CN105085142A - Production method for high-purity n-hexane - Google Patents
Production method for high-purity n-hexane Download PDFInfo
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Abstract
The invention discloses a production method for high-purity n-hexane. According to the method, a raw material (8) is rectified and separated in an isohexane removal tower (1), so a tower bottom component (7) of the isohexane removal tower (1) is obtained; the tower bottom component (7) of the isohexane removal tower (1) enters an extracting and rectifying tower (2) and has countercurrent contact with a circulation solvent so as to realize extraction and rectification; a tower top product (9) of the extracting and rectifying tower (2) enters an n-hexane re-evaporation tower (5); a tower top component of the n-hexane re-evaporation tower (5) is high-purity n-hexane (14), and a tower bottom component (11) of the n-hexane re-evaporation tower (5) enters a solvent recovery tower (3); a tower bottom rich solvent (10) of the extracting and rectifying tower (2) enters the solvent recovery tower (3) for solvent recovery; and a tower bottom circulation solvent (13) of the solvent recovery tower (3) returns to the extracting and rectifying tower (2) for cyclic usage. The method has the advantages of high n-hexane purity and low energy consumption.
Description
Technical field
The present invention relates to the production method of a kind of high purity polymerization-grade normal hexane of petrochemical complex, namely be then separated through hydrogenation and removing impurity with straight run, oil field light hydrocarbon or reforming raffinate oil, the thick normal hexane obtaining normal hexane massfraction content 60% ~ 90% is raw material, have employed dioctyl phthalate (DOP) is that extraction solvent carries out extracting rectification, and through product purification, obtain the production method of high purity normal hexane.
Background technology
Normal hexane is one of varsol that industrial purposes is the widest, is the representational non-polar solvent of most.Normal hexane is as important industrial chemicals and solvent, the industries such as medicine, chemical industry, macromolecular material, rubber industry and food analysis are widely used in, normal hexane is mainly obtained by crack crude and fractionation, is then separated the thick normal hexane of acquisition at straight run, oil field light hydrocarbon or reforming raffinate oil through hydrogenation and removing impurity.Owing to containing the component methylcyclopentane very close with normal hexane boiling point (68.7 DEG C) in raw material, the boiling point (71.8 DEG C) of methylcyclopentane, if with conventional distillation method, obtains highly purified normal hexane uneconomical, also unrealistic.
It is one of main method of preparing of high purity normal hexane that molecular sieve adsorption is separated, Zhao Yajuan, Cheng Yuan. preparation [J] chemical reagent of high-purity normal hexane, 1999,21 (1): 54-55. utilize 5A molecular sieve twin columns pressure-swing absorber to be separated normal hexane and its isomers, and normal hexane content can reach more than 99%.CN101148390A discloses pressure-variable adsorption and extracts high purity normal hexane technique, and its technical process is that multitower is heated pressure-variable adsorption flow process, and its concrete steps are as follows: 1) adsorption process; 2) all pressure drops, to bleed off pressure; 3) desorption process; 4) all voltage rises, pressurising.Separation can obtain the normal hexane of content at 95.0%-99.9% (wt).
CN1765857 discloses the extraction and rectification separation method of a kind of normal hexane and methylcyclopentane, the solvent dimethyl phthalate of primary industry hexane and extracting rectifying is added extractive distillation column with certain proportioning, after separation, tower top is high purity normal hexane, and tower reactor is solvent dimethyl phthalate+methylcyclopentane; Kettle material is sent into solvent regeneration tower and is carried out distillation procedure, overhead extraction is methylcyclopentane, the methylcyclopentane of overhead extraction thing is refining further obtains high-purity methyl pentamethylene, tower reactor solvent dimethyl phthalate is sent extractive distillation column back to and is recycled, methylcyclopentane in the recyclable raw material of this method, the rate of recovery more than 90%, and can obtain the high purity normal hexane of purity >=98%.But the thermal degradation temperature of dimethyl phthalate is at about 200 DEG C, and the method extracting rectifying tower reactor temperature 195-200 DEG C, solvent reclamation tower reactor temperature 215-225 DEG C, this technology does not possess the condition of suitability for industrialized production.
The mensuration of the normal hexanes such as Li Chunli-first class pentamethylene-N-Methyl pyrrolidone three-component system vapor-liquid equilibrium and simulation [J] petrochemical complex of extracting rectifying, 2011,40 (9): 959-962. adopt the Othmer vapour phase single loop equilibrium still improved, and determine the vapor-liquid equilibrium data of normal hexane-first class pentamethylene-N-Methyl pyrrolidone (NMP) three-component system at ambient pressure.Associate with the vapor-liquid equilibrium data of NRTL equation to normal hexane-first class pentamethylene-NMP three-component system, return and obtain NRTL equation model parameter.Analog result shows, employing NMP is extraction agent, and extracting rectifying normal hexane-first class pentamethylene, can obtain highly purified normal hexane.
N-Methyl pyrrolidone is colourless transparent oil liquid, micro-smell having amine, fusing point-24.4 DEG C, boiling point 203 DEG C, for normal hexane-methylcyclopentane, NMP has excellent selectivity and solvability, NMP stable chemical nature, under protection of inert gas, even if the stability of N-Methyl pyrrolidone is still fine more than 315 DEG C, if but produce and expose in atmosphere in storage process, easily there is oxidizing reaction; Under water and oxygen existent condition, more than 175 DEG C, NMP superoxide produces and decomposes, and even hydrolysis generates 4-methyl amido butyric acid, causes acid corrosion.
Dioctyl phthalate (DOP) (DOP) is colourless transparent oil liquid, has special odor, fusing point-55 DEG C, boiling point 386.9 DEG C, and for normal hexane-first class pentamethylene, DOP has excellent selectivity and solvability, and photo and thermal stability is good, lower volatility.
With the thick normal hexane of normal hexane massfraction content 60% ~ 90% for raw material, take dioctyl phthalate (DOP) as extraction solvent, adopt extracting rectification technique, produce the high purity polymerization-grade normal hexane that normal hexane content meets needed for high-end market at the normal hexane of more than 98.5% (wt) and through purification acquisition, realize suitability for industrialized production, there is certain realistic meaning.
Summary of the invention
The object of this invention is to provide a kind of production method of high purity normal hexane, the present invention is then separated through hydrogenation and removing impurity with straight run, oil field light hydrocarbon or reforming raffinate oil, the thick normal hexane obtaining normal hexane massfraction content 60% ~ 90% is raw material, dioctyl phthalate (DOP) (DOP) is adopted to carry out extracting rectification for extraction solvent, through product purification, normal hexane content is greater than 98.5% (weight).
A kind of production method of high purity normal hexane, raw material 8 obtains component 7 at the bottom of de-isohexane tower 1 tower through de-isohexane tower 1 rectifying separation, component 7 at the bottom of de-isohexane tower 1 tower enters extracting rectification tower 2 and carries out extracting rectification with reverse contact of circulating solvent, extracting rectification tower 2 overhead product 7 enters normal hexane and steams tower 5 again, it is high purity normal hexane 14 that normal hexane steams tower 5 tower top again, normal hexane steams component 11 at the bottom of tower 5 tower again and enters into solvent recovery tower 3, rich solvent 10 at the bottom of extracting rectification tower 2 tower enters solvent recovery tower 3 and carries out solvent recuperation, solvent recovery tower 3 tower circulating solvent 13 turns back to extracting rectification tower 2 and recycles.
Described raw material is the C containing 60% ~ 90% normal hexane
6cut, is at least the C6 cut of field condensate device by-product, reformed arene extracting C6 raffinates oil or to be rich in the C6 cut of normal hexane a kind of.
The number of theoretical plate 70 ~ 100 of described de-isohexane tower 1, working pressure (table) 0.05 ~ 0.1MPa, tower top temperature 77 ~ 87 DEG C, column bottom temperature 91 ~ 100 DEG C.
The number of theoretical plate 45 ~ 60 of described extracting rectification tower 2, working pressure (table)-0.055 ~-0.04MPa, tower top temperature 45 ~ 53 DEG C, column bottom temperature 95 ~ 105 DEG C; At the bottom of de-isohexane tower 1 tower, component 7 with the mass ratio of circulating solvent is: 1: 3 ~ 12.Preferably 3 ~ 5.
The number of theoretical plate 15 ~ 20 of described solvent recovery tower 3, working pressure (table) 0.05 ~ 0.055MPa, tower top temperature 85 ~ 89 DEG C, column bottom temperature 152 ~ 157 DEG C.
Described normal hexane steams the number of theoretical plate 25 ~ 30 of tower 5 again, working pressure (table) 0.05 ~ 0.055MPa, tower top temperature 79 ~ 81 DEG C, column bottom temperature 94 ~ 97 DEG C.
Described solvent is dioctyl phthalate (DOP), enters the middle part of extracting rectification tower 2.
Compared with prior art adsorption separating method, the production method of a kind of high purity normal hexane of the present invention, low to the requirement of equipment, quality product is more stable, and energy consumption is reasonable.
Compared with prior art rectifying, hydrogenation rectificating method, the production method of a kind of high purity normal hexane of the present invention, normal hexane product purity is high, and energy consumption is low.
Accompanying drawing explanation
Fig. 1 is a kind of high purity normal hexane production method schematic flow sheet
Wherein:
1. de-isohexane tower, 2. extracting rectification tower, 3. solvent recovery tower, 4. extracting rectification vacuum pump, 5. normal hexane steams tower again, 6. light constituent, 7. component at the bottom of de-isohexane tower 1 tower, 8. raw material, 9. extracting rectification tower 2 overhead product, 10. rich solvent, 11. normal hexanes steam component at the bottom of tower 5 tower again, 12. heavy constituents, 13. circulating solvents, 14. high purity normal hexanes.
Embodiment
Below in conjunction with accompanying drawing, the invention will be further described:
Then be separated through hydrogenation and removing impurity with straight run, oil field light hydrocarbon or reforming raffinate oil, the thick normal hexane obtaining normal hexane massfraction content 60% ~ 90% is raw material, through de-isohexane tower 1, carry out rectifying separation, overhead product is light constituent, the de-light thick normal hexane isohexane massfraction content obtained at the bottom of tower is less than 1%, and this tower operates under pressure-fired.De-light thick normal hexane enters extracting rectification tower 2 middle and lower part, circulating solvent (DOP) enters extracting rectification tower 2 middle and upper part, carry out extracting rectification operation, overhead product is the normal hexane that massfraction content is more than or equal to 98.5%, and this logistics enters normal hexane and steams tower again and to remove in normal hexane the impurity such as the dioctyl phthalate (DOP) of trace and obtain high purity normal hexane.Extracting rectification tower 2 tower base stream rich solvent enters bottom solvent recovery tower 3, carry out batch distillation operation, overhead product is heavy constituent, is circulating solvent at the bottom of tower, circulating solvent loops back extracting rectification tower 2 after taking turns doing de-isohexane tower reboiler thermal source and feed heater thermal source.
The number of theoretical plate 70 ~ 100 of de-isohexane tower 1, working pressure (table) 0.05 ~ 0.1MPa, tower top temperature 77 ~ 87 DEG C, column bottom temperature 91 ~ 100 DEG C; The weight key ingredient of this Deethanizer design is respectively trimethylpentane and normal hexane, and the above light constituent of bottom product isohexane (containing isohexane) massfraction content is less than 0.5%.
The number of theoretical plate 45 ~ 60 of extracting rectification tower 2, working pressure (table)-0.055 ~-0.04MPa, tower top temperature 45 ~ 53 DEG C, column bottom temperature 95 ~ 105 DEG C; The mass flux ratio of de-light thick normal hexane and dioctyl phthalate (DOP) is: 1: 3 ~ 12.Preferably 3 ~ 5.This tower is under the protection of rare gas element, and extracting rectification vacuum pump 4 vacuumizes.
The number of theoretical plate 15 ~ 20 of solvent recovery tower 3, working pressure (table) 0.05 ~ 0.055MPa, tower top temperature 85 ~ 89 DEG C, column bottom temperature 152 ~ 157 DEG C, carry out batch distillation operation, every still distillation time about 6 hours, every still operational cycle is about 8 hours.
Extracting rectification tower 2 overhead product massfraction content is more than or equal to the normal hexane of 98.5%, enter normal hexane and steam tower 5 again, normal hexane steams the number of theoretical plate 25 ~ 30 of tower 5 again, working pressure (table) 0.05 ~ 0.055MPa, tower top temperature 79 ~ 81 DEG C, column bottom temperature 94 ~ 97 DEG C.Tower top obtains high purity normal hexane, and bottom product is interrupted delivers to solvent recovery tower 3.
Embodiment 1
With reforming raffinate oil through hydrogenation and removing impurity, be separated after thick hexane for raw material, raw material composition in table 1.Through de-isohexane tower 1 rectifying separation, overhead components, the composition of component at the bottom of tower is in table 2, the number of theoretical plate 90 of de-isohexane tower 1, working pressure (table) 0.06MPa, tower top temperature 79 DEG C, column bottom temperature 95 DEG C, de-light thick normal hexane enters extracting rectification tower 2 middle and lower part, circulating solvent dioctyl phthalate (DOP) enters extracting rectification tower 2 middle and upper part, carry out extracting rectification operation, overhead product is normal hexane, bottom product is rich solvent, composition is in table 3, the number of theoretical plate 60 of extracting rectification tower 2, working pressure (table)-0.04MPa, tower top temperature 53 DEG C, column bottom temperature 105 DEG C, the mass flux ratio of de-light thick normal hexane and dioctyl phthalate (DOP) is: 1: 5.This tower is under the protection of rare gas element; extracting rectification vacuum pump 4 vacuumizes; rich solvent enters bottom solvent recovery tower 3, and through solvent recovery tower batch distillation, overhead product is heavy constituent; bottom product is circulating solvent; form in table 4, the number of theoretical plate 20 of solvent recovery tower 3, working pressure (table) 0.05MPa; tower top temperature 85 DEG C, column bottom temperature 153 DEG C.Carry out batch distillation operation, every still distillation time 6 hours, every still operational cycle is 8 hours, extracting rectification tower 2 overhead product, enters normal hexane and steams tower 5 again, normal hexane steams the number of theoretical plate 25 of tower 5 again, working pressure (table) 0.05MPa, tower top temperature 79 DEG C, column bottom temperature 94 DEG C, tower top obtains high purity normal hexane, and bottom product is interrupted delivers to solvent recovery tower 3.
The composition of the thick normal hexane raw material of table 1
| Media name | Mass percent, % |
| 2,2-dimethylbutane | 0.0362 |
| 2,3-dimethylbutane | 0.7164 |
| 2-methylpentane | 7.3949 |
| 3-methylpentane | 17.2701 |
| Normal hexane | 62.2865 |
| Methylcyclopentane | 9.9978 |
| 2,2-dimethylpentane | 1.0337 |
| 2,4-dimethylpentane | 0.7009 |
| Triptane | 0.0834 |
| Benzene | - |
| 3,3-dimethylpentane | 0.0238 |
| Hexanaphthene | 0.4501 |
| 2-methyl hexane | 0.0036 |
| 2,3-dimethylpentane | 0.0025 |
| Add up to | 100.00 |
Table 2 takes off the composition of isohexane column overhead and bottom product
| Media name | Overhead product mass percent, % | Bottom product mass percent, % |
| 2,2-dimethylbutane | 0.1128 | - |
| 2,3-dimethylbutane | 2.2329 | - |
| 2-methylpentane | 23.0489 | - |
| 3-methylpentane | 53.6751 | 0.0727 |
| Normal hexane | 19.6571 | 82.4244 |
| Methylcyclopentane | 1.2722 | 14.1197 |
| 2,2-dimethylpentane | 0.0004 | 1.5218 |
| 2,4-dimethylpentane | - | 1.0319 |
| Triptane | - | 0.1228 |
| Benzene | - | - |
| 3,3-dimethylpentane | - | 0.0350 |
| Hexanaphthene | - | 0.6626 |
| 2-methyl hexane | - | 0.0053 |
| 2,3-dimethylpentane | - | 0.0037 |
| Add up to | 100.00 | 100.00 |
The composition of table 3 extracting rectification column overhead and bottom product
| Media name | Overhead product mass percent, % | Bottom product mass percent, % |
| 2-methylpentane | 0.0001 | - |
| 3-methylpentane | 0.0877 | - |
| Normal hexane | 99.0000 | 0.0346 |
| Methylcyclopentane | 0.5728 | 1.0967 |
| 2,2-dimethylpentane | 0.3319 | 0.1002 |
| 2,4-dimethylpentane | 0.0029 | 0.0826 |
| Triptane | - | 0.0970 |
| Benzene | - | - |
| 3,3-dimethylpentane | - | 0.0028 |
| Hexanaphthene | - | 0.0534 |
| 2-methyl hexane | - | 0.0004 |
| 2,3-dimethylpentane | - | 0.0003 |
| Dioctyl phthalate (DOP) | - | 98.6192 |
| Add up to | 100.00 | 100.00 |
The composition of table 4 solvent recuperation column overhead and bottom product
| Media name | Overhead product mass percent, % | Bottom product mass percent, % |
| 3-methylpentane | - | - |
| Normal hexane | 2.5063 | - |
| Methylcyclopentane | 79.7459 | - |
| 2,2-dimethylpentane | 6.9561 | - |
| 2,4-dimethylpentane | 5.9821 | - |
| Triptane | 0.6968 | - |
| Benzene | - | - |
| 3,3-dimethylpentane | 0.2040 | - |
| Hexanaphthene | 3.8565 | - |
| 2-methyl hexane | 0.0309 | - |
| 2,3-dimethylpentane | 0.0214 | - |
| Dioctyl phthalate (DOP) | - | 100.00 |
| Add up to | 100.00 | 100.00 |
Embodiment 2
Then be separated through hydrogenation and removing impurity with reforming raffinate oil, the thick hexane of acquisition is raw material, and raw material composition is with embodiment 1.Through de-isohexane tower 1 rectifying separation, at the bottom of overhead components and tower, the composition of component is in table 5, de-isohexane tower 1 operational condition: number of theoretical plate 75, working pressure (table) 0.05MPa, tower top temperature 78 DEG C, column bottom temperature 92 DEG C, de-light thick normal hexane enters extracting rectification tower 2 middle and lower part, circulating solvent (DOP) enters extracting rectification tower 2 middle and upper part, carry out extracting rectification operation, overhead product is normal hexane, bottom product is rich solvent, composition is in table 6, the number of theoretical plate 55 of extracting rectification tower 2, working pressure (table)-0.05MPa, tower top temperature 48 DEG C, column bottom temperature 98 DEG C, the mass flux ratio of de-light thick normal hexane and dioctyl phthalate (DOP) is: 1: 4.This tower is under the protection of rare gas element; extracting rectification vacuum pump 4 vacuumizes; rich solvent enters in the middle part of solvent recovery tower 3, and through solvent recuperation column distillation, overhead product is heavy constituent; bottom product is circulating solvent; form in table 7, the number of theoretical plate 20 of solvent recovery tower 3, working pressure (table) 0.055MPa; tower top temperature 89 DEG C, column bottom temperature 157 DEG C.Carry out batch distillation operation, every still distillation time 6 hours, every still operational cycle is 8 hours.
Extracting rectification tower 2 overhead product, enters normal hexane and steams tower 5 again, and normal hexane steams the number of theoretical plate 30 of tower 5 again, working pressure (table) 0.055MPa, tower top temperature 81 DEG C, column bottom temperature 97 DEG C, tower top obtains high purity normal hexane, and bottom product is interrupted delivers to solvent recovery tower 3.
Table 5 takes off the composition of isohexane column overhead and bottom product
| Media name | Overhead product mass percent, % | Bottom product mass percent, % |
| 2,2-dimethylbutane | 0.1128 | - |
| 2,3-dimethylbutane | 2.2329 | - |
| 2-methylpentane | 23.0403 | 0.0041 |
| 3-methylpentane | 53.4743 | 0.4799 |
| Normal hexane | 20.4743 | 82.0384 |
| Methylcyclopentane | 1.3256 | 14.5218 |
| 2,2-dimethylpentane | 0.0005 | 1.5218 |
| 2,4-dimethylpentane | 0.0002 | 1.0319 |
| Triptane | - | 0.1228 |
| Benzene | - | - |
| 3,3-dimethylpentane | - | 0.0350 |
| Hexanaphthene | - | 0.6626 |
| 2-methyl hexane | - | 0.0053 |
| 2,3-dimethylpentane | - | 0.0037 |
| Add up to | 100.00 | 100.00 |
The composition of table 6 extracting rectification column overhead and bottom product
| Media name | Overhead product mass percent, % | Bottom product mass percent, % |
| 2-methylpentane | 0.0050 | - |
| 3-methylpentane | 0.5793 | - |
| Normal hexane | 98.9157 | 0.0102 |
| Methylcyclopentane | 0.4995 | 1.2199 |
| 2,2-dimethylpentane | 0.0005 | 0.1357 |
| 2,4-dimethylpentane | - | 0.0920 |
| Triptane | - | 0.0109 |
| Benzene | - | - |
| 3,3-dimethylpentane | - | 0.0031 |
| Hexanaphthene | - | 0.0591 |
| 2-methyl hexane | - | 0.0005 |
| 2,3-dimethylpentane | - | 0.0003 |
| Dioctyl phthalate (DOP) | - | 98.4683 |
| Add up to | 100.00 | 100.00 |
The composition of table 7 solvent recuperation column overhead and bottom product
| Media name | Overhead product mass percent, % | Bottom product mass percent, % |
| 3-methylpentane | - | - |
| Normal hexane | 0.5142 | - |
| Methylcyclopentane | 79.7951 | - |
| 2,2-dimethylpentane | 8.8558 | - |
| 2,4-dimethylpentane | 6.0073 | - |
| Triptane | 0.7148 | - |
| Benzene | - | - |
| 3,3-dimethylpentane | 0.2040 | - |
| Hexanaphthene | 3.8564 | - |
| 2-methyl hexane | 0.0309 | - |
| 2,3-dimethylpentane | 0.0214 | - |
| Dioctyl phthalate (DOP) | - | 100.00 |
| Add up to | - | 100.00 |
Embodiment 3
Then be separated through hydrogenation and removing impurity with reforming raffinate oil, the thick hexane of acquisition is raw material, and raw material composition is with embodiment 1.Through de-isohexane tower 1 rectifying separation, at the bottom of overhead components and tower, the composition of component is in table 8, de-isohexane tower 1 operational condition: number of theoretical plate 80, working pressure (table) 0.1MPa, tower top temperature 87 DEG C, column bottom temperature 100 DEG C, de-light thick normal hexane enters extracting rectification tower 2 middle and lower part, circulating solvent (DOP) enters extracting rectification tower 2 middle and upper part, carry out extracting rectification operation, overhead product is high purity normal hexane, bottom product is rich solvent, composition is in table 9, the number of theoretical plate 50 of extracting rectification tower 2, working pressure (table)-0.055MPa, tower top temperature 45 DEG C, column bottom temperature 95 DEG C, the mass flux ratio of de-light thick normal hexane and dioctyl phthalate (DOP) is: 1: 3.This tower is under the protection of rare gas element; extracting rectification vacuum pump 4 vacuumizes; rich solvent enters in the middle part of solvent recovery tower 3, and through solvent recuperation column distillation, overhead product is heavy constituent; bottom product is circulating solvent; form in table 10, the number of theoretical plate 20 of solvent recovery tower 3, working pressure (table) 0.05MPa; tower top temperature 85 DEG C, column bottom temperature 152 DEG C.Carry out batch distillation operation, every still distillation time 6 hours, every still operational cycle is 8 hours, extracting rectification tower 2 overhead product, enters normal hexane and steams tower 5 again, normal hexane steams the number of theoretical plate 28 of tower 5 again, working pressure (table) 0.05MPa, tower top temperature 80 DEG C, column bottom temperature 95 DEG C, tower top obtains high purity normal hexane, and bottom product is interrupted delivers to solvent recovery tower 3.
Table 9 takes off the composition of isohexane column overhead and bottom product
| Media name | Overhead product mass percent, % | Bottom product mass percent, % |
| 2,2-dimethylbutane | 0.1128 | - |
| 2,3-dimethylbutane | 2.2329 | - |
| 2-methylpentane | 23.0474 | 0.0008 |
| 3-methylpentane | 53.3200 | 0.2404 |
| Normal hexane | 20.0605 | 82.2338 |
| Methylcyclopentane | 1.2253 | 14.1419 |
| 2,2-dimethylpentane | 0.0005 | 1.5219 |
| 2,4-dimethylpentane | 0.0002 | 1.0319 |
| Triptane | - | 0.1228 |
| Benzene | - | - |
| 3,3-dimethylpentane | - | 0.035 |
| Hexanaphthene | - | 0.6626 |
| 2-methyl hexane | - | 0.0053 |
| 2,3-dimethylpentane | - | 0.0037 |
| Add up to | 100.00 | 100.00 |
The composition of table 9 extracting rectification column overhead and bottom product
| Media name | Overhead product mass percent, % | Bottom product mass percent, % |
| 2-methylpentane | 0.0009 | - |
| 3-methylpentane | 0.2903 | - |
| Normal hexane | 98.5000 | 0.0617 |
| Methylcyclopentane | 0.8080 | 1.2709 |
| 2,2-dimethylpentane | 0.3872 | 0.1133 |
| 2,4-dimethylpentane | 0.0079 | 0.0967 |
| Triptane | 0.0057 | 0.0111 |
| Benzene | - | - |
| 3,3-dimethylpentane | - | 0.0033 |
| Hexanaphthene | - | 0.0625 |
| 2-methyl hexane | - | 0.0005 |
| 2,3-dimethylpentane | - | 0.0003 |
| Dioctyl phthalate (DOP) | - | 98.3796 |
| Add up to | 100.00 | 100.00 |
The composition of table 10 solvent recuperation column overhead and bottom product
| Media name | Overhead product mass percent, % | Bottom product mass percent, % |
| 3-methylpentane | 0.0002 | - |
| Normal hexane | 3.8075 | - |
| Methylcyclopentane | 78.4310 | - |
| 2.2-dimethylpentane | 6.9921 | - |
| 2.4-dimethylpentane | 5.9692 | - |
| Triptane | 0.6874 | - |
| Benzene | - | - |
| 3,3-dimethylpentane | 0.2040 | - |
| Hexanaphthene | 3.8564 | - |
| 2-methyl hexane | 0.0309 | - |
| 2,3-dimethylpentane | 0.0214 | - |
| Dioctyl phthalate (DOP) | - | 100.00 |
| Add up to | 100.00 | 100.00 |
Claims (7)
1. the production method of a high purity normal hexane, (8 obtain component (7) at the bottom of de-isohexane tower (1) tower through de-isohexane tower (1) rectifying separation to raw material, component (7) at the bottom of de-isohexane tower (1) tower enters extracting rectification tower (2) and carries out extracting rectification with solvent contacts, extracting rectification tower (2) overhead product (7) enters normal hexane and steams tower (5) again, it is high purity normal hexane (14) that normal hexane steams tower (5) tower top again, normal hexane steams component (11) at the bottom of tower (5) tower again and enters into solvent recovery tower (3), rich solvent (10) at the bottom of extracting rectification tower (2) tower enters solvent recovery tower (3) and carries out solvent recuperation, solvent recovery tower (3) tower circulating solvent (13) turns back to extracting rectification tower (2) and recycles.
2. according to the production method of a kind of high purity normal hexane according to claim 1, it is characterized in that: described raw material is the C containing 60% ~ 90% normal hexane
6cut, is at least the C of field condensate device by-product
6cut, reformed arene extracting C
6raffinate oil or be rich in the C of normal hexane
6cut is a kind of.
3. according to the production method of a kind of high purity normal hexane according to claim 1, it is characterized in that: the number of theoretical plate 70 ~ 100 of described de-isohexane tower (1), working pressure 0.05 ~ 0.1MPa, tower top temperature 77 ~ 87 DEG C, column bottom temperature 91 ~ 100 DEG C.
4. according to the production method of a kind of high purity normal hexane according to claim 1, it is characterized in that: the number of theoretical plate 45 ~ 60 of described extracting rectification tower (2), working pressure-0.055 ~-0.04MPa, tower top temperature 45 ~ 53 DEG C, column bottom temperature 95 ~ 105 DEG C; At the bottom of de-isohexane tower 1 tower, component 7 with the mass ratio of circulating solvent is: 1: 3 ~ 12, preferably 3 ~ 5.
5. according to the production method of a kind of high purity normal hexane according to claim 1, it is characterized in that: the number of theoretical plate 15 ~ 20 of described solvent recovery tower (3), working pressure 0.05 ~ 0.055MPa, tower top temperature 85 ~ 89 DEG C, column bottom temperature 152 ~ 157 DEG C.
6. according to the production method of a kind of high purity normal hexane according to claim 1, it is characterized in that: described normal hexane steams the number of theoretical plate 25 ~ 30 of tower (5) again, working pressure 0.05 ~ 0.055MPa, tower top temperature 79 ~ 81 DEG C, column bottom temperature 94 ~ 97 DEG C.
7., according to the production method of a kind of high purity normal hexane according to claim 1, it is characterized in that: described solvent is dioctyl phthalate (DOP), enter the middle part of extracting rectification tower (2).
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| CN107759471B (en) * | 2017-12-05 | 2023-08-11 | 郑州大学 | Separation and purification device and process for preparing cyclohexane plasticizer product by liquid phase hydrogenation of o-benzene plasticizer |
| CN110229042A (en) * | 2019-06-20 | 2019-09-13 | 山东京博石油化工有限公司 | A kind of preparation method of high-purity n-hexane |
| CN110256190A (en) * | 2019-06-20 | 2019-09-20 | 山东京博石油化工有限公司 | A kind of production method of food-grade n-hexane |
| CN110229042B (en) * | 2019-06-20 | 2022-03-04 | 山东京博石油化工有限公司 | Preparation method of high-purity n-hexane |
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