CN107541231B - A kind of low wax pitch and preparation method thereof - Google Patents
A kind of low wax pitch and preparation method thereof Download PDFInfo
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- CN107541231B CN107541231B CN201710911226.0A CN201710911226A CN107541231B CN 107541231 B CN107541231 B CN 107541231B CN 201710911226 A CN201710911226 A CN 201710911226A CN 107541231 B CN107541231 B CN 107541231B
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- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- 238000010438 heat treatment Methods 0.000 claims abstract description 40
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 23
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 23
- 239000001257 hydrogen Substances 0.000 claims abstract description 23
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 22
- 230000006837 decompression Effects 0.000 claims abstract description 21
- 239000003381 stabilizer Substances 0.000 claims abstract description 21
- 239000001993 wax Substances 0.000 claims description 97
- 239000003921 oil Substances 0.000 claims description 29
- -1 propyl amide amine Chemical class 0.000 claims description 21
- ILRSCQWREDREME-UHFFFAOYSA-N dodecanamide Chemical compound CCCCCCCCCCCC(N)=O ILRSCQWREDREME-UHFFFAOYSA-N 0.000 claims description 20
- IPCSVZSSVZVIGE-UHFFFAOYSA-N hexadecanoic acid Chemical compound CCCCCCCCCCCCCCCC(O)=O IPCSVZSSVZVIGE-UHFFFAOYSA-N 0.000 claims description 20
- WGYKZJWCGVVSQN-UHFFFAOYSA-N propylamine Chemical compound CCCN WGYKZJWCGVVSQN-UHFFFAOYSA-N 0.000 claims description 20
- 238000004821 distillation Methods 0.000 claims description 19
- ZQPPMHVWECSIRJ-KTKRTIGZSA-N oleic acid Chemical compound CCCCCCCC\C=C/CCCCCCCC(O)=O ZQPPMHVWECSIRJ-KTKRTIGZSA-N 0.000 claims description 18
- WRIDQFICGBMAFQ-UHFFFAOYSA-N (E)-8-Octadecenoic acid Natural products CCCCCCCCCC=CCCCCCCC(O)=O WRIDQFICGBMAFQ-UHFFFAOYSA-N 0.000 claims description 17
- LQJBNNIYVWPHFW-UHFFFAOYSA-N 20:1omega9c fatty acid Natural products CCCCCCCCCCC=CCCCCCCCC(O)=O LQJBNNIYVWPHFW-UHFFFAOYSA-N 0.000 claims description 17
- QSBYPNXLFMSGKH-UHFFFAOYSA-N 9-Heptadecensaeure Natural products CCCCCCCC=CCCCCCCCC(O)=O QSBYPNXLFMSGKH-UHFFFAOYSA-N 0.000 claims description 17
- 239000005642 Oleic acid Substances 0.000 claims description 17
- ZQPPMHVWECSIRJ-UHFFFAOYSA-N Oleic acid Natural products CCCCCCCCC=CCCCCCCCC(O)=O ZQPPMHVWECSIRJ-UHFFFAOYSA-N 0.000 claims description 17
- QXJSBBXBKPUZAA-UHFFFAOYSA-N isooleic acid Natural products CCCCCCCC=CCCCCCCCCC(O)=O QXJSBBXBKPUZAA-UHFFFAOYSA-N 0.000 claims description 17
- 238000000034 method Methods 0.000 claims description 13
- 239000000463 material Substances 0.000 claims description 12
- 239000002199 base oil Substances 0.000 claims description 8
- 238000001816 cooling Methods 0.000 claims description 7
- 238000007670 refining Methods 0.000 claims description 6
- 125000000217 alkyl group Chemical group 0.000 claims description 3
- 239000012188 paraffin wax Substances 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 2
- 239000010426 asphalt Substances 0.000 abstract description 24
- 238000005265 energy consumption Methods 0.000 abstract description 2
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 6
- 239000010779 crude oil Substances 0.000 description 6
- 238000005194 fractionation Methods 0.000 description 6
- 238000002844 melting Methods 0.000 description 6
- 230000008018 melting Effects 0.000 description 6
- 244000269722 Thea sinensis Species 0.000 description 5
- 239000003513 alkali Substances 0.000 description 5
- 239000002585 base Substances 0.000 description 5
- 238000004939 coking Methods 0.000 description 5
- 235000009508 confectionery Nutrition 0.000 description 5
- 230000000694 effects Effects 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 230000035515 penetration Effects 0.000 description 5
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- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- SNRUBQQJIBEYMU-UHFFFAOYSA-N Dodecane Natural products CCCCCCCCCCCC SNRUBQQJIBEYMU-UHFFFAOYSA-N 0.000 description 2
- 210000000038 chest Anatomy 0.000 description 2
- 125000003438 dodecyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 2
- 239000002010 green coke Substances 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- RZYKUPXRYIOEME-UHFFFAOYSA-N CCCCCCCCCCCC[S] Chemical compound CCCCCCCCCCCC[S] RZYKUPXRYIOEME-UHFFFAOYSA-N 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 239000004215 Carbon black (E152) Substances 0.000 description 1
- 206010022998 Irritability Diseases 0.000 description 1
- 244000147568 Laurus nobilis Species 0.000 description 1
- 235000017858 Laurus nobilis Nutrition 0.000 description 1
- 235000021314 Palmitic acid Nutrition 0.000 description 1
- 235000005212 Terminalia tomentosa Nutrition 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
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- 150000001412 amines Chemical class 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
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- 230000009286 beneficial effect Effects 0.000 description 1
- 238000009835 boiling Methods 0.000 description 1
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- PSLIMVZEAPALCD-UHFFFAOYSA-N ethanol;ethoxyethane Chemical compound CCO.CCOCC PSLIMVZEAPALCD-UHFFFAOYSA-N 0.000 description 1
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- WQEPLUUGTLDZJY-UHFFFAOYSA-N n-Pentadecanoic acid Natural products CCCCCCCCCCCCCCC(O)=O WQEPLUUGTLDZJY-UHFFFAOYSA-N 0.000 description 1
- HLERILKGMXJNBU-UHFFFAOYSA-N norvaline betaine Chemical compound CCCC(C([O-])=O)[N+](C)(C)C HLERILKGMXJNBU-UHFFFAOYSA-N 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
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Landscapes
- Working-Up Tar And Pitch (AREA)
- Compositions Of Macromolecular Compounds (AREA)
Abstract
The invention discloses a kind of low wax pitch and preparation methods.The low wax pitch after heat treatment obtains low wax pitch by adding hydrogen supply agent and stabilizer in decompression residuum.Compared with prior art, low wax wax content in asphalt prepared by the present invention is low, performance is stable, and preparation process flow is simple, energy consumption is low.
Description
Technical field
The present invention relates to field of bitumen technology more particularly to a kind of low wax pitch and preparation method thereof.
Background technique
Pitch just has begun used in ancient times as a kind of natural engineering material, later due to extensive use and
It is largely manually extracted from petroleum or coal tar, many aspects being applied in our lives provide for our life
Convenience.Asphalt performance is excellent, and it is close to be mainly used in road pavement, roof water-proof, hydraulic engineering as a kind of engineering material
Envelope etc., using extremely extensively especially in terms of road pavement, the highway in the whole world 90% is mixed with pitch at present
Based on material tube face.With the quickening of highway in China especially expressway construction, there is huge space in Asphalt market.
Since China's Chinese Crude Oils are mostly paraffinic base crude oil, pitch wax content produced is high, and ductility and consistency are lower,
Strong to the irritability of temperature, pavement performance is poor, it is difficult to reach the requirement of high-grade highway construction.Although China is always for many years
It is dedicated to researching and developing the production of high-grade highway pitch, but due to the road asphalt durability of domestic most of crude oil productions
Difference, the disadvantages of wax content is high, hinder its use on high-grade highway.Currently, providing wax in external road asphalt standard
Content≤2.0wt% provides wax content≤3.0wt% in China's heavy duty road asphalt standard GB/T/T15180-2000,
A grades of pitch wax content≤2.2wt% are provided in standard specification for construction and acceptance of highway asphalt pavement JTG F40-2004.
Studies have shown that wax has extreme influence to Service Performance of Asphalt Pavement.Wax content in asphalt is excessively high, makes to drip at high temperature
Blueness is easy to feel like jelly, and leads to the reduction of bituminous pavement high-temperature stability, track occurs；Equally, pitch can be made to become brittle in low temperature,
Lead to the reduction of road surface low-temperature cracking-resistance, slight crack occurs.In addition, wax can make the reduction of the adhesiveness of pitch and building stones, in the item for having water
Under part, road surface stone can be made to generate peeling phenomenon, cause pavement destruction.More seriously, wax containing asphalt can make bituminous pavement
Skid resistance reduces, and influences the traffic safety on road surface.
Currently, the crude oil of China's nearly half is paraffinic base or intermediate base, the road asphalt wax content produced is higher.Cause
This, in order to sufficiently develop and use domestic existing crude resources, exploitation reduces wax content technology to improve road asphalt
Quality is of great significance.
Summary of the invention
In view of the above drawbacks of the prior art, the technical problem to be solved by the present invention is to be depressurized using paraffinic base crude oil
The decompression residuum obtained after distillation develops a kind of wax drop technique, prepares low wax pitch.
To achieve the above object, the present invention provides a kind of preparation methods of low wax pitch, it is characterised in that comprising following
Step:
A. 8~10 parts by weight decompression residuum, 0.8~1.5 parts by weight hydrogen supply agent, 1.0~2.0 parts by weight stabilizers are mixed
Melting obtains fusant；
B. fusant is sent into wax drop reacting furnace and is heat-treated；
C. wax drop reacting furnace tower bottom oil is sent and is fractionated into vacuum tower；
D. vacuum tower base oil is through pump output to get low wax pitch.
Preferably, a kind of preparation method of low wax pitch, it is characterised in that comprise the steps of:
A. 8~10 parts by weight decompression residuum, 0.8~1.5 parts by weight hydrogen supply agent, 1.0~2.0 parts by weight stabilizers are added
It is heated to obtain fusant into heating furnace 1；
B. fusant in heating furnace 1 is delivered in wax drop reacting furnace 3 by pump 2 and is heat-treated；
C. 3 tower bottom oil of wax drop reacting furnace is delivered in vacuum furnace 5 by pump 4 and is heated, subsequently entered in vacuum tower 6 and carry out
Fractionation；It is back in vacuum tower 6 after wherein 6 second line of distillation oil of vacuum tower is cooling；
D. 6 base oil of vacuum tower through pump 7 from tower bottom export, exchanged heat, cool down after obtain low wax pitch.
Preferably, the feeding temperature of the wax drop reacting furnace 3 is 200~220 DEG C, and temperature is 330~350 in burner hearth
DEG C, furnace pressure is maintained at 200~206KPa, and control material is 80~100min in dwell time in the tower, wax drop reacting furnace 3
Feeding temperature passes through 2 control of heating furnace 1 and pump.
Preferably, the feeding temperature of the vacuum furnace 5 is 330~350 DEG C, and drop temperature is 380~400 DEG C.
Preferably, the feeding temperature of the vacuum tower 6 is 380~400 DEG C, and vacuum degree is 90~93KPa, tower top temperature
It is 40~60 DEG C, column bottom temperature is 340~360 DEG C, and second line of distillation oil is back in vacuum tower 6.
Preferably, the decompression residuum is the decompression residuum that paraffinic base crude oil obtains after reduced pressure distillation process,
Middle wax content is 4.0~6.0wt%.
Preferably, the hydrogen supply agent is one or more of palmitinic acid, oleic acid；
It is further preferred that the hydrogen supply agent is mixed by palmitinic acid and oleic acid, the wherein weight of palmitinic acid and oleic acid
Amount is than being (1~3): (1~3).
Palmitinic acid and oleic acid boiling point with higher, while containing active hydrogen on carboxyl, the condensation of asphalitine can be inhibited
Reaction carries out, and reduces the generation of green coke.
Preferably, the stabilizer is by cocamidopropyl propyl amide amine oxide, dodecanamide propyl amine oxide, dodecyl sulphur
Propyl betaine 1:1:1 in mass ratio, which is stirred evenly, to be obtained by mixing.
Cocamidopropyl propyl amide amine oxide, dodecanamide propyl amine oxide, dodecyl azochlorosulfonate propyl lycine have parents spy
Property.It is adsorbed in asphalitine, the solvability of asphalitine with peptized asphaltenes, can be made to increase, reduce the aggregation of asphalitine, reduced
Asphalitine chemical polymerization and association, to improve the stability of system.
Beneficial effects of the present invention:
1, a kind of preparation method of low wax pitch of the present invention carries out heat to decompression residuum after addition hydrogen supply agent and stabilizer
Processing, is especially added to palmitinic acid and oleic acid, and controls heat treatment temperature at 330~350 DEG C, heat treatment time 80~
100min.Ensure that heat treatment degree is moderate, will not a large amount of green cokes, destroy residual oil colloidal dispersion, influence the service performance of pitch.Together
When ensure the cracking severity of residual oil, the wax content in decompression residuum is greatly reduced, finally obtains the low wax pitch of function admirable.
2, a kind of preparation method of low wax pitch of the present invention compares traditional straight asphalt technique, and it is simple to have a process, energy consumption
The features such as low, meets the demand of environmentally friendly sustainable development.
3, low wax pitch prepared by the present invention at 25 DEG C needle penetration (1/10mm) >=63, softening point >=53 DEG C, at 15 DEG C
Ductility >=100cm, wax content≤2.2%.Standard specification for construction and acceptance of highway asphalt pavement JTG F40-2004 is complied fully with to road
The technical requirements of pitch.
Detailed description of the invention
Fig. 1 is low wax pitch preparation technology flow chart
Appended drawing reference: 1 is heating furnace, and 2 be pump, and 3 be wax drop reacting furnace, and 4 be pump, and 5 be vacuum furnace, and 6 be vacuum tower, and 7 are
Pump.
Specific embodiment
Each raw material sources in embodiment:
Decompression residuum: Xinjiang Jiu Qu decompression residuum, paraffin content 5.0wt%, Xinjiang Zhong Hua Ke Run Limited Liability Co., Ltd；
Palmitinic acid: also known as palmitic acid, No. CAS: 57-10-3, content >=99.0%, Guangzhou Yin Lin Chemical Co., Ltd.；
Oleic acid: No. CAS: 112-80-1, content >=99.9%, Shandong De Fa Chemical Co., Ltd.；
Cocamidopropyl propyl amide amine oxide: No. CAS: 68155-09-9, active matter content 30%, upper sea blue wild chemical industry is limited
Company；
Dodecanamide propyl amine oxide: No. CAS: 61792-31-2, active matter content 30%, the green gloomy chemical industry of Linyi City has
Limit company；
Dodecyl azochlorosulfonate propyl lycine: No. CAS: 683-10-3, active matter content 30%, Henan Zhong Haiyuan chemical industry produces
Product Co., Ltd；
Embodiment 1
As shown in Figure 1, a kind of preparation method of low wax pitch comprising the steps of:
A. 9 parts by weight Xinjiang Jiu Qu decompression residuum, 1.0 parts by weight hydrogen supply agents, 1.5 parts by weight stabilizers are added to heating
Heating melting is carried out in furnace 1；
B. fusant in heating furnace 1 is delivered in wax drop reacting furnace 3 by pump 2 and is heat-treated；
C. 3 tower bottom oil of wax drop reacting furnace is delivered in vacuum furnace 5 by pump 4 and is heated, subsequently entered in vacuum tower 6 and carry out
Fractionation；It is back in vacuum tower 6 after wherein 6 second line of distillation oil of vacuum tower is cooling；
D. 6 base oil of vacuum tower through pump 7 from tower bottom export, then exchanged heat, cool down after obtain low wax pitch.
The feeding temperature of the wax drop reacting furnace 3 is 220 DEG C, and temperature is 310 DEG C in burner hearth, and furnace pressure is maintained at
206KPa, control material are 90min in dwell time in the tower, and the feeding temperature of wax drop reacting furnace 3 passes through 2 control of heating furnace 1 and pump
System.
The feeding temperature of the vacuum furnace 5 is 310 DEG C, and drop temperature is 400 DEG C.
The feeding temperature of the vacuum tower 6 is 400 DEG C, vacuum degree 93KPa, and tower top temperature is 60 DEG C, column bottom temperature
It is 360 DEG C, second line of distillation oil is back in vacuum tower 6.
Refining amount is controlled in 50m3/h。
The hydrogen supply agent is that palmitinic acid and oleic acid 1:1 in mass ratio are uniformly mixed and form.
The stabilizer is by cocamidopropyl propyl amide amine oxide, dodecanamide propyl amine oxide, dodecyl sulfopropyl sweet tea
Dish alkali 1:1:1 in mass ratio is uniformly mixed and forms.
Embodiment 2
As shown in Figure 1, a kind of preparation method of low wax pitch comprising the steps of:
A. 9 parts by weight Xinjiang Jiu Qu decompression residuum, 1.0 parts by weight hydrogen supply agents, 1.5 parts by weight stabilizers are added to heating
Heating melting is carried out in furnace 1；
B. fusant in heating furnace 1 is delivered in wax drop reacting furnace 3 by pump 2 and is heat-treated；
C. 3 tower bottom oil of wax drop reacting furnace is delivered in vacuum furnace 5 by pump 4 and is heated, subsequently entered in vacuum tower 6 and carry out
Fractionation；It is back in vacuum tower 6 after wherein 6 second line of distillation oil of vacuum tower is cooling；
D. 6 base oil of vacuum tower through pump 7 from tower bottom export, then exchanged heat, cool down after obtain low wax pitch.
The feeding temperature of the wax drop reacting furnace 3 is 220 DEG C, and temperature is 320 DEG C in burner hearth, and furnace pressure is maintained at
206KPa, control material are 90min in dwell time in the tower, and the feeding temperature of wax drop reacting furnace 3 passes through 2 control of heating furnace 1 and pump
System.
The feeding temperature of the vacuum furnace 5 is 320 DEG C, and drop temperature is 400 DEG C.
The feeding temperature of the vacuum tower 6 is 400 DEG C, vacuum degree 93KPa, and tower top temperature is 60 DEG C, column bottom temperature
It is 360 DEG C, second line of distillation oil is back in vacuum tower 6.
Refining amount is controlled in 50m3/h。
The hydrogen supply agent is that palmitinic acid and oleic acid 1:1 in mass ratio are uniformly mixed and form.
The stabilizer is by cocamidopropyl propyl amide amine oxide, dodecanamide propyl amine oxide, dodecyl sulfopropyl sweet tea
Dish alkali 1:1:1 in mass ratio is uniformly mixed and forms.
Embodiment 3
As shown in Figure 1, a kind of preparation method of low wax pitch comprising the steps of:
A. 9 parts by weight Xinjiang Jiu Qu decompression residuum, 1.0 parts by weight hydrogen supply agents, 1.5 parts by weight stabilizers are added to heating
Heating melting is carried out in furnace 1；
B. fusant in heating furnace 1 is delivered in wax drop reacting furnace 3 by pump 2 and is heat-treated；
C. 3 tower bottom oil of wax drop reacting furnace is delivered in vacuum furnace 5 by pump 4 and is heated, subsequently entered in vacuum tower 6 and carry out
Fractionation；It is back in vacuum tower 6 after wherein 6 second line of distillation oil of vacuum tower is cooling；
D. 6 base oil of vacuum tower through pump 7 from tower bottom export, then exchanged heat, cool down after obtain low wax pitch.
The feeding temperature of the wax drop reacting furnace 3 is 220 DEG C, and temperature is 360 DEG C in burner hearth, and furnace pressure is maintained at
206KPa, control material are 90min in dwell time in the tower, and the feeding temperature of wax drop reacting furnace 3 passes through 2 control of heating furnace 1 and pump
System.
The feeding temperature of the vacuum furnace 5 is 360 DEG C, and drop temperature is 400 DEG C.
The feeding temperature of the vacuum tower 6 is 400 DEG C, vacuum degree 93KPa, and tower top temperature is 60 DEG C, column bottom temperature
It is 360 DEG C, second line of distillation oil is back in vacuum tower 6.
Refining amount is controlled in 50m3/h。
The hydrogen supply agent is that palmitinic acid and oleic acid 1:1 in mass ratio are uniformly mixed and form.
The stabilizer is by cocamidopropyl propyl amide amine oxide, dodecanamide propyl amine oxide, dodecyl sulfopropyl sweet tea
Dish alkali 1:1:1 in mass ratio is uniformly mixed and forms.
Embodiment 4
As shown in Figure 1, a kind of preparation method of low wax pitch comprising the steps of:
A. 9 parts by weight Xinjiang Jiu Qu decompression residuum, 1.0 parts by weight hydrogen supply agents, 1.5 parts by weight stabilizers are added to heating
Heating melting is carried out in furnace 1；
B. fusant in heating furnace 1 is delivered in wax drop reacting furnace 3 by pump 2 and is heat-treated；
C. 3 tower bottom oil of wax drop reacting furnace is delivered in vacuum furnace 5 by pump 4 and is heated, subsequently entered in vacuum tower 6 and carry out
Fractionation；It is back in vacuum tower 6 after wherein 6 second line of distillation oil of vacuum tower is cooling；
D. 6 base oil of vacuum tower through pump 7 from tower bottom export, then exchanged heat, cool down after obtain low wax pitch.
The feeding temperature of the wax drop reacting furnace 3 is 220 DEG C, and temperature is 370 DEG C in burner hearth, and furnace pressure is maintained at
206KPa, control material are 90min in dwell time in the tower, and the feeding temperature of wax drop reacting furnace 3 passes through 2 control of heating furnace 1 and pump
System.
The feeding temperature of the vacuum furnace 5 is 370 DEG C, and drop temperature is 400 DEG C.
The feeding temperature of the vacuum tower 6 is 400 DEG C, vacuum degree 93KPa, and tower top temperature is 60 DEG C, column bottom temperature
It is 360 DEG C, second line of distillation oil is back in vacuum tower 6.
Refining amount is controlled in 50m3/h。
The hydrogen supply agent is that palmitinic acid and oleic acid 1:1 in mass ratio are uniformly mixed and form.
The stabilizer is by cocamidopropyl propyl amide amine oxide, dodecanamide propyl amine oxide, dodecyl sulfopropyl sweet tea
Dish alkali 1:1:1 in mass ratio is uniformly mixed and forms.
Embodiment 5
As shown in Figure 1, a kind of preparation method of low wax pitch comprising the steps of:
A. 9 parts by weight Xinjiang Jiu Qu decompression residuum, 1.0 parts by weight hydrogen supply agents, 1.5 parts by weight stabilizers are added to heating
Heating melting is carried out in furnace 1；
B. fusant in heating furnace 1 is delivered in wax drop reacting furnace 3 by pump 2 and is heat-treated；
C. 3 tower bottom oil of wax drop reacting furnace is delivered in vacuum furnace 5 by pump 4 and is heated, subsequently entered in vacuum tower 6 and carry out
Fractionation；It is back in vacuum tower 6 after wherein 6 second line of distillation oil of vacuum tower is cooling；
D. 6 base oil of vacuum tower through pump 7 from tower bottom export, then exchanged heat, cool down after obtain low wax pitch.
The feeding temperature of the wax drop reacting furnace 3 is 220 DEG C, and temperature is 340 DEG C in burner hearth, and furnace pressure is maintained at
206KPa, control material are 90min in dwell time in the tower, and the feeding temperature of wax drop reacting furnace 3 passes through 2 control of heating furnace 1 and pump
System.
The feeding temperature of the vacuum furnace 5 is 340 DEG C, and drop temperature is 400 DEG C.
The feeding temperature of the vacuum tower 6 is 400 DEG C, vacuum degree 93KPa, and tower top temperature is 60 DEG C, column bottom temperature
It is 360 DEG C, second line of distillation oil is back in vacuum tower 6.
Refining amount is controlled in 50m3/h。
The hydrogen supply agent is that palmitinic acid and oleic acid 1:1 in mass ratio are uniformly mixed and form.
The stabilizer is by cocamidopropyl propyl amide amine oxide, dodecanamide propyl amine oxide, dodecyl sulfopropyl sweet tea
Dish alkali 1:1:1 in mass ratio is uniformly mixed and forms.
Embodiment 6
Substantially the same manner as Example 5, difference is only in that: the feeding temperature of the wax drop reacting furnace 3 is 220 DEG C, furnace
Temperature is 330 DEG C in thorax, and furnace pressure is maintained at 206KPa, and control material is 90min, wax drop reacting furnace in dwell time in the tower
3 feeding temperature passes through 2 control of heating furnace 1 and pump.
The feeding temperature of the vacuum furnace 5 is 330 DEG C, and drop temperature is 400 DEG C.
Embodiment 7
Substantially the same manner as Example 5, difference is only in that: the feeding temperature of the wax drop reacting furnace 3 is 220 DEG C, furnace
Temperature is 350 DEG C in thorax, and furnace pressure is maintained at 206KPa, and control material is 90min, wax drop reacting furnace in dwell time in the tower
3 feeding temperature passes through 2 control of heating furnace 1 and pump.
The feeding temperature of the vacuum furnace 5 is 350 DEG C, and drop temperature is 400 DEG C.
Embodiment 8
Substantially the same manner as Example 5, difference is only in that: the hydrogen supply agent is palmitinic acid.
Embodiment 9
Substantially the same manner as Example 5, difference is only in that: the hydrogen supply agent is oleic acid.
Embodiment 10
Substantially the same manner as Example 5, difference is only in that: the stabilizer is by cocamidopropyl propyl amide amine oxide and laurel
Amidopropyl amine oxide 1:1 in mass ratio is uniformly mixed and forms.
Embodiment 11
Substantially the same manner as Example 5, difference is only in that: the stabilizer is by dodecanamide propyl amine oxide and 12
Alkyl azochlorosulfonate propyl lycine 1:1 in mass ratio is uniformly mixed and forms.
Embodiment 12
Substantially the same manner as Example 5, difference is only in that: the stabilizer is by cocamidopropyl propyl amide amine oxide and 12
Alkyl azochlorosulfonate propyl lycine 1:1 in mass ratio is uniformly mixed and forms.
Test case 1
The test method of coking yield:
It takes 1g oil sample to be placed in 250mL conical flask, 100mL toluene is added, stand 1h after vibrating 30min, weigh filter paper weight
It after measuring m, is filtered with filter paper, uses toluene shower during filtering, until filtrate is colourless.Filter paper is put into vacuum oven,
Dry 60min, is cooled to room temperature, weighs filter weight m` at 105 DEG C.Coking yield is oil sample matter shared by the increased quality of filter paper
The percentage of amount.
Cracking distillation method measures wax content:
50g ± 1g sample is weighed, accurately to 0.01g.Sample is put into cracking distillation bottle and is distilled.It is completed in 25min
Distillation process collects fraction with conical flask weighed in advance, weighs up the quality after collecting.Take the appropriate distillate sample (no
Obtain more than 10g), it is accurate to claim to 0.001g, make the wax content measured 50 between 100mg.With the diethylether-ethanol of same ratio
Mixed liquor makees dewaxing agent, and every gram of sample is added 10mL mixed liquor, dewaxes under conditions of -20 DEG C ± 0.5 DEG C.By gatch petroleum
It is dried in vacuo (400~500mmHg negative pressure, 105~110 DEG C) after ether dissolution, measures the quality of wax.Wax is calculated with following formula to contain
It measures X (%):
X=100% × (D × P) ÷ (S × d)
Wherein, S-sample amount (g)；D-distillates oil mass (g)；Sampling amount (g) in d-distillate oil；P-gained
Wax amount (g).
The test method of wax content is referring to " People's Republic of China's petrochemical industry standard (SH/T 0425-2003) stone
Oil asphalt wax content measuring method ", embodiment 1-9 is tested.
Influence of the 1 different heat treatment temperature of table to low wax pitch preparation process
| Embodiment | Heat treatment temperature (DEG C) | Coking yield % | Wax content % |
| Embodiment 1 | 310 | 0.02 | 3.9 |
| Embodiment 2 | 320 | 0.04 | 2.8 |
| Embodiment 3 | 360 | 0.18 | 3.0 |
| Embodiment 4 | 370 | 0.33 | 3.7 |
| Embodiment 5 | 340 | 0.06 | 1.5 |
| Embodiment 6 | 330 | 0.05 | 1.7 |
| Embodiment 7 | 350 | 0.08 | 1.9 |
| Embodiment 8 | 340 | 0.06 | 2.0 |
| Embodiment 9 | 340 | 0.06 | 2.1 |
By the comparison of Examples 1 to 9 it can be found that carrying out hot place after adding hydrogen agent, stabilizer to decompression residuum altogether
Reason, when heat treatment temperature is less than 330 DEG C, wax drop effect is general, and obtained wax content in asphalt is in 2.2wt% or more, Bu Nengda
To requirement；At 330~350 DEG C, wax drop significant effect is promoted heat treatment temperature, and wax content in asphalt is in 2.2wt% hereinafter, same
When coking yield below 0.1%；When heat treatment temperature is greater than 350 DEG C, the decline of wax drop significant effect, while coking yield is much larger than
0.1%, seriously affect asphalt performance.Its reason may is that, fragrant in aromatic wax in decompression residuum when heat treatment temperature is too low
Hydrocarbon and cycloalkane side chain, Long carbon chain cracking severity are inadequate, and wax drop effect is not significant；Heat treatment temperature is excessively high, palmitinic acid, oleic acid from
Volatilization causes hydrogen supply effect to weaken significantly to lead to wax drop decreased effectiveness in decompression residuum, while heat treatment temperature is excessively high leads to green coke
Rate is excessively high.
Comparing embodiment 5 and embodiment 8,9, the paraffin content of the pitch of embodiment 5 (compounding of palmitinic acid and oleic acid) preparation
Significantly lower than embodiment 8,9 (only addition one of palmitinic acid and oleic acid).
Test case 2
Softening point: the softening point of pitch indicates in the presence of certain external force, and pitch is heated from solid or sticky to be not easy to flow
Dynamic substance is changed into the temperature of the states of matter with certain fluid ability.Softening point tests GB/T4507- according to national standards
The regulation of 1999 " asphalt softening point measuring method (ring and ball methods) " carries out.
Needle penetration: the needle penetration of pitch refers in the constant temperature bath that sample is placed in 25 ± 0.1 DEG C, the standard of loading 100g
Needle moves vertically under without obvious friction, the depth of vertical injection bitumen samples, referred to as Asphalt Penetration in 5 seconds.Needle enters
Degree is tested by the regulation of standard GB/T/T4509-2010 " petroleum asphalt penetration measuring method ".
Ductility: the ductility of pitch is that pitch is made into 8 font standard specimens, according to requiring to use temperature for 15 DEG C, with 5cm
Length when speed tensile per minute to fracture.Ductility presses the rule of standard GB/T/T 4508-1999 " effecting determination of asphalt ductility method "
Surely it is tested.
Viscous toughness: viscous toughness test be measure pitch at the specified temperature high-speed stretch when with the viscous toughness of metal hemisphere and
Toughness." pitch glues toughness examination by People's Republic of China's petrochemical industry standard SH/T 0735-2003 for viscous toughness and toughness
Proved recipe method " regulation tested.
The performance parameter of low wax pitch obtained in 2 embodiment 5,8,9 of table
The preferred embodiment of the present invention has been described in detail above.It should be appreciated that those skilled in the art without
It needs creative work according to the present invention can conceive and makes many modifications and variations.Therefore, all technologies in the art
Personnel are available by logical analysis, reasoning, or a limited experiment on the basis of existing technology under this invention's idea
Technical solution, all should be within the scope of protection determined by the claims.
Claims (6)
1. a kind of preparation method of low wax pitch, it is characterised in that comprise the steps of:
A. 8 ~ 10 parts by weight decompression residuum, 0.8 ~ 1.5 parts by weight hydrogen supply agent, 1.0 ~ 2.0 parts by weight stabilizers are added to heating
It is heated to obtain fusant in furnace；The hydrogen supply agent is mixed by palmitinic acid and oleic acid, wherein palmitinic acid and oleic acid
Weight ratio is (1 ~ 3): (1 ~ 3)；The stabilizer is by cocamidopropyl propyl amide amine oxide, dodecanamide propyl amine oxide, 12
Alkyl azochlorosulfonate propyl lycine 1:1:1 in mass ratio, which is stirred evenly, to be obtained by mixing；
B. fusant in heating furnace is delivered in wax drop reacting furnace by pump and is heat-treated；The wax drop reacting furnace
Feeding temperature is 200 ~ 220 DEG C, and temperature is 330 ~ 350 DEG C in burner hearth, and furnace pressure is maintained at 200 ~ 206 KPa, controls material
It is 80 ~ 100 min in dwell time in the tower；
C. wax drop reacting furnace tower bottom oil is delivered in vacuum furnace by pump and is heated, subsequently entered in vacuum tower and be fractionated；Its
It is back in vacuum tower after middle vacuum tower second line of distillation oil is cooling；
D. vacuum tower base oil pumped from tower bottom export, then exchanged heat, cool down after obtain low wax pitch.
2. the preparation method of low wax pitch as described in claim 1, it is characterised in that: the feeding temperature of the vacuum furnace is
330 ~ 350 DEG C, drop temperature is 380 ~ 400 DEG C.
3. the preparation method of low wax pitch as described in claim 1, it is characterised in that: the feeding temperature of the vacuum tower is
380 ~ 400 DEG C, vacuum degree is 90 ~ 93 KPa, and tower top temperature is 40 ~ 60 DEG C, and column bottom temperature is 340 ~ 360 DEG C.
4. the preparation method of low wax pitch as described in claim 1, it is characterised in that: the decompression residuum is paraffin base
The decompression residuum that oil obtains after reduced pressure distillation process, wherein wax content is 4.0 ~ 6.0 wt%.
5. the preparation method of low wax pitch as described in claim 1, it is characterised in that: 40 ~ 60 m of refining amount of the process flow3/
h。
6. the low wax pitch that method is prepared either described in -5 according to claim 1.
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| CN201485417U (en) * | 2009-05-31 | 2010-05-26 | 中海沥青股份有限公司 | Wax content reducing device for producing oil asphalt |
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| CN104559251A (en) * | 2013-10-22 | 2015-04-29 | 中国石油化工股份有限公司 | Zwitter-ion and nonionic composite asphalt warm-mixing agent and preparation method thereof |
| CN104711014A (en) * | 2015-03-11 | 2015-06-17 | 中国海洋石油总公司 | Hard asphalt 20# and preparation method thereof |
| CN105733283A (en) * | 2016-04-07 | 2016-07-06 | 无锡华通沥青新技术发展有限公司 | SBS-modified asphalt stabilizing agent |
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2017
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN201485417U (en) * | 2009-05-31 | 2010-05-26 | 中海沥青股份有限公司 | Wax content reducing device for producing oil asphalt |
| CN103044933A (en) * | 2011-10-17 | 2013-04-17 | 中国石油天然气股份有限公司 | Stabilizer composition for polymer modified asphalt |
| CN103525101A (en) * | 2013-09-17 | 2014-01-22 | 镇江金阳道路材料科技发展有限公司 | Novel asphalt mixture modifier capable of being warmly mixed as well as preparation method thereof and preparation method of mixture thereof |
| CN104559251A (en) * | 2013-10-22 | 2015-04-29 | 中国石油化工股份有限公司 | Zwitter-ion and nonionic composite asphalt warm-mixing agent and preparation method thereof |
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| CN105733283A (en) * | 2016-04-07 | 2016-07-06 | 无锡华通沥青新技术发展有限公司 | SBS-modified asphalt stabilizing agent |
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