CN102676210B - Hydrogenated pre-treating method for coal tar - Google Patents

Hydrogenated pre-treating method for coal tar Download PDF

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CN102676210B
CN102676210B CN201210178435.6A CN201210178435A CN102676210B CN 102676210 B CN102676210 B CN 102676210B CN 201210178435 A CN201210178435 A CN 201210178435A CN 102676210 B CN102676210 B CN 102676210B
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coal tar
oil
dewaters
extraction
extraction agent
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CN102676210A (en
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李鑫
邱泽刚
赵敏
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Shanxi Zhongke Huamei Science and Technology Co., Ltd.
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SHANXI SHENGCHI TECHNOLOGY Co Ltd
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Abstract

The invention provides a hydrogenated pre-treating method for coal tar, belongs to the technical field of hydrogenated pre-treating of coal tar, provides a pre-treatment method for removing moisture and impurities from coal tar, and adopts the technical scheme that demulsifying agent is added for removing moisture firstly, distillation is carried out for removing moisture secondly to ensure that light oil of coal tar is distilled out, and extracted heavy oil and the light oil are mixed to obtain the pre-treated coal tar thirdly. The method has the advantages that the operation cost is low; the operation is simple and convenient; coal tar can enter a hydrogenization device directly after being treated; distillation and extraction are combined to sufficiently extract effective ingredients in coal tar; the two filtering processes ensure that all impurities in coal tar are completely removed; the coal tar conversion rate is high; and suitability for coal tar comprehensive utilization and further treating is realized.

Description

A kind of coal tar hydrogenating pretreatment process
Technical field
A kind of coal tar hydrogenating pretreatment process of the present invention belongs to coal tar hydrogenating preconditioning technique field.
Background technology
Coal tar is the have irritating smell of coal at high temperature carbonization and gasification byproduct in process, and the viscous liquid product of black or chocolate, is a kind of complex mixture being mainly made up of aromatics, and its component reaches up to ten thousand kinds of materials.Coal-tar products has irreplaceable status in global industrial chemicals demand.
But domestic existing coal tar processing exists all drawbacks, a lot of enterprises directly sell coal tar as fuel, do poor product quality like this, added value is low, and also very serious to the pollution of environment.Along with continuous intensification and national standard and the requirement at increasingly stringent aspect environmental protection of market competition, adequately and reasonably utilize tar resource to become the hot issue that people more and more pay close attention to.
Hydrogenation of tar technology can be hauled out the material of the burning such as sulphur, nitrogen after stain environment in coal tar, improves smell, color and the stability of oil product, improves oil quality, is a kind of important means of coal tar comprehensive utilization.The components such as coal tar is necessary process and processing before entering hydrogenation unit, removal water, impurity and bituminous matter wherein, just can make hydrogenation process normally carry out.Therefore, to the research of coal tar preprocessing process, improving energy utilization rate, reducing energy consumption and increasing enterprise profit aspect significant.
Summary of the invention
The present invention, in order to overcome the deficiencies in the prior art, provides a kind of pretreatment process of removing coal tar water content in oil and impurity.
In order to solve the problems of the technologies described above, a kind of coal tar hydrogenating pretreatment process of the present invention, carries out according to following steps:
The first step, dewaters
Original coal tar is heated to 70-90 ℃ with 100 object strainer filterings, then in the coal tar after filtration, adds emulsion splitter and water, keep Heating temperature, standing separation water after stirring, obtains the coal tar that dewaters;
Second step, distillation
Will described in the coal tar distillation that dewaters, the light oil that obtains steaming and the heavy oil not steaming, the heavy oil not steaming by weight percentage accounts for 20% of the coal tar that dewaters;
The 3rd step, extraction
To in described heavy oil, add extraction agent to mix, be then warming up to 100-120 ℃, isolate extraction agent solvend and extraction agent insolubles, then after the extraction agent in extraction agent solvend being steamed, mix with described light oil, finally use 200 object strainer filterings, obtain pre-treatment coal tar.
The ratio of described original coal tar, emulsion splitter and water is 700-1450 (g): 1 (mL): 50-100 (mL).
Described emulsion splitter is polyethers emulsion splitter.
Described polyethers emulsion splitter is phenol amine aldehyde resin polyoxyethylene polyoxypropylene ether.
The described the first step dewater middle stirring after 0.5-3 hour leave standstill 3-5.5 hour Separation of Water.
Described in the 3rd step extraction, extraction agent is aromatic solvent.
Described aromatic solvent is one or more in benzene,toluene,xylene and high boiling aromatic hydrocarbon solvent oil.
Described in the 3rd step extraction, the volume ratio of heavy oil and extraction agent is 1:1.2-1.8.
Described pre-treatment coal tar is used as hydrogenation feed oil after mixing according to volume ratio 3:1 with diesel oil.
The present invention compared with prior art has following beneficial effect.
1, working cost is low, easy and simple to handle, and coal tar after treatment can directly enter hydrogenation unit.
2, being combined with of distillation and extraction process, has fully extracted the active principle in coal tar, and twice of front and back filtration procedure has guaranteed that the various impurity in coal tar are completely removed.
3, coal tar transformation efficiency is high, is suitable for comprehensive utilization and the further deep processing of coal tar.
Original coal tar is the coal tar without any processing.
The object of filtering is for the first time to remove solid impurity in original coal tar, comprises bulk or particulate contamination beyond the coal tar composition of accidentally sneaking in the processes such as transportation.
The object of filtering is for the second time to remove a small amount of bituminous matter and colloid etc. remaining in coal tar.After oil after filtration mixes with diesel oil, as hydrogenation feed oil, be to enter the thermal value after hydrogenation unit in order to reduce feed oil, be conducive to hydrogenation reaction and normally carry out.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described.
The condition of coal tar distillation is normal condition.The high boiling aromatic hydrocarbon solvent oil of mentioning in following examples is purchased from Wujiang grand environmental protection auxiliary agent company limited.
Embodiment 1
Get 3528g coal tar, be heated to 80 ℃, with 100 object stainless (steel) wires filtrations, in the oil after filtration, add 3ml polyethers emulsion splitter and 200ml water, keep Heating temperature, after stirring 30min, leave standstill 5h, separate water outlet 236g; Coal tar after dewatering is distilled, to distill remaining 20% heavy constituent 698g and 605g toluene by volume 1:1.2 mix, further be heated to 100 ℃, layering obtains toluene solvend and toluene insolubles, and the toluene in toluene solvend is steamed, and steaming excess quality is 449g, mix with oil after 80% distillation, filter with 200 object stainless (steel) wires again, after filtering, mix according to volume ratio 3:1 with diesel oil, obtain hydrogenation feed oil.Coal tar utilization ratio is 91.9%.Coal tar character before and after pre-treatment is in table 1.
Coal tar character (sample 1) before and after table 1 pre-treatment
Analysis project Before pre-treatment After pre-treatment
Density, kg/m 3 1010.6 909.8
Carbon residue, % 6.3 0.71
Ash content, % 0.076 0.07
Fe/Na,ppm 121.5/40.3 10.4/12.1
Ni/V,ppm 0.5/<0.1 <0.1/<0.1
Al/Cu,ppm 15.9/<0.7 3.5/<0.1
Ca/Mg,ppm 41.2/12.8 1.0/<0.1
K/Pb,ppm 3.3/<0.1 1.7/<0.1
Sulphur content, % 0.25 0.097
Nitrogen content, % 0.43 0.325
Open flash point, ℃ 128 94
Bituminous matter, % 12.40 2.89
Colloid, % 23.19 6.15
Fragrance part, % 26.78 11.84
Saturated part, % 10.29 19.20
Moisture, % 1.34 0.011
Mechanical impurity, % 2.652 0.581
Acid number, mgKOH/g 10.20 1.56
Condensation point, ℃ 20 4
Embodiment 2
Get 1465g coal tar, be heated to 70 ℃, with 100 object stainless (steel) wires filtrations, in the oil after filtration, add 2ml phenol amine aldehyde resin polyoxyethylene polyoxypropylene ether and 100ml water, keep Heating temperature, after stirring 1h, leave standstill 5h, separate water outlet 121g; Coal tar after dewatering is distilled, to distill remaining 20% heavy constituent 289g and 285g benzene by volume 1:1.4 mix, further be heated to 100 ℃, layering obtains benzene solvend and benzene insoluble, and the toluene in toluene solvend is steamed, and steaming excess quality is 203g, mix with oil after 80% distillation, filter with 200 object stainless (steel) wires again, after filtering, mix according to volume ratio 3:1 with diesel oil, obtain hydrogenation feed oil.Coal tar utilization ratio is 92.7%.Coal tar character before and after pre-treatment is in table 2.
Coal tar character (sample 2) before and after table 2 pre-treatment
Analysis project Before pre-treatment After pre-treatment
Density, kg/m 3 1022.3 912.5
Carbon residue, % 7.4 0.67
Ash content, % 0.083 0.09
Fe/Na,ppm 116.4/37.9 11.4/11.6
Ni/V,ppm 0.8/<0.1 <0.1/<0.1
Al/Cu,ppm 16.8/1.1 4.3/<0.1
Ca/Mg,ppm 24.5/15.8 3.2/0.6
K/Pb,ppm 5.7/<0.1 1.9/<0.1
Sulphur content, % 0.98 0.14
Nitrogen content, % 0.56 0.397
Open flash point, ℃ 125 91
Bituminous matter, % 15.56 3.28
Colloid, % 24.26 7.06
Fragrance part, % 22.31 11.42
Saturated part, % 11.04 18.26
Moisture, % 1.43 0.012
Mechanical impurity, % 2.379 0.524
Acid number, mgKOH/g 11.13 1.65
Condensation point, ℃ 23 6
Embodiment 3
Get 2857g coal tar, be heated to 90 ℃, with 100 object stainless (steel) wires filtrations, in the oil after filtration, add 2ml polyethers emulsion splitter and 200ml water, keep Heating temperature, after stirring 2h, leave standstill 4h, separate water outlet 224g; Coal tar after dewatering is distilled, to distill remaining 20% heavy constituent 513g and 560g dimethylbenzene by volume 1:1.5 mix, further be heated to 100 ℃, layering obtains xylene soluble part and dimethylbenzene insolubles, and the toluene in toluene solvend is steamed, and steaming excess quality is 340g, mix with oil after 80% distillation, filter with 200 object stainless (steel) wires again, after filtering, mix according to volume ratio 3:1 with diesel oil, obtain hydrogenation feed oil.Coal tar utilization ratio is 92.4%.Coal tar character before and after pre-treatment is in table 3.
Coal tar character (sample 3) before and after table 3 pre-treatment
Analysis project Before pre-treatment After pre-treatment
Density, kg/m 3 1025.5 898.8
Carbon residue, % 8.2 1.58
Ash content, % 0.091 0.054
Fe/Na,ppm 119.4 /33.8 7.5/8.1
Ni/V,ppm 1.2/1.1 <0.1/<0.1
Al/Cu,ppm 55.8/6.2 12.4/1.6
Ca/Mg,ppm 85.4/7.3 0.9/<0.1
K/Pb,ppm 7.6/<0.1 3.4/<0.1
Sulphur content, % 0.20 0.076
Nitrogen content, % 0.68 0.331
Open flash point, ℃ 115 87
Bituminous matter, % 16.24 3.27
Colloid, % 19.86 4.72
Fragrance part, % 30.21 13.85
Saturated part, % 11.95 18.42
Moisture, % 1.83 0.027
Mechanical impurity, % 3.695 0.627
Acid number, mgKOH/g 8.20 0.95
Condensation point, ℃ 22 5
Embodiment 4
Get 4157g coal tar, be heated to 80 ℃, with 100 object stainless (steel) wires filtrations, in the oil after filtration, add 3ml phenol amine aldehyde resin polyoxyethylene polyoxypropylene ether and 300ml water, keep Heating temperature, after stirring 3h, leave standstill 5h, separate water outlet 365g; Coal tar after dewatering is distilled, to distill remaining 20% heavy constituent 818g and 1054g toluene by volume 1:1.8 mix, further be heated to 100 ℃, layering obtains toluene solvend and toluene insolubles, and the toluene in toluene solvend is steamed, and steaming excess quality is 572g, mix with oil after 80% distillation, filter with 200 object stainless (steel) wires again, after filtering, mix according to volume ratio 3:1 with diesel oil, obtain hydrogenation feed oil.Coal tar utilization ratio is 92.5%.Coal tar character before and after pre-treatment is in table 4.
Coal tar character (sample 4) before and after table 4 pre-treatment
Analysis project Before pre-treatment After pre-treatment
Density, kg/m 3 1033.1 925.7
Carbon residue, % 8.2 0.84
Ash content, % 0.134 0.088
Fe/Na,ppm 117.5/36.1 4.4/6.4
Ni/V,ppm 0.4/1.1 <0.1/<0.1
Al/Cu,ppm 27.5<3.9 1.2/<0.1
Ca/Mg,ppm 83.4/17.6 2.7/0.3
K/Pb,ppm 1.5/<0.1 <0.1/<0.1
Sulphur content, % 0.19 0.064
Nitrogen content, % 1.07 0.527
Open flash point, ℃ 124 90
Bituminous matter, % 17.35 4.28
Colloid, % 21.35 5.27
Fragrance part, % 22.37 13.95
Saturated part, % 12.75 20.80
Moisture, % 2.15 0.097
Mechanical impurity, % 1.955 0.425
Acid number, mgKOH/g 9.24 1.25
Condensation point, ℃ 22 6
Can find out from above several embodiment, after the method for the invention is carried out pre-treatment, the indices value of coal tar is all greatly improved, and can directly enter hydrogenation unit.
Embodiment 5
A kind of coal tar hydrogenating pretreatment process, carries out according to following steps:
The first step, dewaters
Original coal tar is heated to 75 ℃ with 100 object strainer filterings, then in the coal tar after filtration, add polyethers emulsion splitter and water, the ratio of original coal tar, polyethers emulsion splitter and water is 700 (g): 1 (mL): 50 (mL), keep Heating temperature, stir after 0.5 hour and leave standstill 3 hours Separation of Waters, obtain the coal tar that dewaters;
Second step, distillation
Will described in the coal tar distillation that dewaters, the light oil that obtains steaming and the heavy oil not steaming, the heavy oil not steaming by weight percentage accounts for 20% of the coal tar that dewaters;
The 3rd step, extraction
To in described heavy oil, add benzene to mix, the volume ratio of heavy oil and benzene be 1:1.2, is then warming up to 120 ℃, isolate benzene solvend and benzene insoluble, after then the benzene in benzene solvend being steamed, mix with described light oil, finally use 200 object strainer filterings, obtain pre-treatment coal tar; Pre-treatment coal tar is used as hydrogenation feed oil after mixing according to volume ratio 3:1 with diesel oil.
Embodiment 6
A kind of coal tar hydrogenating pretreatment process, carries out according to following steps:
The first step, dewaters
Original coal tar is heated to 85 ℃ with 100 object strainer filterings, then in the coal tar after filtration, add polyethers emulsion splitter and water, the ratio of original coal tar, polyethers emulsion splitter and water is 1450 (g): 1 (mL): 100 (mL), keep Heating temperature, stir after 3 hours and leave standstill 5.5 hours Separation of Waters, obtain the coal tar that dewaters;
Second step, distillation
Will described in the coal tar distillation that dewaters, the light oil that obtains steaming and the heavy oil not steaming, the heavy oil not steaming by weight percentage accounts for 20% of the coal tar that dewaters;
The 3rd step, extraction
To in described heavy oil, add toluene to mix, the volume ratio of heavy oil and toluene is 1:1.8, then be warming up to 110 ℃, isolate toluene solvend and toluene insolubles, then after the toluene in toluene solvend being steamed, mix with described light oil, finally use 200 object strainer filterings, obtain pre-treatment coal tar; Pre-treatment coal tar is used as hydrogenation feed oil after mixing according to volume ratio 3:1 with diesel oil.
Embodiment 7
A kind of coal tar hydrogenating pretreatment process, carries out according to following steps:
The first step, dewaters
Original coal tar is heated to 82 ℃ with 100 object strainer filterings, then in the coal tar after filtration, add polyethers emulsion splitter and water, the ratio of original coal tar, polyethers emulsion splitter and water is 1000 (g): 1 (mL): 75 (mL), keep Heating temperature, stir after 2.5 hours and leave standstill 4 hours Separation of Waters, obtain the coal tar that dewaters;
Second step, distillation
Will described in the coal tar distillation that dewaters, the light oil that obtains steaming and the heavy oil not steaming, the heavy oil not steaming by weight percentage accounts for 20% of the coal tar that dewaters;
The 3rd step, extraction
To in described heavy oil, add dimethylbenzene to mix, the volume ratio of heavy oil and dimethylbenzene is 1:1.5, then be warming up to 115 ℃, separating dimethyl benzene solvend and dimethylbenzene insolubles, then after the dimethylbenzene in xylene soluble part being steamed, mix with described light oil, finally use 200 object strainer filterings, obtain pre-treatment coal tar; Pre-treatment coal tar is used as hydrogenation feed oil after mixing according to volume ratio 3:1 with diesel oil.
Embodiment 8
A kind of coal tar hydrogenating pretreatment process, carries out according to following steps:
The first step, dewaters
Original coal tar is heated to 82 ℃ with 100 object strainer filterings, then in the coal tar after filtration, add polyethers emulsion splitter and water, the ratio of original coal tar, polyethers emulsion splitter and water is 1000 (g): 1 (mL): 75 (mL), keep Heating temperature, stir after 2.5 hours and leave standstill 4 hours Separation of Waters, obtain the coal tar that dewaters;
Second step, distillation
Will described in the coal tar distillation that dewaters, the light oil that obtains steaming and the heavy oil not steaming, the heavy oil not steaming by weight percentage accounts for 20% of the coal tar that dewaters;
The 3rd step, extraction
To in described heavy oil, add high boiling aromatic hydrocarbon solvent oil to mix, the volume ratio of heavy oil and high boiling aromatic hydrocarbon solvent oil is 1:1.5, then be warming up to 115 ℃, isolate high boiling aromatic hydrocarbon solvent oil solvend and high boiling aromatic hydrocarbon solvent oil insolubles, then after the high boiling aromatic hydrocarbon solvent oil in high boiling aromatic hydrocarbon solvent oil solvend being steamed, mix with described light oil, finally use 200 object strainer filterings, obtain pre-treatment coal tar; Pre-treatment coal tar is used as hydrogenation feed oil after mixing according to volume ratio 3:1 with diesel oil.
The present invention can summarize with other the specific form without prejudice to spirit of the present invention or principal character.Therefore, no matter from that, above-mentioned embodiment of the present invention all can only think explanation of the present invention can not limit invention, claims have been pointed out scope of the present invention, and scope of the present invention is not pointed out in above-mentioned explanation, therefore, any variation in implication and the scope suitable with claims of the present invention, all should think to be included in the scope of claims.

Claims (7)

1. a coal tar hydrogenating pretreatment process, is characterized in that carrying out according to following steps:
The first step, dewaters
Original coal tar is heated to 70-90 ℃ with 100 object strainer filterings, then in the coal tar after filtration, adds emulsion splitter and water, keep Heating temperature, standing separation water after stirring, obtains the coal tar that dewaters; The ratio of described original coal tar, emulsion splitter and water is 700-1450 (g): 1 (mL): 50-100 (mL); Described emulsion splitter is polyethers emulsion splitter;
Second step, distillation
Will described in the coal tar distillation that dewaters, the light oil that obtains steaming and the heavy oil not steaming, the heavy oil not steaming by weight percentage accounts for 20% of the coal tar that dewaters;
The 3rd step, extraction
To in described heavy oil, add extraction agent to mix, be then warming up to 100-120 ℃, isolate extraction agent solvend and extraction agent insolubles, then after the extraction agent in extraction agent solvend being steamed, mix with described light oil, finally use 200 object strainer filterings, obtain pre-treatment coal tar.
2. a kind of coal tar hydrogenating pretreatment process according to claim 1, is characterized in that described polyethers emulsion splitter is phenol amine aldehyde resin polyoxyethylene polyoxypropylene ether.
3. a kind of coal tar hydrogenating pretreatment process according to claim 1, it is characterized in that the described the first step dewater middle stirring after 0.5-3 hour leave standstill 3-5.5 hour Separation of Water.
4. a kind of coal tar hydrogenating pretreatment process according to claim 1, is characterized in that described in the 3rd step extraction, extraction agent is aromatic solvent.
5. a kind of coal tar hydrogenating pretreatment process according to claim 4, is characterized in that described aromatic solvent is one or more in benzene,toluene,xylene and high boiling aromatic hydrocarbon solvent oil.
6. a kind of coal tar hydrogenating pretreatment process according to claim 1, is characterized in that the volume ratio of heavy oil described in the 3rd step extraction and extraction agent is 1:1.2-1.8.
7. a kind of coal tar hydrogenating pretreatment process according to claim 1, is characterized in that being used as hydrogenation feed oil after described pre-treatment coal tar mixes according to volume ratio 3:1 with diesel oil.
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CN103666540B (en) * 2013-11-29 2015-09-09 陕西延长石油(集团)有限责任公司研究院 Middle coalite tar dewatering agent and application
CN103695036B (en) * 2013-12-31 2015-10-28 上海新佑能源科技有限公司 Middle coalite tar processing and treating method
CN105154122B (en) * 2015-07-14 2018-01-05 陕西双翼石油化工有限责任公司 A kind of method of combined type coal tar dehydration
CN107099327A (en) * 2017-06-27 2017-08-29 上海蓝科石化环保科技股份有限公司 A kind of biomass coke tar pretreatment purification method and system

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