operating parameters of pulsed extraction column is as shown in table 1:
The operating parameters of table 1 pulsed extraction column
The extraction oil properties of preparation is as shown in table 2:
Oil properties extracted out by table 2
3) preparation of bitumen regenerant:
By step 2) extraction prepared oil and AH-70 pitch mixes according to " hot asphalt regenerator " (SH/T0819-2010) petrochemical industry standard according to the weight ratio of 1: 9-9: 1, extraction oil and straight-run pitch AH-70 are in harmonious proportion by different ratios, prepare the bitumen regenerant meeting different viscosity grade, the results are shown in Table 4,60 DEG C of viscosity of regenerator sample and the relation of extracting oil ratio example out can be obtained thus, see Fig. 1, its relation meets following equation.
y=-0.0353x+4.8646(R 2=0.985)
Y: viscosity; X: extract oil ratio example out.
According to above relational expression, adopt interpolation technique can determine to meet the ratio of the extraction oil of each viscosity grade requirement regenerator in table 1, in table 5.
The character of each regenerator is in table 6
Table 3 heat is mixed and is used bitumen regenerant technical requirements
The preliminary composition of table 4 regenerator
Table 5 regenerator composition and viscosity
Table 6 regenerator character
Embodiment 2
The regeneration of aged petroleum pitch (aged petroleum pitch is selected from October, 2011 old asphalt pavement that the rebuilding milling of Road, Hong Kong, Shinan District, Qingdao City gets off)
1. the useless compound that old asphalt pavement milling is got off is screened, then Separation and Recovery aged asphalt;
25 DEG C of penetration degrees of the aged asphalt 2. reclaimed are 32, and softening temperature is 58 DEG C, and 15 DEG C of ductilities are 10cm.
For regenerator R1-1, weighed according to mass ratio 46.1: 53.9 by the aged asphalt of R1-1 and recovery, heating mixes, and obtains 1# regeneration asphalt, and each index meets the requirement to AH-70 pitch in GB/T151980-2000, in table 7.
To regenerator R1-2, weighed according to mass ratio 22.1: 77.9 by the aged asphalt of R1-2 and recovery, heating mixes, and obtains 2# regeneration asphalt, to the requirement of AH-70 pitch in each index GB/T151980-2000, in table 7.
To regenerator R1-4, weighed according to mass ratio 11.3: 88.7 by the aged asphalt of R1-4 and recovery, heating mixes, and obtains 3# regeneration asphalt, to the requirement of AH-70 pitch in each index GB/T151980-2000, in table 7.
To regenerator R1-5, weighed according to mass ratio 9.4: 90.6 by the aged asphalt of R1-4 and recovery, heating mixes, and obtains 4# regeneration asphalt, to the requirement of AH-70 pitch in each index GB/T151980-2000, in table 7.
To regenerator R1-6, weighed according to mass ratio 44.1: 55.9 by the aged asphalt of R1-4 and recovery, heating mixes, and obtains 5# regeneration asphalt, to the requirement of AH-70 pitch in each index GB/T151980-2000, in table 7.
To regenerator R1-7, weighed according to mass ratio 17.0: 83.0 by the aged asphalt of R1-4 and recovery, heating mixes, and obtains 6# regeneration asphalt, the aged asphalt that each index reclaims, in table 7.
Table 7 regeneration asphalt character
As can be seen here, use petroleum pitch regenerator prepared by the inventive method, can effectively reclaim aged petroleum pitch, the petroleum pitch after recovery can reach the requirement to AH-70 pitch in GB/T151980-2000.
Above-mentioned detailed description of compounded injectivity profile modifying agents and preparation method thereof being carried out with reference to embodiment; illustrative instead of determinate; several embodiments can be listed according to institute's limited range; therefore in the change do not departed under general plotting of the present invention and amendment, should belong within protection scope of the present invention.

Claims (1)

1. utilize the extract of wax tailings to reclaim a method for aged petroleum pitch, it is characterized in that concrete step is as follows:
1) preparation of the distillate of 300 DEG C is greater than
Use true boiling point distillation instrument by wax tailings in residual voltage for carrying out underpressure distillation under about 10mmHg, be filled with 6 × 6mm stainless steel protruded packing in distillation column, distillation obtains being less than the distillate of 300 DEG C and being greater than the distillate of 300 DEG C, reclaims respectively; Concrete steps are as follows:
(1) connect true boiling point distillation instrument, start vacuum pump, make residual voltage in true boiling point distillation instrument keep 10mmHg;
(2) thermal still and distillation column is added;
(3) obtain being less than the distillate of 300 DEG C and being greater than the distillate of 300 DEG C; Be 10 ~ 15mmHg with tower top pressure reduction at the bottom of still, the speed of distillating is 3 ~ 5mLmin -1;
(4), when still temperature is close to 300 DEG C, stops all heating, unload electric furnace, accelerating cooling;
(5) when still temperature drop is to less than 150 DEG C, slowly put into air by blow-off valve, make residual voltage increase, then stop vacuum pump, continue to put into air, until system recovery normal pressure;
2) solvent extraction:
By solvent and step 1) distillate being greater than 300 DEG C that obtains is mixed to join in pulsed extraction column according to weight ratio 1: 1-6: 1 and carries out extracting, obtain extracting oil out and raffinating oil; Described solvent is: furfural, phenol or N-Methyl pyrrolidone;
3) preparation of bitumen regenerant:
By step 2) extraction prepared oil and AH-70 pitch mixes according to the weight ratio of 1: 9-9: 1, prepares bitumen regenerant;
4) regeneration of aged petroleum pitch:
(1) the useless compound that old asphalt pavement milling is got off is screened, then Separation and Recovery aged petroleum pitch;
(2) aged petroleum pitch bitumen regenerant and step (1) reclaimed, according to the ratio Hybrid Heating of weight ratio 1: 1.2-1: 10, fully stirs.
CN201410271715.0A 2014-06-12 2014-06-12 A kind of method utilizing the extract of wax tailings to reclaim aged petroleum pitch Expired - Fee Related CN104032652B (en)

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113201225A (en) * 2021-05-17 2021-08-03 山东京博石油化工有限公司 Method for improving ductility of inferior asphalt

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS54120627A (en) * 1978-03-13 1979-09-19 Nittetsu Kakoki Kk Regenaration of asphalt concrete
US4238241A (en) * 1978-07-12 1980-12-09 Schneider Gordon L Acidic asphaltic composition and method
CN1085620A (en) * 1992-10-14 1994-04-20 贵州省公路局 Regenerant for old bituminous-coated macadam
CN1580130A (en) * 2004-05-19 2005-02-16 杨林江 Waste alphalt regenerating agent and its preparing method
CN101041743A (en) * 2006-03-24 2007-09-26 孙延忠 Pavement bitumen regenerative agent
CN102604401A (en) * 2012-03-31 2012-07-25 英达热再生有限公司 SBR (styrene butadiene rubber) modified recycling agent for aged asphalt road surface in alpine regions, and preparation method and usage of the recycling agent

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS54120627A (en) * 1978-03-13 1979-09-19 Nittetsu Kakoki Kk Regenaration of asphalt concrete
US4238241A (en) * 1978-07-12 1980-12-09 Schneider Gordon L Acidic asphaltic composition and method
CN1085620A (en) * 1992-10-14 1994-04-20 贵州省公路局 Regenerant for old bituminous-coated macadam
CN1580130A (en) * 2004-05-19 2005-02-16 杨林江 Waste alphalt regenerating agent and its preparing method
CN101041743A (en) * 2006-03-24 2007-09-26 孙延忠 Pavement bitumen regenerative agent
CN102604401A (en) * 2012-03-31 2012-07-25 英达热再生有限公司 SBR (styrene butadiene rubber) modified recycling agent for aged asphalt road surface in alpine regions, and preparation method and usage of the recycling agent

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Address after: 266000 No. 57 East Huaihe Road, Qingdao economic and Technological Development Zone, Shandong

Co-patentee after: CHINA University OF PETROLEUM (EAST CHINA)

Patentee after: QINGDAO HUI CHENG ENVIRONMENTAL TECHNOLOGY Co.,Ltd.

Address before: 266000 No. 57 East Huaihe Road, Qingdao economic and Technological Development Zone, Shandong

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Address after: 266555 No. 66 West Changjiang Road, Qingdao economic and Technological Development Zone, Shandong

Patentee after: CHINA University OF PETROLEUM (EAST CHINA)

Address before: 266000 No. 57 East Huaihe Road, Qingdao economic and Technological Development Zone, Shandong

Co-patentee before: CHINA University OF PETROLEUM (EAST CHINA)

Patentee before: QINGDAO HUI CHENG ENVIRONMENTAL TECHNOLOGY Co.,Ltd.

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Granted publication date: 20160210