CN101538185A - Method for extracting mesitylene fraction rich in hydrocracking C 9 by combination of continuous lateral line distillation and extractive distillation - Google Patents
Method for extracting mesitylene fraction rich in hydrocracking C 9 by combination of continuous lateral line distillation and extractive distillation Download PDFInfo
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Abstract
The invention discloses a method for extracting mesitylene fractions rich in hydrocracking C 9 by combination of continuous lateral line distillation and extractive distillation, comprising the following steps: (1) material hydrocracking C 9 aromatic is added into a continuous lateral line distillation tower, the tower bottom is heated, fractions 2 with a boiling range of 155 DEG C to 170 DEG C, fractions 3 with a boiling range of 170 DEG C to 190 DEG C and fractions 4 with a boiling range of 190 DEG C to 210 DEG C are obtained at the same time after pretreatment, content of mesitylene in the fractions 2 achieves above 90 percent, and a little mesitylene and a great deal of heavy aromatic are contained in the fractions 3 and the fractions 4; (2) the fractions 2 enter an extractive distillation tower, content of mesitylene fractions on the top 5 of the extractive distillation tower achieves above 98 percent, and fractions 6 containing a great deal of extraction solvent and heavy aromatic hydrocarbon are left at the tower bottom; (3) the fractions 6 are treated through a solvent recovery tower, heavy aromatic fractions 7 are left on the top of the solvent recovery tower, a tower reactor extracts solvent, and the solvent flows into the extractive distillation tower for recycling use. The invention only needs one distillation tower, obviously improves the efficiency, and lowers the energy consumption and the cost.
Description
Technical field
The present invention relates to a kind of chemical separating method, particularly a kind of continuous lateral line rectifying and extracting rectifying are in conjunction with extracting hydrocracking C
9In be rich in the method for trimethylbenzene cut.
Background technology
Cracking C
9Aromatic hydrocarbons is the by product of ethylene unit, accounts for 10～20% of ethene ultimate production.At present, China's cracking C
9The output of aromatic hydrocarbons is 1.06 * 10
6More than the t/a, will reach 1.1 * 10 in 2010
6More than the t/a.Cracking C
9Aromatic hydrocarbons form extremely complexity, and color is dark, peculiar smell is big along with cracking stock, cracking severity and cracking technology is different and different.By method of hydrotreating it is made with extra care, can improve its quality, it is effectively utilized.At present, hydrocracking C
9Aromatic hydrocarbons mainly contains the application of the following aspects: hydrocracking C
9Aromatic hydrocarbons is produced petroleum resin; Hydrocracking C
9Aromatic hydrocarbons prepares the lightweight cracking stock; Hydrocracking C
9Aromatic hydrocarbons is done the gasoline blend component; Hydrocracking C
9Aromatic hydrocarbons is used to produce Mixed XYLENE; Hydrocracking C
9Arene light formation volume increase BTX aromatic hydrocarbons.As seen, hydrocracking C
9The emphasis of aromatic hydrocarbons comprehensive utilization having become petrochemical enterprise deep processing will produce huge economic benefit and environmental benefit, will produce far-reaching influence to the improvement and the development of ethylene production technology.
Traditional trimethylbenzene production, isolating method mainly contain cryogenic crystallization method, extraction extracting/isomerization method, transalkylation and extraction fractional distillation.The cryogenic crystallization method is to utilize molten difference of aromatic hydrocarbons and carry out isolating method, and low temperature is operation down, and investment is big, energy consumption is high, and economic target is poor; Extraction extracting/isomerization method is to utilize the difference of each component relative basicity in the aromatic hydrocarbons to carry out isolating method, and successfully separation and purification goes out trimethylbenzene from the heavy aromatics of xylene isomerization by-product, but organic reaction is very complicated, also have side reactions such as disproportionation and alkylation in isomerization reaction, by product is more; Transalkylation is to carry out alkylated reaction with benzene under the effect of heterogeneous acid catalyst, and first and second benzene can selectively be converted into light constituents such as toluene or ethylbenzene, and light constituent can easily be separated with rectification method from trimethylbenzene, wherein difficult coupling of catalyzer; Extraction fractional distillation mainly is to increase relative volatility between each component by extraction solvent, thereby reaches isolating purpose, and the selection of extraction solvent is crucial in this method.
Summary of the invention
At the deficiency on the prior art, the purpose of this invention is to provide a kind of continuous lateral line rectifying and extracting rectifying in conjunction with extracting hydrocracking C
9Be rich in the method for trimethylbenzene cut in the aromatic hydrocarbons.Technology of the present invention mainly contains: the one, and the method pre-treatment hydrocracking C of employing continuous lateral line rectifying
9Aromatic hydrocarbons, traditional technology need two rectifying tower just can finish this task, and present method only needs a rectifying tower can reach target, and can obtain the cut of a plurality of boiling ranges; The 2nd, adopt the method for extracting rectifying to extract the highly purified cut that is rich in trimethylbenzene, use the compound extracting solvent of dibutyl phthalate-aniline in this process first, separation efficiency obviously improves; The 3rd, the extraction solvent recovery tower reclaims solvent cycle and uses.This method is simple, and the separation efficiency height cuts down the consumption of energy in the production process greatly, saves production cost the having a high potential of suitability for industrialized production.
The scheme of finishing the foregoing invention task is: a kind of continuous lateral line rectifying and extracting rectifying are in conjunction with extracting hydrocracking C
9In be rich in the method for trimethylbenzene cut, step is as follows:
(1). raw material hydrocracking C
9Aromatic hydrocarbons adds the continuous lateral line rectifying tower, heating at the bottom of the tower, through pre-treatment, obtain boiling range simultaneously and be 155 ℃～170 ℃ cut 2., boiling range be 170 ℃～190 ℃ cut 3. with boiling range be 190 ℃～210 ℃ cut 4.; Wherein, cut 2. in the content of trimethylbenzene be more than 90%, cut is 3., contain a spot of trimethylbenzene and a large amount of heavy aromaticss in 4.;
(2). 2. cut enters extractive distillation column, and the content that 5. the extracting rectifying column overhead obtains the trimethylbenzene cut is more than 98%, at the bottom of the tower be contain a large amount of extraction solvents and heavy aromatics cut 6.;
(3). 6. cut is handled through the solvent solvent recovery tower, and 7. the solvent recuperation column overhead attaches most importance to aromatic fraction, and the tower still is that extraction solvent flows into extractive distillation column again, recycles.
Above scheme, the extraction solvent in described (2) step is the compound extracting solvent of dibutyl phthalate and aniline, the volume ratio of dibutyl phthalate and aniline is 1: 0.8～1.2; The volume ratio of this compound extracting solvent and extractive distillation column raw material inlet amount is 1: 0.8～1.2.
The application recommends: the optimum volume ratio of dibutyl phthalate and aniline is 1: 1; The optimum volume ratio of this compound extracting solvent and extractive distillation column raw material inlet amount is 1: 1.
(1). raw material hydrocracking C
9Aromatic hydrocarbons adds the continuous lateral line rectifying tower, heat by voltate regulator controlling resistance silk at the bottom of the tower, through the pre-treatment of continuous lateral line rectifying tower, can obtain boiling range simultaneously and be 155 ℃～170 ℃ cut 2., boiling range be 170 ℃～190 ℃ cut 3. with boiling range be 190 ℃～210 ℃ cut 4., the cut 2. content of trimethylbenzene cut is more than 90%, and 3., 4. cut contains a spot of trimethylbenzene cut and a large amount of heavy aromaticss.
(2). 2. the overhead fraction of continuous lateral line rectifying tower enters extractive distillation column, and the content that 5. the extracting rectifying column overhead obtains the trimethylbenzene cut is more than 98%, at the bottom of the tower be contain a large amount of extraction solvents and heavy aromatics cut 6..
(3). 6. the cut that contains a large amount of extraction solvents and heavy aromatics is handled through solvent recovery tower, and 7. the solvent recuperation column overhead attaches most importance to aromatic fraction, and the tower still is that extraction solvent flows into extractive distillation column again, recycles.
Say that more specifically and more optimally operation steps of the present invention is:
(1). raw material hydrocracking C
9Aromatic hydrocarbons adds the continuous lateral line rectifying tower, and the tower still heats by voltate regulator controlling resistance silk: the control inlet amount is 2ml/min, load D
2, D
3And D
4Be respectively 0.5ml/min, 0.5ml/min and 1.0ml/min, tower top temperature is at 162.5～163.5 ℃, tower still temperature is at 200～202 ℃, reflux ratio 3～4, theoretical plate number is 45, feed entrance point is at the 25th column plate place, through the pre-treatment of continuous lateral line rectifying tower, can obtain boiling range simultaneously and be 155 ℃～170 ℃ cut 2., boiling range be 170 ℃～190 ℃ cut 3. with boiling range be 190 ℃～210 ℃ cut 4., the overhead fraction 2. content of trimethylbenzene cut is 90.8789%, and 3., 4. cut contains a spot of trimethylbenzene cut and a large amount of heavy aromaticss;
(2). 2. the overhead fraction of continuous lateral line rectifying tower enters extractive distillation column, and inlet amount is 2ml/min, load D
5And D
6Be respectively 1.7ml/min, 0.6ml/min, the control tower top temperature is at 161～162 ℃, tower still temperature is at 205～208 ℃, reflux ratio is 3～4, theoretical plate number is 40, and cat head is rich in trimethylbenzene cut feed entrance point at the 25th block of plate, and the extraction solvent feed entrance point is at the 5th block of plate, the content that 5. the extracting rectifying column overhead obtains the trimethylbenzene cut is 98.6332%, the tower still be contain a large amount of extraction solvents and heavy aromatics cut 6..
Described extraction solvent is the compound extracting solvent of dibutyl phthalate and aniline, and both volume ratios are 1: 1; The optimum volume ratio of this compound extracting solvent and extractive distillation column raw material inlet amount is 1: 1.
(3). 6. the above-mentioned cut that contains a large amount of extraction solvents and heavy aromatics is handled through solvent recovery tower, and the control inlet amount is 2ml/min, load D
7And D
8Be respectively 0.5ml/min, 1.5ml/min, tower top temperature is at 168～170 ℃, and tower still temperature is at 230～235 ℃, feed entrance point is at the 15th block of plate, and reflux ratio is 1～2, and 7. the solvent recuperation column overhead attaches most importance to aromatic fraction, the tower still is that extraction solvent flows into extractive distillation column again, recycles.
The processing condition of table 1 sepn process
| Processing parameter | The continuous lateral line rectifying tower | Extractive distillation column | Solvent recovery tower |
| Inlet amount (ml/min) | 2 | 2 | 2 |
| Load (ml/min) | D 2＝0.5 D 3＝0.5 D 4＝1.0 | D 5＝1.7 D 6＝0.3 | D 7＝0.5 D 8＝1.5 |
| Tower top temperature (℃) | 162.5～163.5 | 161～162 | 168～170 |
| Column bottom temperature (℃) | 200～202 | 205～208 | 230～235 |
| Reflux ratio (R) | 3～4 | 3～4 | 1～2 |
| Theoretical plate number (N) | 45 | 40 | 20 |
| Raw material feed entrance point (N) | 25 | 25 | 15 |
| Extractant feed position (N) | / | 5 | / |
The composition and the content of each cut of table 2 sepn process
| The |
① | ② | ③ | ④ | ⑤ | ⑥ | ⑦ |
| 1.C 8Component | 0.5495 | 4.0943 | / | / | 2.7977 | 1.1572 | 1.3683 |
| 2. propyl benzene | 4.9763 | 16.5573 | / | / | 15.2293 | 9.1298 | 10.0021 |
| 3. a p-methyl-ethylbenzene | 13.4975 | 32.4526 | / | / | 49.0996 | 19.7367 | 20.8386 |
| 4. sym-trimethylbenzene | 1.6272 | 1.7988 | / | / | 6.8950 | 3.5635 | 3.8542 |
| 5. o-methylethylbenzene | 3.6187 | 11.9264 | / | / | 14.8165 | 7.7639 | 8.0213 |
| 6. unsym-trimethyl benzene | 2.9694 | 9.9833 | / | / | 9.6000 | 8.9794 | 9.0034 |
| 7. hemimellitene | 3.0119 | 2.0662 | 3.2304 | / | 0.1952 | 6.1359 | 5.8233 |
| 8. indane | 2.4900 | 4.7604 | 1.8209 | / | 1.3668 | 12.9579 | 11.3789 |
| 9. dicyclo pentane | 51.1952 | 4.3620 | 80.4996 | 61.7300 | / | 30.5758 | 29.7099 |
| 10. other the unknowns | 16.0643 | / | 14.4491 | 38.2700 | / | / | / |
Compare with traditional technology, the present invention changes conventional distillation into continuous lateral line rectifying, only needs a rectifying tower can reach target, hydrocracking C
9Aromatic hydrocarbons is after pre-treatment, and the content that is rich in the trimethylbenzene cut brings up to 90.8789%, and yield is 76.4948%, and can to obtain content be 80.4996% dicyclo pentane cut; Adopt the compound extracting solvent in extracting rectifying, obviously improved separation efficiency, the content that is rich in the trimethylbenzene cut brings up to 98.6332%, and yield is 92.6435%.This process not only technology is simple, separation efficiency height, and the energy consumption of sepn process reduces greatly, saves production cost, the having a high potential of suitability for industrialized production.
Description of drawings
Fig. 1 extracts the process flow sheet that is rich in the trimethylbenzene cut for continuous lateral line rectifying and extracting rectifying combine;
Fig. 2 is hydrocracking C
9The aroamtic hydrocarbon raw material analysis of spectra;
Fig. 3 is a continuous lateral line rectifying tower overhead fraction analysis of spectra;
Fig. 4 is an extractive distillation column overhead fraction analysis of spectra.
Embodiment
Claims (5)
1, a kind of continuous lateral line rectifying and extracting rectifying are in conjunction with extracting hydrocracking C
9In be rich in the method for trimethylbenzene cut, step is as follows:
(1). raw material hydrocracking C
9Aromatic hydrocarbons adds the continuous lateral line rectifying tower, heating at the bottom of the tower, through pre-treatment, obtain boiling range simultaneously and be 155 ℃～170 ℃ cut 2., boiling range be 170 ℃～190 ℃ cut 3. with boiling range be 190 ℃～210 ℃ cut 4.; Wherein, cut 2. in the content of trimethylbenzene be more than 90%, cut is 3., contain a spot of trimethylbenzene and a large amount of heavy aromaticss in 4.;
(2). 2. cut enters extractive distillation column, and the content that 5. the extracting rectifying column overhead obtains the trimethylbenzene cut is more than 98%, at the bottom of the tower be contain a large amount of extraction solvents and heavy aromatics cut 6.;
(3). 6. cut is handled through the solvent solvent recovery tower, and 7. the solvent recuperation column overhead attaches most importance to aromatic fraction, and the tower still is that extraction solvent flows into extractive distillation column again, recycles.
2, continuous lateral line rectifying according to claim 1 and extracting rectifying are in conjunction with extracting hydrocracking C
9In be rich in the method for trimethylbenzene cut, it is characterized in that,
Extraction solvent in described (2) step is the compound extracting solvent of dibutyl phthalate and aniline, and the volume ratio of dibutyl phthalate and aniline is 1: 0.8～1.2; The volume ratio of this compound extracting solvent and extractive distillation column raw material inlet amount is 1: 0.8～1.2.
3, continuous lateral line rectifying according to claim 2 and extracting rectifying are in conjunction with extracting hydrocracking C
9In be rich in the method for trimethylbenzene cut, it is characterized in that the volume ratio of dibutyl phthalate and aniline is 1: 1; The volume ratio of described compound extracting solvent and extractive distillation column raw material inlet amount is 1: 1.
4, according to claim 1 or 2 or 3 described continuous lateral line rectifying and extracting rectifying in conjunction with extracting hydrocracking C
9In be rich in the method for trimethylbenzene cut, it is characterized in that the concrete operations step is:
(1). raw material hydrocracking C
9Aromatic hydrocarbons adds the continuous lateral line rectifying tower, and the tower still heats by voltate regulator controlling resistance silk: the control inlet amount is 2ml/min, load D
2, D
3And D
4Be respectively 0.5ml/min, 0.5ml/min and 1.0ml/min, tower top temperature is at 162.5～163.5 ℃, tower still temperature is at 200～202 ℃, reflux ratio 3～4, theoretical plate number is 45, feed entrance point is at the 25th column plate place, through the pre-treatment of continuous lateral line rectifying tower, obtain boiling range simultaneously and be 155 ℃～170 ℃ cut 2., boiling range be 170 ℃～190 ℃ cut 3. with boiling range be 190 ℃～210 ℃ cut 4., the overhead fraction 2. content of trimethylbenzene cut is 90.8789%, and 3., 4. cut contains a spot of trimethylbenzene cut and a large amount of heavy aromaticss;
(2). 2. the overhead fraction of continuous lateral line rectifying tower enters extractive distillation column, and inlet amount is 2ml/min, load D
5And D
6Be respectively 1.7ml/min, 0.6ml/min, the control tower top temperature is at 161～162 ℃, tower still temperature is at 205～208 ℃, reflux ratio is 3～4, theoretical plate number is 40, and cat head is rich in trimethylbenzene cut feed entrance point at the 25th block of plate, and the extraction solvent feed entrance point is at the 5th block of plate, the content that 5. the extracting rectifying column overhead obtains the trimethylbenzene cut is 98.6332%, the tower still be contain a large amount of extraction solvents and heavy aromatics cut 6.;
(3). 6. the above-mentioned cut that contains a large amount of extraction solvents and heavy aromatics is handled through solvent recovery tower, and the control inlet amount is 2ml/min, load D
7And D
8Be respectively 0.5ml/min, 1.5ml/min, tower top temperature is at 168～170 ℃, and tower still temperature is at 230～235 ℃, feed entrance point is at the 15th block of plate, and reflux ratio is 1～2, and 7. the solvent recuperation column overhead attaches most importance to aromatic fraction, the tower still is that extraction solvent flows into extractive distillation column again, recycles.
5, continuous lateral line rectifying according to claim 4 and extracting rectifying are in conjunction with extracting hydrocracking C
9In be rich in the method for trimethylbenzene cut, it is characterized in that the composition of described processing condition and each cut and content such as following two tables:
The processing condition of table 1 sepn process
The composition and the content of each cut of table 2 sepn process
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Application publication date: 20090923 |