CN101734998A - Method for extracting trimethylbenzene fraction in hydrocracking C9 by combined solvent extraction rectification method - Google Patents

Method for extracting trimethylbenzene fraction in hydrocracking C9 by combined solvent extraction rectification method Download PDF

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CN101734998A
CN101734998A CN200910264447A CN200910264447A CN101734998A CN 101734998 A CN101734998 A CN 101734998A CN 200910264447 A CN200910264447 A CN 200910264447A CN 200910264447 A CN200910264447 A CN 200910264447A CN 101734998 A CN101734998 A CN 101734998A
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solvent
tower
cut
extraction
hydrocracking
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顾正桂
林军
刘俊华
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Nanjing Normal University
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Nanjing Normal University
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Abstract

The invention relates to a method for extracting trimethylbenzene fraction in hydrocracking C9 by a combined solvent extraction rectification method, comprising the following steps: 1. adding the raw material of hydrocracking C9 arene (1) and mixed extraction solvent to an extraction rectifying tower; controlling the temperature of the top of the rectifying tower to be in a range of 175.1-176.5 DEG C and controlling the temperature of the tower bottoms to be in a range of 205-208 DEG C; extracting the top of the rectifying tower (2) to obtain the trimethylbenzene fraction with the content being over 99%, wherein, the content of indan and bicyclopentane is lower than 1% and the bottom of the tower contains a large amount of mixed extraction solvent and the fraction (3) of heavy arene; and 2. processing the fraction (3) by a solvent recovery tower the top of which contains heavy arene fraction (5), wherein, the bottom contains the mixed extraction solvent to flow into the extraction rectifying tower for recycling. The feeding position is at the fifteenth plate, the number of theoretical plate is 32, the reflux ratio is 2-3, the top of the solvent recovery tower is heavy arene fraction, and the bottom of the tower is extraction solvent to flow into the extraction rectifying tower for recycling. The method of the invention only needs one-time extractive rectification, obviously improves efficiency and reduces energy consumption and cost.

Description

The double solvents extraction fractional distillation extracts hydrocracking C 9The method of middle trimethylbenzene cut
Technical field
The present invention relates to a kind of chemical separating method, particularly a kind of double solvents extraction fractional distillation extracts hydrocracking C 9The method of middle trimethylbenzene cut.
Background technology
Cracking C 9Aromatic hydrocarbons is the by product of ethylene unit, accounts for 10～20% of ethene ultimate production.Along with the raising of ethylene yield, to cracking C in 2010 9The output of aromatic hydrocarbons will reach 1.1 * 10 6More than the t/a.Cracking C 9Aromatic hydrocarbons and crude oil and the course of processing thereof have confidential relation, form extremely complexity, and color are dark, peculiar smell is big.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 double solvents extraction fractional distillation and extract hydrocracking C 9The method of trimethylbenzene cut in the aromatic hydrocarbons.Technology of the present invention mainly contains: the one, select composite extractant; The 2nd, the method for employing extracting rectifying is extracted the cut that is rich in trimethylbenzene of higher degree, uses the hybrid extraction solvent of tetramethylene sulfone and dibutyl phthalate in this process first, and 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 double solvents extraction fractional distillation extracts hydrocracking C 9The method of middle trimethylbenzene cut, step is as follows:
(1). raw material hydrocracking C 91. aromatic hydrocarbons join extractive distillation column with the hybrid extraction solvent, the control tower top temperature is at 175.1～176.5 ℃, tower still temperature is at 205～208 ℃, the content that 2. the extracting rectifying column overhead obtains the trimethylbenzene cut is more than 99%, at the bottom of the tower be contain macro-mixing extraction solvent and heavy aromatics cut 3.;
(2). 3. cut is handled through solvent recovery tower, and 5. the solvent recuperation column overhead attaches most importance to aromatic fraction, and still is that the hybrid extraction solvent flows into extractive distillation column again, recycles.
Above scheme, the hybrid extraction solvent that the described hybrid extraction solvent in described (1) step adopts tetramethylene sulfone and dibutyl phthalate to form, the volume ratio of tetramethylene sulfone and dibutyl phthalate is 0.5～1: 1; The volume ratio of this hybrid extraction solvent and extractive distillation column raw material inlet amount is 0.5～1.2: 1.
The application recommends: the volume ratio of tetramethylene sulfone and dibutyl phthalate is 0.8: 1; The volume ratio of this hybrid extraction solvent and extractive distillation column raw material inlet amount is 1: 1.
Say that more specifically and more optimally operation steps of the present invention is:
(1) raw material hydrocracking C 91. aromatic hydrocarbons add extractive distillation column, 38 of feed entrance points, inlet amount is 2ml/min, and the extraction solvent feed entrance point is at the 5th block of plate, and theoretical plate number is 47, the control tower top temperature is at 175.1～176.5 ℃, 2. and 3. tower still temperature is at 205～208 ℃, and reflux ratio is 3～4, and load is respectively 0.51ml/min, 3.29ml/min, the content that 2. cat head obtains the trimethylbenzene cut reaches more than 99%, the tower still be contain a large amount of extraction solvents and heavy aromatics cut 3.;
(2) 3. the above-mentioned cut that contains a large amount of extraction solvents and heavy aromatics is handled through solvent recovery tower, the control inlet amount is 3.29ml/min, 4. and 5. load is respectively 1.49ml/min, 1.8ml/min, and tower top temperature is at 185.4～187.6 ℃, and tower still temperature is at 237.3～242.6 ℃, feed entrance point is at the 15th block of plate, number of theoretical plate is 32, and reflux ratio is 2～3, and 5. 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.
Above scheme, the tetramethylene sulfone in described (1) step and the hybrid extraction solvent of dibutyl phthalate, the volume ratio of tetramethylene sulfone and dibutyl phthalate is 0.5～1: 1; The volume ratio of this hybrid extraction solvent and extractive distillation column raw material inlet amount is 0.5～1.2: 1.
The processing condition of table 1 sepn process
Processing parameter Extractive distillation column Solvent recovery tower
Raw material inlet amount (ml/min) ??2 ??3.3
Composite extractant inlet amount (ml/min) ??1.8 ??/
Load (ml/min) ??D 2＝1.7??D 3＝0.3 ??D 4＝1.49??D 5＝1.8
Tower top temperature (℃) ??175.1～176.5 ??185.4～187.6
Column bottom temperature (℃) ??205.2～208.9 ??237.3～242.6
Reflux ratio (R) ??3～4 ??2～3
Theoretical plate number (N) ??47 ??32
Raw material feed entrance point (N) ??38 ??15
Extractant feed position (N) ??5 ??/
The composition and the content of each cut of table 2 sepn process
Figure G2009102644479D00041
Compare with bibliographical information technology, the present invention selects tetramethylene sulfone and dimethyl phthalate composite extractant, adopts extracting rectifying to extract the trimethylbenzene cut, and the content of trimethylbenzene cut is brought up to more than 99%, and yield is 84.51%.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 of trimethylbenzene cut in the hydrocracking carbon nine for the double solvents extracting rectifying;
Fig. 2 is a double solvents extracting rectifying experimental installation.
Embodiment
Embodiment 1, and double solvents extraction rectification technique and experimental installation see figures.1.and.2 respectively, and wherein 1 is feed sump, and 2 is pump, 3 is glass rotameter, and 4 is tower still sampler, and 5 is electric mantle, 6 is the tower still, and 7 is tower still thermometer, and 8 is solvent feed tank, 9 is pump, and 10 is glass rotameter, and 11 is glass fibre cotton and chuck, 12 is filler, and 13 is the cat head sampler, and 14 is refluxing opening, 15 is the tower top temperature meter, and 16 is electromagnetic wand, and 17 is condenser.The double solvents extraction fractional distillation extracts and is rich in the trimethylbenzene cut, and each tower internal diameter is 22cm, adopts The type Stainless Steel Helices, through measuring with standards system, this height equivalent to one theoretical plate HETP=27mm, tower still adopt the heating of voltate regulator controlling resistance silk, are undertaken quantitatively and qualitative analysis by the gas chromatography-mass spectrometry chromatogram instrument.Hydrocracking C 91. aroamtic hydrocarbon raw material enters extractive distillation column, and the control inlet amount is 2ml/min, and the extractant feed amount is 1.8ml/min, load D 2And D 3Be respectively 0.51ml/min and 3.29ml/min, the control tower top temperature is at 175.1～176.5 ℃, tower still temperature is at 205～208 ℃, reflux ratio is 3～4, theoretical plate number is 47, and feed entrance point is at 38 column plate places, and extractant feed is located at 5, the volume ratio of tetramethylene sulfone and dibutyl phthalate is 0.8: 1, and the volume ratio of compound extracting solvent and extractive distillation column raw material inlet amount is 1: 1.Cat head trimethylbenzene cut can be brought up to more than 99%, and indane and dicyclo pentane content are lower than 1%, and detailed analysis sees Table 2; 3. cut is handled through solvent recovery tower, the control inlet amount is 3.29ml/min, and 4. and 5. load is respectively 1.49ml/min, 1.8ml/min, and tower top temperature is at 185.4～187.6 ℃, tower still temperature is at 237.3～242.6 ℃, feed entrance point is at the 15th block of plate, and number of theoretical plate is 32, and reflux ratio is 2～3,5. 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, and detailed analysis sees Table 2.
Embodiment 2, and is substantially the same manner as Example 1, but described (2) extraction solvent is the compound extracting solvent of tetramethylene sulfone and dibutyl phthalate, and the volume ratio of tetramethylene sulfone and dibutyl phthalate is 0.5～1: 1; The volume ratio of this compound extracting solvent and extractive distillation column raw material inlet amount is 0.5～1.2: 1.
Embodiment 3, and is substantially the same manner as Example 1, but the extraction solvent in described (2) step is the compound extracting solvent of tetramethylene sulfone and dibutyl phthalate, and the volume ratio of tetramethylene sulfone and dibutyl phthalate is 0.5: 1; The volume ratio of this compound extracting solvent and extractive distillation column raw material inlet amount is 0.5: 1.
Embodiment 4, and is substantially the same manner as Example 1, but the extraction solvent in described (2) step is the compound extracting solvent of tetramethylene sulfone and dibutyl phthalate, and the volume ratio of tetramethylene sulfone and dibutyl phthalate is 0.7: 1; The volume ratio of this compound extracting solvent and extractive distillation column raw material inlet amount is 0.7: 1.
Embodiment 5, and is substantially the same manner as Example 1, but the extraction solvent in described (2) step is the compound extracting solvent of tetramethylene sulfone and dibutyl phthalate, and the volume ratio of tetramethylene sulfone and dibutyl phthalate is 0.9: 1; The volume ratio of this compound extracting solvent and extractive distillation column raw material inlet amount is 0.9: 1.
Embodiment 6, and is substantially the same manner as Example 1, but the extraction solvent in described (2) step is the compound extracting solvent of tetramethylene sulfone and dibutyl phthalate, and the volume ratio of tetramethylene sulfone and dibutyl phthalate is 1: 1; The volume ratio of this compound extracting solvent and extractive distillation column raw material inlet amount is 1.2: 1.

Claims (5)

1. a double solvents extraction fractional distillation extracts hydrocracking C 9The method of middle trimethylbenzene cut, step is as follows:
(1). raw material hydrocracking C 91. aromatic hydrocarbons join extractive distillation column with the hybrid extraction solvent, the control tower top temperature is at 175.1～176.5 ℃, tower still temperature is at 205～208 ℃, the content that 2. the extracting rectifying column overhead obtains the trimethylbenzene cut is more than 99%, at the bottom of the tower be contain macro-mixing extraction solvent and heavy aromatics cut 3.;
(2). 3. cut is handled through solvent recovery tower, and 5. the solvent recuperation column overhead attaches most importance to aromatic fraction, and still is that the hybrid extraction solvent flows into extractive distillation column again, recycles.
2. double solvents extraction fractional distillation according to claim 1 extracts hydrocracking C 9The method of middle trimethylbenzene cut is characterized in that,
Composite extractant described in (1) step is the hybrid extraction solvent that tetramethylene sulfone and dibutyl phthalate are formed, and wherein, the volume ratio of tetramethylene sulfone and dibutyl phthalate is 0.5～1.0: 1; The volume ratio of this compound extracting solvent and extractive distillation column raw material inlet amount is 0.5～1.2: 1.
3. double solvents extraction fractional distillation according to claim 2 extracts hydrocracking C 9The method of middle trimethylbenzene cut is characterized in that the volume ratio of described tetramethylene sulfone and dibutyl phthalate is 0.8: 1; The volume ratio of described compound extracting solvent and raw material inlet amount is 1: 1.
4. extract hydrocracking C according to claim 1 or 2 or 3 described double solvents extraction fractional distillations 9In be rich in the method for trimethylbenzene cut, it is characterized in that the concrete operations step is:
(1). raw material hydrocracking C 91. aromatic hydrocarbons add extractive distillation column, 41 of feed entrance points, inlet amount is 2ml/min, the extraction solvent feed entrance point is at the 5th block of plate, theoretical plate number is 47, the control tower top temperature is at 175.1～176.5 ℃, tower still temperature is at 205～208 ℃, reflux ratio is 3～4,2. and 3. load is respectively 0.51ml/min, 1.49ml/min, the content that 2. cat head obtains the trimethylbenzene cut is more than 99%, and indane and dicyclo pentane total content be less than 1%, the tower still be contain a large amount of extraction solvents and heavy aromatics cut 3.;
(2). 3. the above-mentioned cut that contains a large amount of extraction solvents and heavy aromatics is handled through solvent recovery tower, the control inlet amount is 3.29ml/min, 4. and 5. load is respectively 1.49ml/min, 1.8ml/min, and tower top temperature is at 185.4～187.6 ℃, and tower still temperature is at 237～242 ℃, feed entrance point is at the 15th block of plate, number of theoretical plate is 32, and reflux ratio is 2～3, and 5. the solvent recuperation column overhead attaches most importance to aromatic fraction, the tower still is that composite extractant flows into extractive distillation column again, recycles.
5. double solvents extraction fractional distillation according to claim 4 extracts hydrocracking C 9The method of middle trimethylbenzene cut is characterized in that the composition of described processing condition and each cut and content are as shown in Table 1 and Table 2.
The processing condition of table 1 sepn process
Processing parameter Extractive distillation column Solvent recovery tower Raw material inlet amount (ml/min) ??2 ??3.3 Composite extractant inlet amount (ml/min) ??1.8 ??/ Load (ml/min) ??D 2＝1.7??D 3＝0.3 ??D 4＝1.49??D 5＝1.8 Tower top temperature (℃) ??175.1～176.5 ??185.4～187.6
Processing parameter Extractive distillation column Solvent recovery tower Column bottom temperature (℃) ??205.2～208.9 ??237.3～242.6 Reflux ratio (R) ??3～4 ??1～2 Theoretical plate number (N) ??47 ??32 Raw material feed entrance point (N) ??38 ??15 Extractant feed position (N) ??5 ??/
The composition and the content of each cut of table 2 sepn process
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102850158A (en) * 2011-06-29 2013-01-02 中国石油化工股份有限公司 Mixed solvent for C 5 separation
CN103113179A (en) * 2013-02-07 2013-05-22 天津大学 Thermal coupling system and method for extractive distillation of normal hexane, isohexane and benzene
CN103772230A (en) * 2014-02-13 2014-05-07 南京师范大学 Method for separating mixing solution of sodium salt, dimethyl formamide, methylbenzene and water through integration of azeotropic/extractive distillation and liquid-liquid stratification

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102850158A (en) * 2011-06-29 2013-01-02 中国石油化工股份有限公司 Mixed solvent for C 5 separation
CN102850158B (en) * 2011-06-29 2014-12-31 中国石油化工股份有限公司 Mixed solvent for C5 separation
CN103113179A (en) * 2013-02-07 2013-05-22 天津大学 Thermal coupling system and method for extractive distillation of normal hexane, isohexane and benzene
CN103113179B (en) * 2013-02-07 2015-03-25 天津大学 Thermal coupling system and method for extractive distillation of normal hexane, isohexane and benzene
CN103772230A (en) * 2014-02-13 2014-05-07 南京师范大学 Method for separating mixing solution of sodium salt, dimethyl formamide, methylbenzene and water through integration of azeotropic/extractive distillation and liquid-liquid stratification
CN103772230B (en) * 2014-02-13 2016-01-27 南京师范大学 The method of the mixing solutions of azeotropic extraction rectifying and liquid liquid layering integrated purification sodium salt, dimethyl formamide, toluene and water

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Application publication date: 20100616