CN102617262B - Energy-saving process method for separating cyclohexane-cyclohexene-benzene - Google Patents

Energy-saving process method for separating cyclohexane-cyclohexene-benzene Download PDF

Info

Publication number
CN102617262B
CN102617262B CN201210041613.0A CN201210041613A CN102617262B CN 102617262 B CN102617262 B CN 102617262B CN 201210041613 A CN201210041613 A CN 201210041613A CN 102617262 B CN102617262 B CN 102617262B
Authority
CN
China
Prior art keywords
extractive distillation
distillation column
tower
benzene
tetrahydrobenzene
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Fee Related
Application number
CN201210041613.0A
Other languages
Chinese (zh)
Other versions
CN102617262A (en
Inventor
蓝仁水
黄贵明
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Tianjin New Tianjin Technology And Development Co Ltd
Original Assignee
Individual
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Individual filed Critical Individual
Priority to CN201210041613.0A priority Critical patent/CN102617262B/en
Publication of CN102617262A publication Critical patent/CN102617262A/en
Application granted granted Critical
Publication of CN102617262B publication Critical patent/CN102617262B/en
Expired - Fee Related legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Images

Landscapes

  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)

Abstract

The invention relates to an energy-saving process method for separating cyclohexane-cyclohexene-benzene, which is used for respectively obtaining cyclohexane, cyclohexane and benzene from mixed raw materials containing the cyclohexane, the cyclohexane and the benzene by means of extractive distillation. A traditional four-tower and two-step extractive distillation process is changed into a one-step extractive distillation process, and the cyclohexane is separated from the cyclohexane and the benzene while the cyclohexane is separated from the benzene by means of extractive distillation, so that energy consumption needed during separation is greatly reduced. The energy-saving process method overcomes the shortcomings of the prior art, and has remarkable practicability and energy-saving effects.

Description

The energy-saving process method of a kind of hexanaphthene-tetrahydrobenzene-benzene separation
Technical field
The present invention relates to the extraction rectification technique in chemical separation engineering, particularly the energy-saving process method of a kind of hexanaphthene-tetrahydrobenzene-benzene separation, can generally be applied in various extracting rectifying processes.
Background technology
For the very little system of boiling point difference, extracting rectifying is a kind of product separation method comparatively generally adopting in chemical separation engineering.The for example sepn process of hexanaphthene-tetrahydrobenzene-benzene, boiling-point difference between hexanaphthene (80.7 ℃ of boiling points), tetrahydrobenzene (83 ℃ of boiling points), benzene (80.1 ℃ of boiling points) is very little, the general N that adopts, N-N,N-DIMETHYLACETAMIDE (DMAC) is as extraction agent, the method that adopts extracting rectifying, is separated into hexanaphthene, tetrahydrobenzene and three products of benzene by above-mentioned three components.Above-mentioned common process flow process as shown in Figure 1.
As shown in Figure 1, the mixing raw material that contains hexanaphthene, tetrahydrobenzene, benzene, be introduced into T-201 debenzolizing tower bottom, T-201 top adds extraction agent (adopting DMAC as extraction agent), benzene in charging is extracted into tower reactor, tower top obtains hexanaphthene, tetrahydrobenzene mixture (substantially not containing benzene), and tower reactor is the mixture (substantially not containing hexanaphthene and tetrahydrobenzene) of benzene and extraction agent.T-201 tower reactor material enters T-202 benzene recovery tower.T-202 tower parses the benzene in extraction agent, and tower top obtains benzaldehyde product, and tower reactor is substantially not containing the extraction agent of benzene, returns to T-201 tower top recycle through heat exchange, after cooling.The discharging of T-201 tower top enters T-203 tetrahydrobenzene knockout tower bottom.T-203 top adds extraction agent, and tetrahydrobenzene is extracted into tower reactor, and tower top obtains hexanaphthene product (substantially not containing tetrahydrobenzene), and tower reactor is the mixture (substantially not containing hexanaphthene) of tetrahydrobenzene and extraction agent.T-203 tower reactor material enters T-204 tetrahydrobenzene recovery tower.T-204 tower parses the tetrahydrobenzene in extraction agent, and T-204 tower top obtains tetrahydrobenzene product, and tower reactor is substantially not containing the extraction agent of tetrahydrobenzene, returns to T-203 tower top recycle through heat exchange, after cooling.
The greatest drawback of above-mentioned technical process is, whole tetrahydrobenzene in raw material have been extracted rectifying twice, be for the first time in T-201 under the effect of extraction agent, all tetrahydrobenzene (containing hexanaphthene) is separated with benzene, all tetrahydrobenzene (containing hexanaphthene) is distillated by T-201 tower top, and all benzene is distillated by T-201 tower reactor; Be for the second time in T-203 under the effect of extraction agent, all tetrahydrobenzene are separated with hexanaphthene, all tetrahydrobenzene are distillated by T-203 tower reactor, all hexanaphthenes are distillated by T-203 tower top.Therefore all tetrahydrobenzene, by twice extracting rectifying, has increased operation energy consumption greatly.
As shown in Figure 2, Chinese patent CN200410036497.9 discloses a kind of pair of partitioned column and has extracted 1, the devices and methods therefor of 3-divinyl, its basic conception is that twice extracting rectifying of traditional divinyl operated in a tower and completed, but its essence is just carried out simple combination by two traditional crosscurrent extraction rectifying tower.Wash plate 2 in Fig. 2 is divided into left and right two portions by whole extractive distillation column top, the separation of extractive distillation process of divinyl and butylene completes in dividing plate left side, the extracting rectifying process of divinyl and alkynes completes on the right side of dividing plate, this patent is only to utilize this Novel tower structure of partitioned column, two extractive distillation columns that traditional twice extracting rectifying process is used carry out simple combination, from two crosscurrent extraction rectifying tower are become to a partitioned column of establishing central dividing plate in form, its essence remains extracting rectifying process twice, so its butylene, divinyl, the overall energy consumption of alkynes three separation of extractive distillation process cannot reduce.
Chinese patent CN200410036497.9 discloses a kind of method of separation of extractive distillation hexanaphthene and tetrahydrobenzene, consistent with the method for traditional technology shown in Fig. 1 of the processing method providing, only scope is contracted to the T-203 in flow process shown in Fig. 1, T-204 two towers, the specifically hexanaphthene of T-203 tower and tetrahydrobenzene extracting rectifying, the solvent reclamation process of T-204 tower, this extracting rectifying, solvent regeneration process method itself be well-known, the essence of Chinese patent CN200410036497.9 is to propose solvent---the tetramethylene sulfone that another kind of extracting rectifying is used.
Summary of the invention
The energy-saving process method that the object of this invention is to provide the separation of a kind of hexanaphthene-tetrahydrobenzene-benzene, can overcome the defect of prior art.It is from containing the mixing raw material of hexanaphthene, tetrahydrobenzene, benzene, by the method for extracting rectifying, obtain respectively the energy-saving process method of hexanaphthene, tetrahydrobenzene, three products of benzene, there is significant practicality and extremely significant energy-saving effect, have a extensive future.
As shown in Figure 3, the energy-saving process method of a kind of hexanaphthene-tetrahydrobenzene-benzene provided by the invention separation be the mixture that contains hexanaphthene, tetrahydrobenzene, benzene be raw material, by extracting rectifying, operate the processing method of separating benzene-cyclohexane, tetrahydrobenzene and benzene, it is characterized in that comprising following step:
(1) at least comprise extractive distillation column, benzene recovery tower and tetrahydrobenzene recovery tower.
(2) annexation between extractive distillation column A, extractive distillation column B, extractive distillation column C is: in extractive distillation column A, be provided with dividing plate 128 extractive distillation column A is divided into Shang Ta and lower tower two portions, and gas-liquid is not communicated with mutually.The upper tower tower reactor gas-phase feed (origin of heat) of extractive distillation column A is extractive distillation column B and extractive distillation column C top gaseous phase.Extractive distillation column B and extractive distillation column C tower top liquid phase feeding are the upper tower tower reactor liquid of extractive distillation column A.Extractive distillation column B and extractive distillation column C tower reactor gas-phase feed (origin of heat) are column overhead gas phase under extractive distillation column A.Under extractive distillation column A, column overhead liquid phase feeding is extractive distillation column B and extractive distillation column C tower reactor liquid.
(3) the upper tower of extractive distillation column A completes the separated of hexanaphthene and tetrahydrobenzene, and the tower top of extractive distillation column A obtains the hexanaphthene that purity is qualified; Under extractive distillation column A, tower completes the separated of tetrahydrobenzene and benzene, and tower reactor discharging is benzene and solvent, substantially containing hexanaphthene and tetrahydrobenzene;
(4) in extractive distillation column B, complete benzene separated with hexanaphthene, complete the separated of a part of tetrahydrobenzene and benzene simultaneously, in the discharging of extractive distillation column B top gaseous phase, only contain hexanaphthene, tetrahydrobenzene and solvent, substantially containing benzene; In the discharging of extractive distillation column B tower reactor liquid phase, only contain tetrahydrobenzene, benzene and solvent, substantially not containing hexanaphthene;
(5) extractive distillation column C top completes the completely separated of hexanaphthene and tetrahydrobenzene, and bottom completes the completely separated of tetrahydrobenzene and benzene, the solvent-laden tetrahydrobenzene of middle part side line extraction.
(6) charging of tetrahydrobenzene recovery tower is the solvent-laden tetrahydrobenzene of extractive distillation column C middle part side line extraction, and tetrahydrobenzene recovery tower tower top obtains the tetrahydrobenzene product that purity is qualified.
(7) charging of benzene recovery tower is tower tower reactor discharging under extractive distillation column A, and benzene recovery tower tower top obtains the benzaldehyde product that purity is qualified; Benzene recovery tower tower reactor material is as circulating solvent, through heat exchange, after cooling, returns to the upper tower solvent discharging of extractive distillation column A position.
Step (2) and (3) said solvent enter the middle and upper part of the upper tower of extractive distillation column A, and mixing raw material enters extractive distillation column B middle and upper part.Typical solvent is DMAC (N,N-DIMETHYLACETAMIDE), also can adopt the conventional solvents such as tetramethylene sulfone, N-Methyl pyrrolidone for the present invention.
The said extractive distillation column C of step (5) middle part side-stream typically is the gaseous stream from extractive distillation column C middle and lower part; Or from the liquid phase stream of extractive distillation column C middle and lower part; Also can a part be that gaseous stream, another part from extractive distillation column C middle and lower part is the liquid phase stream from extractive distillation column C middle and lower part.
The said tetrahydrobenzene recovery tower of step (6) tower reactor material can return to extractive distillation column C lateral line discharging position, or extractive distillation column C tower reactor material is carried out to holomorphosis, and tetrahydrobenzene recovery tower tower reactor material is returned to position, the upper tower middle and upper part of extractive distillation column A.
The said extractive distillation column B in step (1)~(5) and extractive distillation column C can arrange respectively intermediate reboiler, use and heat compared with low-grade heat source.
By processing method provided by the invention, can draw one gas phase by top of tower under extractive distillation column A and remove benzene recovery tower, this burst of gas phase, as the charging of benzene recovery tower, again as benzene recovery tower tower reactor thermal source, can be saved benzene recovery tower tower reactor reboiler simultaneously.
By processing method provided by the invention, extractive distillation column typically can adopt three towers shown in Fig. 3 (C-201A, C-201B and C-201C) series connection; Also can adopt two towers shown in Fig. 4 (C-201A and C-201B) series connection; Or the C-201B shown in Fig. 4 is placed in to C-201A top, and C-201A and C-201B merge into a high tower; Extractive distillation column (for example: 3~6 tower serial operations) can also be divided into three above tower series connection.
The essential distinction of the present invention and common process is, twice extracting rectifying process of the tetrahydrobenzene in the common process flow process of hexanaphthene, tetrahydrobenzene and benzene extracting rectifying combined.The charging of extractive distillation column B has three strands, first strand of mixing raw material 102 for containing hexanaphthene, tetrahydrobenzene, benzene, second strand is the liquid phase mixture that contains hexanaphthene/tetrahydrobenzene and solvent 104 from the upper tower tower reactor of extractive distillation column A, the 3rd strand is from the tetrahydrobenzene/hexanaphthene of column overhead under extractive distillation column A and the gas phase mixture of solvent 103, in extractive distillation column B, complete the extracting rectifying process of hexanaphthene and benzene, extractive distillation column B tower top distillates the gaseous stream 106 that does not substantially contain benzene, and extractive distillation column B tower reactor obtains substantially not containing the liquid phase stream 105 of hexanaphthene.
Extractive distillation column B has completed the completely separated of benzene and hexanaphthene, and tetrahydrobenzene is divided into two portions simultaneously, a part is admitted to the tower reactor of tower on extractive distillation column A together with hexanaphthene in 106 logistics, and another part is admitted to the tower top of tower under extractive distillation column A together with benzene in 105 logistics.
The charging of extractive distillation column C has two strands, first strand is the gas phase mixture that contains tetrahydrobenzene/benzene and solvent 107 from top of tower under extractive distillation column A, second strand is from the upper tetrahydrobenzene/hexanaphthene of tower tower reactor of extractive distillation column A and the liquid phase mixture of solvent 108, in extractive distillation column C, complete the extracting rectifying process of hexanaphthene and benzene, extractive distillation column C tower top distillates the gaseous stream 110 that does not substantially contain benzene, and extractive distillation column C tower reactor obtains substantially not containing the liquid phase stream 109 of hexanaphthene.
Extractive distillation column C when carrying out above-mentioned hexanaphthene/benzene extracting rectifying process, has also completed residue ring hexene that extractive distillation column B do not complete and the sepn process of benzene.The top of extractive distillation column C completed the separated of hexanaphthene and tetrahydrobenzene, and bottom has completed the separated of tetrahydrobenzene and benzene, and tetrahydrobenzene is in the enrichment of the middle and lower part of extractive distillation column C.
The top of extractive distillation column C distillates (containing part tetrahydrobenzene) by the hexanaphthene in logistics 108 through logistics 110, and the top of extractive distillation column C is by the tetrahydrobenzene purifying in logistics 108 and be enriched in side line position, extractive distillation column C middle and lower part.The bottom of extractive distillation column C distillates (containing part tetrahydrobenzene) by the benzene in logistics 107 through logistics 109, and the bottom of extractive distillation column C is by the tetrahydrobenzene purifying in logistics 107 and be enriched in side line position, extractive distillation column C middle and lower part.Tetrahydrobenzene in mixing raw material is delivered to extractive distillation column C through 107,108 two bursts of logistics, and by the upper and lower of extractive distillation column C respectively to extractive distillation column C middle and lower part side line position purifying and enrichment, in side line position, extractive distillation column C middle and lower part, only have tetrahydrobenzene and solvent (hardly containing hexanaphthene and benzene).Then the whole tetrahydrobenzene in mixing raw material are transported to tetrahydrobenzene recovery tower C-203 through logistics 123, by C-203 tower top, obtain the tetrahydrobenzene product that purity is qualified.The logistics of C-203 tower reactor is the solvent that contains part tetrahydrobenzene, returns to extractive distillation column C lateral line discharging position.
Under extractive distillation column A, tower tower reactor logistics 114 is that benzene and solvent (substantially containing hexanaphthene and tetrahydrobenzene) are admitted to benzene recovery tower C-202, by C-202 tower top, obtain the benzaldehyde product 118 that purity is qualified, C-202 tower reactor is regenerated solvent 119, returns to the upper tower solvent feed of extractive distillation column A position after heat exchange is cooling.
In sum, the present invention compares with common process flow process, by twice extracting rectifying process of whole tetrahydrobenzene, become the pre-extracting rectifying process of a part of tetrahydrobenzene in extractive distillation column B, and organic parallel work-flow of the pre-extracting rectifying process of another part tetrahydrobenzene in extractive distillation column C.The required heat of above-mentioned concurrent extracting rectifying is all provided by tower rising steam under extractive distillation column A, and the required cold of above-mentioned concurrent extracting rectifying is all provided by the upper tower dropping liq of extractive distillation column A.Therefore the energy of whole separation of extractive distillation process is only equivalent to T-201 and the more person of T-203 tower institute energy requirement in conventional extracting rectifying process, for hexanaphthene, tetrahydrobenzene, benzene separation of extractive distillation process, the energy of required energy equivalence T-203 tower in conventional extracting rectifying process (the required energy of T-203 tower is greater than T-201 tower institute energy requirement).
The energy-saving process method typical operation conditions of a kind of hexanaphthene-tetrahydrobenzene-benzene provided by the invention separation is as follows.
Except specified otherwise, in this specification sheets in all pressure all refer to absolute pressure.
According to the energy-saving process method of a kind of hexanaphthene-tetrahydrobenzene-benzene provided by the invention separation, the ratio range of extractive distillation column solvent load and hexanaphthene, tetrahydrobenzene, benzene mixing raw material amount is 2~8: 1, preferably 3~6: 1.
The present invention not only can, for said hexanaphthene-tetrahydrobenzene-benzene extracting rectifying, can also be applied in the extracting rectifying process of the butane/butylene of mixed c 4, the similar extracting rectifying processes such as extracting rectifying process of the extracting rectifying process of divinyl/butylene/alkynes, mixing pentadiene.
The present invention can also be respectively by the technical process of extractive distillation column B and extractive distillation column C and extractive distillation column A merging (shown in Fig. 4).
The present invention can also be respectively by the technical process of extractive distillation column B and extractive distillation column C and extractive distillation column A merging (shown in Fig. 5).
In the present invention, extractive distillation column B and extractive distillation column C also can arrange respectively intermediate reboiler, use and heat compared with low-grade heat source.
In the present invention, by extractive distillation column B middle and lower part side line, draw one liquid phase stream 136 and go to extractive distillation column C middle and lower part, extractive distillation column B and extractive distillation column C tower reactor obtain respectively the material that only contains benzene and solvent, and then C-202 benzene recovery tower is removed in merging.
In the present invention, under extractive distillation column A, tower reboiler can adopt structure as shown in Figure 8, by preferentially entering tower reactor reboiler after the liquid collecting declining in lower tower, to increase the heat transfer temperature difference of tower reactor reboiler.
In the present invention, under extractive distillation column A, tower reboiler can adopt structure as shown in Figure 9, by preferentially entering tower reactor reboiler after the liquid collecting declining in lower tower, to increase the heat transfer temperature difference of tower reactor reboiler.
The present invention has overcome the shortcoming of prior art, has significant practicality and extremely significant energy-saving effect, has a extensive future.
Accompanying drawing explanation
Fig. 1 is existing common process flow process, the hexanaphthene-tetrahydrobenzene of four towers of employing, twice extracting rectifying-benzene sepn process general flow chart.
Fig. 2 is the devices and methods therefor that a kind of pair of partitioned column extracts 1,3-butadiene.
Fig. 3 is the energy-saving process method general flow chart of a kind of hexanaphthene-tetrahydrobenzene-benzene provided by the invention separation.
Fig. 4 is the modified flow a kind of of equal value of the energy-saving process method flow process of hexanaphthene-tetrahydrobenzene-benzene separation of providing of Fig. 3.
Fig. 5 is the another kind modified flow of equal value of the energy-saving process method flow process of hexanaphthene-tetrahydrobenzene-benzene separation of providing of Fig. 3.
Fig. 6 is the modified flow a kind of of equal value of the energy-saving process method flow process of a kind of hexanaphthene-tetrahydrobenzene-benzene separation of providing of Fig. 3, at extractive distillation column B and extractive distillation column C tower reactor, intermediate reboiler is set respectively.
Fig. 7 is the another kind modified flow of equal value of the energy-saving process method flow process of hexanaphthene-tetrahydrobenzene-benzene separation of providing of Fig. 3.
Fig. 8 is a kind of method to set up of tower reboiler under extractive distillation column A.
Fig. 9 is the another kind of method to set up of tower reboiler under extractive distillation column A.
Figure 10 draws one gas phase by top of tower under extractive distillation column A to remove benzene recovery tower.
Embodiment
Specific embodiment of the invention scheme is described in detail as follows with reference to accompanying drawing, but for illustrative purposes only rather than restriction the present invention.
As shown in Figure 3, the invention provides the energy-saving process method of a kind of hexanaphthene-tetrahydrobenzene-benzene separation, the mixing raw material 101 that contains hexanaphthene, tetrahydrobenzene and benzene enters the middle and upper part of extractive distillation column B after preheating as the charging 102 of extractive distillation column B (C-201B).Extractive distillation column A (C-201A) establishes a dividing plate 128 in inside, and extractive distillation column A is divided into tower 132 under the upper tower 131 of extractive distillation column A and extractive distillation column A, and between 131 and 132 in tower gas-liquid be not communicated with.The upper tower tower reactor liquid phase of extractive distillation column A is divided into two strands, one is 104 (only containing hexanaphthene, tetrahydrobenzene and solvent, substantially containing benzene) enter C-201B tower top, another strand 108 (only containing hexanaphthene, tetrahydrobenzene and solvent, substantially not containing benzene) enters the top of extractive distillation column C (C-201C).Under extractive distillation column A, column overhead gas phase is divided into two strands, one is 103 (only containing tetrahydrobenzene, benzene and solvent, substantially containing hexanaphthene) tower reactor that enters C-201B, the tower reactor that another strand 107 (only containing tetrahydrobenzene, benzene and solvent, substantially containing hexanaphthene) enters C-201C.
In the top gaseous phase 106 of C-201B, only contain the bottom that hexanaphthene, tetrahydrobenzene and solvent (substantially not containing benzene) enter the upper tower of extractive distillation column A.In the tower reactor liquid phase 105 of C-201B, only containing tetrahydrobenzene, benzene and solvent (substantially not containing hexanaphthene), enter the top of tower 132 under extractive distillation column A.
In the top gaseous phase 110 of C-201C, only contain the bottom that hexanaphthene, tetrahydrobenzene and solvent (substantially not containing benzene) enter the upper tower of extractive distillation column A.In the tower reactor liquid phase 109 of C-201C, only containing tetrahydrobenzene, benzene and solvent (substantially not containing hexanaphthene), enter the top of tower 132 under extractive distillation column A.
Extraction solvent 122 enters the top of the upper tower of extractive distillation column A, and the upper column overhead gas phase 111 of extractive distillation column A is returned to the upper column overhead of extractive distillation column A through condensation rear portion as backflow 112, and another part is as 113 extraction of hexanaphthene product.
Under C-201A, tower tower reactor discharging 114 forms and is mainly benzene and solvent (substantially containing hexanaphthene and tetrahydrobenzene) enters benzene recovery tower C-202, C-202 top gaseous phase 116 returns to C-202 tower top through condensation rear portion as backflow 117, and another part is as benzaldehyde product 118 extraction.
C-201C middle and lower part is extracted tetrahydrobenzene (containing solvent) side line 123 out and is entered tetrahydrobenzene recovery tower C-203, and C-203 top gaseous phase 124 returns to C-203 tower top through condensation rear portion as backflow 125, and another part is as 126 extraction of tetrahydrobenzene product.C-203 tower reactor material 127 is mainly solvent (containing a small amount of tetrahydrobenzene) and returns to C-201C lateral line withdrawal function position.
Fig. 4 is the modified flow of equal value such as energy-saving process method flow process of a kind of hexanaphthene-tetrahydrobenzene-benzene separation of providing of Fig. 3.The processing method that Fig. 4 provides is respectively three extractive distillation columns in Fig. 3 to be merged into two extractive distillation columns, and under extractive distillation column A, tower C-201A establishes dividing plate 129 in top, and C-201A top is divided into the not connected two portions of gas-liquid.On extractive distillation column B, tower C-201B establishes dividing plate 130 in bottom, and C-201B bottom is divided into the not connected two portions of gas-liquid.After preheating, mixing raw material 102 enters C-201A upper baffle plate left side, and C-201A dividing plate left side top gaseous phase 128 enters C-201B tower lower partition left side tower reactor, and C-201A dividing plate left side tower top is returned in C-201B tower lower partition left side tower reactor liquid phase discharging 130.C-201A dividing plate right side top gaseous phase 129 enters C-201B tower lower partition right side tower reactor, and C-201A dividing plate right side tower top is returned in C-201B tower lower partition right side tower reactor liquid phase discharging 131.
Fig. 5 is the modified flow of equal value such as energy-saving process method flow process of a kind of hexanaphthene-tetrahydrobenzene-benzene separation of providing of Fig. 3.The processing method that Fig. 5 provides is that under extractive distillation column A, tower is divided into two portions, then respectively by the extractive distillation column B in Fig. 3 and extractive distillation column C with connect, as new extractive distillation column B and new extractive distillation column C.More succinct from overall procedure, be new extractive distillation column B and a new reboiler of each need of extractive distillation column C tower reactor, Fig. 3 flow process reboiler quantity is many one relatively.
Fig. 6 is on the method basis providing at Fig. 3, and extractive distillation column B and extractive distillation column C arrange respectively intermediate reboiler, uses and heats compared with low-grade heat source.
Fig. 7 is on the method basis providing at Fig. 3, by extractive distillation column B middle and lower part side line, draw one liquid phase stream 136 and go to extractive distillation column C middle and lower part, extractive distillation column B and extractive distillation column C tower reactor obtain respectively the material that only contains benzene and solvent, and then C-202 benzene recovery tower is removed in merging.
Fig. 8 is a kind of method to set up of tower reboiler under extractive distillation column A.Under C-201A, tower tower reactor adopts two reboilers, tower reactor arranges dividing plate 132, and the preferential reboiler entrance that imports after dropping liq in tower is collected, to improve heat transfer temperature difference in reboiler, be beneficial to reboiler and stablize heat exchange, reduce reboiler area, under C-201A, the discharging of tower tower reactor is the liquid after reboiler heat exchange.
Fig. 9 is the another kind of method to set up of tower reboiler under extractive distillation column A.Under C-201A, tower tower reactor adopts separate unit reboiler, and the preferential reboiler inlet zone 134 that imports after dropping liq in tower is collected, and to improve heat transfer temperature difference in reboiler, is beneficial to reboiler and stablizes heat exchange, reduces reboiler area.Liquid after reboiler heat exchange enters tower reactor exit side 135 after 133 overflows of tower reactor dividing plate, and under C-201A, the discharging of tower tower reactor is the liquid after reboiler heat exchange.
Figure 10 draws one gas phase by top of tower under extractive distillation column A to remove benzene recovery tower, and this burst of gas phase, as the charging of benzene recovery tower, again as benzene recovery tower tower reactor thermal source, can be saved benzene recovery tower tower reactor reboiler simultaneously.
Application Example 1:
The energy-saving process method of a kind of hexanaphthene-tetrahydrobenzene-benzene separation that employing Fig. 3 provides contains the separation of the mixing raw material of hexanaphthene, tetrahydrobenzene, benzene, the 200000 tons/year of Caprolactam units of take are example, operation hours was by 8000 hours/year, the treatment capacity of the mixing raw material of hexanaphthene per hour, tetrahydrobenzene, benzene is 59344.3kg/h, and the classical group of mixing raw material becomes:
Title Each composition flow rate, kg/h Form wt%
Hexanaphthene 6855.6 52.247
Tetrahydrobenzene 21345.1 35.968
Benzene 31005.4 11.552
Light constituent 138.2 0.233
Add up to 59344.3 100.000
By the energy-saving process method of a kind of hexanaphthene-tetrahydrobenzene-benzene provided by the invention separation (processing method that Fig. 3 provides) and the processing method (shown in Fig. 1) of routine four towers that extensively adopt at present, twice extracting rectifying, carried out operation energy consumption (by adopting the saturation steam of gauge pressure 1.2Mpa to calculate) contrast, each tower operational condition and energy-saving effect contrast are listed in table 1~table 3.
Processing method operational condition and the energy consumption of conventional four towers of table 1, twice extracting rectifying
Figure BSA00000673864000071
Energy-saving process method operational condition and the energy consumption of the separation of table 2 a kind of hexanaphthene-tetrahydrobenzene-benzene provided by the invention
The above-mentioned two kinds of processing method operation energy consumptions contrast of table 3
Figure BSA00000673864000082
By above-mentioned correlation data, adopt the energy-saving process method of a kind of hexanaphthene-tetrahydrobenzene-benzene separation shown in Fig. 3 to compare operation energy consumption and reduced with adopting four towers, twice extraction rectification technique method (as shown in Figure 1):
(100.0-62.5)/100.0×100%=37.5%
The steam 100.0-62.5=37.5 ton of saving per hour.
Operation hours calculates for 8000 hours per year, can save steam every year
37.5 * 8000=300000 ton (300,000 tons).
By 200 yuan of calculating of steam per ton, can save steam expense every year:
300000 tons/year * 200 yuan/ton=6,000 ten thousand yuan/year.
When saving steam, also mean and saved a large amount of recirculated water consumption, and saved a large amount of general facilities configurations and power consumption.
The energy-saving process method of a kind of hexanaphthene-tetrahydrobenzene-benzene provided by the invention separation, has extremely distinct economic.Illustrated, the personnel of association area completely can suitably change or change and combine according to method provided by the invention, realize this technology in conjunction with the embodiments.It should be noted that, all these are by technical process provided by the invention being carried out to similar change or change and being reconfigured, apparent to those skilled in the art, are all regarded as in spirit of the present invention, scope and content.

Claims (7)

1. an energy-saving process method for hexanaphthene-tetrahydrobenzene-benzene separation, it be the mixture that contains hexanaphthene, tetrahydrobenzene, benzene be raw material, by extracting rectifying, operate separating benzene-cyclohexane, tetrahydrobenzene and benzene, it is characterized in that comprising following step:
(1) at least comprise extractive distillation column, benzene recovery tower and tetrahydrobenzene recovery tower;
(2) annexation between extractive distillation column A, extractive distillation column B, extractive distillation column C is: in extractive distillation column A, be provided with dividing plate extractive distillation column A is divided into Shang Ta and lower tower two portions, and gas-liquid is not communicated with mutually; The upper tower tower reactor gas-phase feed of extractive distillation column A is extractive distillation column B and extractive distillation column C top gaseous phase; Extractive distillation column B and extractive distillation column C tower top liquid phase feeding are the upper tower tower reactor liquid of extractive distillation column A; Extractive distillation column B and extractive distillation column C tower reactor gas-phase feed are column overhead gas phase under extractive distillation column A; Under extractive distillation column A, column overhead liquid phase feeding is extractive distillation column B and extractive distillation column C tower reactor liquid;
(3) the upper tower of extractive distillation column A completes the separated of hexanaphthene and tetrahydrobenzene, and the tower top of extractive distillation column A obtains the hexanaphthene that purity is qualified; Under extractive distillation column A, tower completes the separated of tetrahydrobenzene and benzene, and tower reactor discharging is benzene and solvent, containing hexanaphthene and tetrahydrobenzene;
(4) in extractive distillation column B, complete benzene separated with hexanaphthene, complete the separated of a part of tetrahydrobenzene and benzene simultaneously, in the discharging of extractive distillation column B top gaseous phase, only contain hexanaphthene, tetrahydrobenzene and solvent, containing benzene; In the discharging of extractive distillation column B tower reactor liquid phase, only contain tetrahydrobenzene, benzene and solvent, not containing hexanaphthene;
(5) extractive distillation column C top completes the completely separated of hexanaphthene and tetrahydrobenzene, and bottom completes the completely separated of tetrahydrobenzene and benzene, the solvent-laden tetrahydrobenzene of middle part side line extraction;
(6) charging of tetrahydrobenzene recovery tower is the solvent-laden tetrahydrobenzene of extractive distillation column C middle part side line extraction, and tetrahydrobenzene recovery tower tower top obtains the tetrahydrobenzene product that purity is qualified;
(7) charging of benzene recovery tower is tower tower reactor discharging under extractive distillation column A, and benzene recovery tower tower top obtains the benzaldehyde product that purity is qualified; Benzene recovery tower tower reactor material is as circulating solvent, through heat exchange, after cooling, returns to the upper tower solvent discharging of extractive distillation column A position.
2. according to the said processing method of claim 1, it is characterized in that in step (3), solvent enters the middle and upper part of the upper tower of extractive distillation column A; In step (4), mixing raw material enters extractive distillation column B middle and upper part.
3. according to the said processing method of claim 1, it is characterized in that said extractive distillation column C middle part side-stream is the gaseous stream from extractive distillation column C middle and lower part; Or from the liquid phase stream of extractive distillation column C middle and lower part; Or a part is that gaseous stream, another part from extractive distillation column C middle and lower part is the liquid phase stream from extractive distillation column C middle and lower part.
4. according to the said processing method of claim 1, it is characterized in that said tetrahydrobenzene recovery tower tower reactor material returns to extractive distillation column C lateral line discharging position, or extractive distillation column C tower reactor material is carried out to holomorphosis, tetrahydrobenzene recovery tower tower reactor material is returned to position, the upper tower middle and upper part of extractive distillation column A.
5. according to the said processing method of claim 1, it is characterized in that said extractive distillation column B and extractive distillation column C arrange respectively intermediate reboiler, use and heat compared with low-grade heat source.
6. according to the said processing method of claim 1, it is characterized in that by top of tower under extractive distillation column A, drawing one gas phase removes benzene recovery tower, this burst of gas phase, both as the charging of benzene recovery tower, again as benzene recovery tower tower reactor thermal source, can be saved benzene recovery tower tower reactor reboiler simultaneously.
7. according to the said processing method of claim 1, it is characterized in that the ratio range of said extractive distillation column solvent load and hexanaphthene, tetrahydrobenzene, benzene mixing raw material amount is 2~8: 1.
CN201210041613.0A 2012-02-23 2012-02-23 Energy-saving process method for separating cyclohexane-cyclohexene-benzene Expired - Fee Related CN102617262B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201210041613.0A CN102617262B (en) 2012-02-23 2012-02-23 Energy-saving process method for separating cyclohexane-cyclohexene-benzene

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201210041613.0A CN102617262B (en) 2012-02-23 2012-02-23 Energy-saving process method for separating cyclohexane-cyclohexene-benzene

Publications (2)

Publication Number Publication Date
CN102617262A CN102617262A (en) 2012-08-01
CN102617262B true CN102617262B (en) 2014-04-09

Family

ID=46557536

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201210041613.0A Expired - Fee Related CN102617262B (en) 2012-02-23 2012-02-23 Energy-saving process method for separating cyclohexane-cyclohexene-benzene

Country Status (1)

Country Link
CN (1) CN102617262B (en)

Families Citing this family (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN103864554B (en) * 2014-04-09 2015-09-30 天津市昊永化工科技有限公司 The method of separation of extractive distillation alkane, alkene and aromatic hydrocarbons from hydrocarbon mixture
CN106518598A (en) * 2016-10-09 2017-03-22 大连理工大学 Device and method for purifying n-hexane with N,N-dimethylacetamide solvent
CN108586216A (en) * 2018-01-23 2018-09-28 山东亚科环保科技有限公司 A kind of process of effectively refining cyclohexanone by-product hexamethylene
CN109438167B (en) * 2018-12-27 2024-04-12 成都科特瑞兴科技有限公司 Cyclohexene energy-saving production system and production method
CN114560749A (en) * 2022-02-23 2022-05-31 杭州浥能科技有限公司 Method for extracting, rectifying and separating cyclohexene three times

Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1157811A (en) * 1995-10-20 1997-08-27 三菱化学株式会社 Method for separating cyclohexene
CN101796001A (en) * 2007-09-05 2010-08-04 旭化成化学株式会社 Method of separating cyclohexene and production process

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1157811A (en) * 1995-10-20 1997-08-27 三菱化学株式会社 Method for separating cyclohexene
CN101796001A (en) * 2007-09-05 2010-08-04 旭化成化学株式会社 Method of separating cyclohexene and production process

Also Published As

Publication number Publication date
CN102617262A (en) 2012-08-01

Similar Documents

Publication Publication Date Title
CN102617262B (en) Energy-saving process method for separating cyclohexane-cyclohexene-benzene
CN104027995B (en) The method of Separation of Benzene, ethylbenzene, many ethylbenzene, heavy constituent mixing system
CN108101748B (en) Four-tower three-effect methanol rectification energy-saving process method and device
CN101050159B (en) Method for separating butane and butylenes, and dedicated installation
CN104528647A (en) Method and device for preparing hydrogen and high-purity carbon monoxide by separating synthetic gas
CN108610229B (en) Light hydrocarbon separation system and method
CN105837394A (en) Purifying method of highly-pure 1,2,3-trimethylbenzene
CN203007175U (en) Heat integration device for methanol synthesis and rectification
CN106336337A (en) Method for separating toluene and n-propanol azeotrope through heat-integrated pressure-swing distillation
CN103694088B (en) The separation method of ethylene glycol mixture system
CN103449950A (en) Method and system for recycling ethylene in tail gas through barren liquor effect in demethanization process
CN109646980B (en) Fusel-free oil dividing wall tower coupled methanol multi-effect rectification energy-saving device and method
US4778566A (en) Energy-saving circuit for continuously operated distillation units
CN113233960B (en) Multi-effect methanol rectification process method and device for avoiding ethanol accumulation
CN204932917U (en) Extractive distillation device in a kind of hydrofining process of crude benzene
CN104624022B (en) Biabsorption is bilingual to inhale hydrogen and lighter hydrocarbons comprehensive recovery system
CN103896702B (en) Light hydrocarbon separation method and system from middle precut of fraction
CN204702504U (en) A kind of synthetic gas is separated hydrogen making and high-purity CO device
CN104591952A (en) Method for refining mesitylene by virtue of differential pressure thermal coupling rectification
CN204455032U (en) The device of recovering of vaporized hydrocarbons and extraction regenerated methanol
CN108046974B (en) System and method for separating benzene, cyclohexane and cyclohexene
CN103664460B (en) System and method for preparing 1,3-pentadiene (PD) and dicyclopentadiene (DCPD)
CN110553463A (en) Energy-saving optimization system and process of HyCO cryogenic separation device
CN102924212B (en) Solvent composition for separating mesitylene by extractive distillation and extractive distillation method
CN215906119U (en) Multi-effect methanol rectification process method device for avoiding ethanol accumulation

Legal Events

Date Code Title Description
C06 Publication
PB01 Publication
C10 Entry into substantive examination
SE01 Entry into force of request for substantive examination
C14 Grant of patent or utility model
GR01 Patent grant
C41 Transfer of patent application or patent right or utility model
TR01 Transfer of patent right

Effective date of registration: 20160824

Address after: 300193 Tianjin, Nankai District, building A floor, block 12

Patentee after: Tianjin New Tianjin Technology and Development Co., Ltd.

Address before: 300193, Nankai District, Tianjin pure building A block 12 (Yangtze River Road and Nanfeng road junction southeast side) Tianjin Xintian Technology Development Co., Ltd.

Patentee before: Lan Renshui

Patentee before: Huang Guiming

CF01 Termination of patent right due to non-payment of annual fee
CF01 Termination of patent right due to non-payment of annual fee

Granted publication date: 20140409

Termination date: 20210223