CN105837394A - Purifying method of highly-pure 1,2,3-trimethylbenzene - Google Patents
Purifying method of highly-pure 1,2,3-trimethylbenzene Download PDFInfo
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- FYGHSUNMUKGBRK-UHFFFAOYSA-N 1,2,3-trimethylbenzene Chemical compound CC1=CC=CC(C)=C1C FYGHSUNMUKGBRK-UHFFFAOYSA-N 0.000 title claims abstract description 90
- 238000000034 method Methods 0.000 title claims abstract description 49
- 238000000895 extractive distillation Methods 0.000 claims abstract description 62
- 239000002904 solvent Substances 0.000 claims abstract description 51
- 238000011084 recovery Methods 0.000 claims abstract description 39
- 239000002994 raw material Substances 0.000 claims abstract description 22
- 238000000605 extraction Methods 0.000 claims abstract description 17
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims abstract description 14
- 230000008878 coupling Effects 0.000 claims abstract description 12
- 238000010168 coupling process Methods 0.000 claims abstract description 12
- 238000005859 coupling reaction Methods 0.000 claims abstract description 12
- HXJUTPCZVOIRIF-UHFFFAOYSA-N sulfolane Chemical compound O=S1(=O)CCCC1 HXJUTPCZVOIRIF-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 5
- 230000010354 integration Effects 0.000 claims abstract 2
- PQNFLJBBNBOBRQ-UHFFFAOYSA-N indane Chemical compound C1=CC=C2CCCC2=C1 PQNFLJBBNBOBRQ-UHFFFAOYSA-N 0.000 claims description 46
- 238000010992 reflux Methods 0.000 claims description 21
- 238000009835 boiling Methods 0.000 claims description 8
- 238000009833 condensation Methods 0.000 claims description 6
- 230000005494 condensation Effects 0.000 claims description 6
- 238000012938 design process Methods 0.000 claims description 2
- DCHMYKCLUYFWCL-UHFFFAOYSA-N C1CCC2=CC=CC=C12.CC=1C(=C(C=CC1)C)C Chemical compound C1CCC2=CC=CC=C12.CC=1C(=C(C=CC1)C)C DCHMYKCLUYFWCL-UHFFFAOYSA-N 0.000 claims 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 abstract description 5
- 239000007789 gas Substances 0.000 description 9
- 239000012071 phase Substances 0.000 description 8
- 238000000926 separation method Methods 0.000 description 7
- 238000005265 energy consumption Methods 0.000 description 6
- 239000000203 mixture Substances 0.000 description 4
- 238000000746 purification Methods 0.000 description 4
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 3
- 238000005516 engineering process Methods 0.000 description 3
- 238000002360 preparation method Methods 0.000 description 3
- 238000011027 product recovery Methods 0.000 description 3
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 description 2
- 239000003849 aromatic solvent Substances 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- 238000009776 industrial production Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 238000002156 mixing Methods 0.000 description 2
- 241000402754 Erythranthe moschata Species 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000029936 alkylation Effects 0.000 description 1
- 238000005804 alkylation reaction Methods 0.000 description 1
- 239000003146 anticoagulant agent Substances 0.000 description 1
- 229940127219 anticoagulant drug Drugs 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 229940079593 drug Drugs 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 239000007792 gaseous phase Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000002407 reforming Methods 0.000 description 1
- 238000001179 sorption measurement Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 238000005292 vacuum distillation Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/005—Processes comprising at least two steps in series
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C7/00—Purification; Separation; Use of additives
- C07C7/04—Purification; Separation; Use of additives by distillation
- C07C7/05—Purification; Separation; Use of additives by distillation with the aid of auxiliary compounds
- C07C7/08—Purification; Separation; Use of additives by distillation with the aid of auxiliary compounds by extractive distillation
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Analytical Chemistry (AREA)
- Oil, Petroleum & Natural Gas (AREA)
- Water Supply & Treatment (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
本发明提供一种高纯连三甲苯的提纯方法，包括原料预处理和萃取精馏两部分，采用过程集成差压热耦合设计。预脱重塔T2塔顶为预脱轻塔T1塔底供热，萃取精馏塔T3塔顶为预脱重塔T2塔底供热，溶剂回收塔T4塔顶为萃取精馏塔T3塔底供热，溶剂回收塔T4用蒸汽供热；预脱轻塔T1、预脱重塔T2和萃取精馏塔T3塔均设置有再沸器。过程采用质量比为10～5:1的环丁砜/二甲基亚砜作萃取剂，采用集成的差压热耦合萃取精馏设计，降低设备投资和操作成本，同时提高连三甲苯的收率。该系统能够有效的从混合C9芳烃溶剂油中提取高纯的连三甲苯，使产品纯度≥99wt％，收率在92～95％之间。
The invention provides a method for purifying high-purity trimethylbenzene, which includes two parts: raw material pretreatment and extraction and rectification, and adopts process integration differential pressure thermal coupling design. The top of the pre-deweighting tower T2 supplies heat to the bottom of the pre-delightening tower T1, the top of the extractive distillation tower T3 supplies heat to the bottom of the pre-deweighting tower T2, and the top of the solvent recovery tower T4 serves as the bottom of the extractive distillation tower T3 For heat supply, the solvent recovery tower T4 uses steam for heat supply; the pre-light removal tower T1, the pre-weight removal tower T2 and the extractive distillation tower T3 are all equipped with reboilers. The process uses sulfolane/dimethyl sulfoxide with a mass ratio of 10 to 5:1 as the extraction agent, and adopts an integrated differential pressure thermal coupling extraction and rectification design to reduce equipment investment and operating costs while increasing the yield of trimethylbenzene. The system can effectively extract high-purity trimethylbenzene from mixed C9 aromatic hydrocarbon solvent oil, so that the product purity is more than 99% by weight, and the yield is between 92% and 95%.
Description
技术领域technical field
本发明涉及一种高纯连三甲苯的提纯方法，尤其涉及一种从混合C9芳烃溶剂油中提纯连三甲苯的方法。The present invention relates to a kind of purification method of high-purity trimethylbenzene, relate in particular to a kind of method of purifying trimethylbenzene from mixed C 9 aromatic hydrocarbon solvent oil.
背景技术Background technique
连三甲苯作为一种重要的医药、化工行业中间体，其在生产苯胺染料、连苯三酸，合成西藏麝香，制取血小板防凝剂等药品方面具有广泛的用途。混合C9芳烃主要来自炼油厂重整装置，其中含有的大量连三甲苯大多作为汽油的调和组分被烧掉，资源浪费严重。采用合理的分离技术获得高纯度的连三甲苯产品，对其加工利用有着重要的意义，并且能够创造巨大的经济、社会效益。目前其分离难点主要在于连三甲苯与茚满等组分的沸点相差很小，采用普通精馏很难获得高纯的连三甲苯产品。As an important intermediate in the pharmaceutical and chemical industry, trimethylbenzene is widely used in the production of aniline dyes, pyrellitic acid, the synthesis of Tibetan musk, and the preparation of platelet anticoagulants and other drugs. The mixed C 9 aromatics mainly come from the reforming unit of the refinery, and a large amount of trimethylbenzene contained in it is mostly burned as a blending component of gasoline, which is a serious waste of resources. Using reasonable separation technology to obtain high-purity trimethylbenzene products is of great significance for its processing and utilization, and can create huge economic and social benefits. At present, the separation difficulty is mainly due to the small difference in the boiling points of components such as trimethylbenzene and indane, and it is difficult to obtain high-purity trimethylbenzene products by ordinary rectification.
发明专利申请公开号CN 1900034 A“从混合C9芳烃溶剂油中提纯连三甲苯的方法”采用烷基化转换法分离提纯连三甲苯。利用该方法可获得质量分数92％以上的连三甲苯产品，但该法工艺过程复杂，经济性差，催化剂寿命短，不易于工业化生产。Invention Patent Application Publication No. CN 1900034 A "Method for Purifying Ptylene from Mixed C9 Aromatic Solvent Oil" adopts an alkylation conversion method to separate and purify pylene. Utilize this method to obtain the trimethylbenzene product of mass fraction more than 92%, but this method process is complicated, economic efficiency is poor, catalyst life is short, and industrial production is not easy.
发明专利申请公开号CN 101704706 A“从重芳烃中分离提纯连三甲苯和茚满的方法”利用吸附分离结合精密精馏法获得了质量分数不低于95％的连三甲苯产品，但该方法过程繁琐，催化剂活性低、寿命短，成本高，工业化生产困难。Invention Patent Application Publication No. CN 101704706 A "Method for Separating and Purifying Pthylene and Indane from Heavy Aromatics" uses adsorption separation combined with precision rectification to obtain a product with a mass fraction of not less than 95%. Complicated, low catalyst activity, short life, high cost, difficult industrial production.
因此，提出一种产品纯度高，过程能耗小，操作工艺简单，易于工业化的连三甲苯分离提纯工艺很有必要。Therefore, it is necessary to propose a process for separation and purification of trimethylbenzene with high product purity, low process energy consumption, simple operation process and easy industrialization.
发明内容Contents of the invention
本发明的目的在于提供一种从混合C9芳烃溶剂油中获取高纯连三甲苯的生产方法，过程采用质量比为10～5:1的环丁砜/二甲基亚砜作萃取剂，采用集成的差压热耦合萃取精馏设计，降低设备投资和操作成本，同时提高连三甲苯的收率。该系统能够有效的从混合C9芳烃溶剂油中提取高纯的连三甲苯，使产品纯度≥99wt％，收率在92～95％之间。The object of the present invention is to provide a kind of production method that obtains high-purity phenylthylene from mixing C 9 aromatic hydrocarbon solvent oil, and process adopts sulfolane/dimethyl sulfoxide that mass ratio is 10～5:1 to make extraction agent, adopts integrated difference The pressure-heat coupling extractive distillation design reduces equipment investment and operating costs while increasing the yield of trimethylbenzene. The system can effectively extract high-purity trimethylbenzene from mixed C9 aromatic hydrocarbon solvent oil, so that the product purity is more than 99% by weight, and the yield is between 92% and 95%.
本发明的技术解决方案如下：Technical solution of the present invention is as follows:
一种高纯连三甲苯的提纯方法，包括原料预处理和萃取精馏两部分，采用过程集成差压热耦合设计。A method for purifying high-purity trimethylbenzene, including two parts: raw material pretreatment and extractive distillation, adopts a process-integrated differential pressure thermal coupling design.
所述集成差压热耦合设计流程为：预脱重塔塔顶为预脱轻塔塔底供热，萃取精馏塔塔顶为预脱重塔塔底供热，溶剂回收塔塔顶为萃取精馏塔塔底供热，溶剂回收塔用蒸汽供热；预脱轻塔、预脱重塔和萃取精馏塔均设置有再沸器。The design process of the integrated differential pressure thermal coupling is as follows: the top of the pre-deweighting tower supplies heat to the bottom of the pre-delightening tower, the top of the extractive distillation tower supplies heat to the bottom of the pre-deweighting tower, and the top of the solvent recovery tower supplies heat to the bottom of the pre-deweighting tower. The heat is supplied from the bottom of the rectification tower, and the steam is used to supply heat to the solvent recovery tower; the pre-light removal tower, the pre-weight removal tower and the extractive distillation tower are all equipped with reboilers.
原料预处理部分包括预脱轻塔和预脱重塔，萃取精馏部分包括萃取精馏塔和溶剂回收塔；预脱轻塔脱除原料中比连三甲苯沸点低的组分；预脱重塔脱除比茚满沸点高的组分；萃取精馏塔增大连三甲苯和茚满的相对挥发度，脱除茚满，得到连三甲苯产品；溶剂回收塔回收萃取剂。The raw material pretreatment part includes a pre-delightening tower and a pre-deweighting tower, and the extractive distillation part includes an extractive distillation tower and a solvent recovery tower; the pre-delightening tower removes components with a lower boiling point than trimethylbenzene in the raw material; The tower removes components with a higher boiling point than indane; the extractive distillation tower increases the relative volatility of trimethylbenzene and indan to remove indan to obtain the trimethylbenzene product; the solvent recovery tower recovers the extractant.
操作方法为：待提纯的混合C9原料进入预脱轻塔的中部，脱去大部分的轻组分并损失少量的连三甲苯，预脱轻塔再沸器利用预脱重塔塔顶气相物流冷凝做为热源，经预脱轻塔再沸器换热后的塔顶冷凝液回到预脱重塔部分作为回流，部分采出；预脱轻塔塔釜脱轻后混合C9物流进入预脱重塔的中部，脱去大部分的重组分并损失少量的连三甲苯，预脱重塔再沸器利用萃取精馏塔塔顶气相物流冷凝作为热源，经预脱重塔再沸器换热后的塔顶冷凝液回到萃取精馏塔部分作为回流，部分采出；预脱重塔塔顶浓缩的连三甲苯物流进入萃取精馏塔中部，循环溶剂物流在萃取精馏塔上部加入，经萃取精馏脱除茚满，萃取精馏塔塔顶得到高纯连三甲苯产品，萃取精馏塔再沸器利用溶剂回收塔塔顶气相物流冷凝作为热源，经萃取精馏塔再沸器换热后的塔顶冷凝液回到溶剂回收塔部分作为回流，部分采出；萃取剂及茚满等重组分物流进入溶剂回收塔，溶剂回收塔塔顶得到茚满及重组分，塔底得到回收的萃取剂；回收的萃取剂与补充的新鲜萃取剂混合后返回萃取精馏塔。The operation method is: the mixed C9 raw material to be purified enters the middle part of the pre-delightening tower, most of the light components are removed and a small amount of trimethylbenzene is lost, and the reboiler of the pre-delightening tower uses the gas phase at the top of the pre-delightening tower. Stream condensation is used as a heat source, and the tower top condensate after heat exchange in the pre-light removal tower reboiler is returned to the pre-light removal tower part as reflux, and partly extracted; the mixed C9 stream enters the In the middle part of the pre-deweighting tower, most of the heavy components are removed and a small amount of trimethylbenzene is lost. The pre-deweighting tower reboiler uses the condensation of the gas phase stream at the top of the extractive distillation tower as a heat source, and passes through the pre-deweighting tower reboiler The top condensate after heat exchange is returned to the extractive distillation tower part as reflux, and part of it is extracted; the trimethylbenzene stream concentrated at the top of the pre-deweighting tower enters the middle part of the extractive distillation tower, and the circulating solvent stream is in the upper part of the extractive distillation tower Adding, removing indane through extraction and rectification, high-purity trimethylbenzene product is obtained from the top of the extractive distillation tower, the reboiler of the extractive distillation tower uses the condensation of the gas phase stream at the top of the solvent recovery tower as a heat source, and passes through the reboiler of the extractive distillation tower The condensate at the top of the tower after heat exchange is returned to the solvent recovery tower part as reflux, and part of it is extracted; the heavy components such as extractant and indane flow into the solvent recovery tower, and the top of the solvent recovery tower gets indane and heavy components, and the bottom of the tower gets Recovered extractant; the recovered extractant is mixed with replenished fresh extractant and returned to the extractive distillation column.
所述预脱轻塔塔顶操作压力5～30KPa，塔釜操作温度80～140℃，理论板数30～150，进料位置为理论板10～70，回流比20～70。The operating pressure at the top of the pre-light removal tower is 5-30KPa, the operating temperature at the bottom of the tower is 80-140°C, the number of theoretical plates is 30-150, the feeding position is 10-70 theoretical plates, and the reflux ratio is 20-70.
所述预脱重塔塔顶操作压力20～90KPa，塔釜操作温度120～190℃，理论板数40～150，进料位置为理论板20～80，回流比4～40。The operating pressure at the top of the pre-weight removal tower is 20-90KPa, the operating temperature at the bottom of the tower is 120-190°C, the number of theoretical plates is 40-150, the feeding position is 20-80 theoretical plates, and the reflux ratio is 4-40.
所述萃取精馏塔塔顶操作压力70～100KPa，塔釜温度220～280℃，理论板数100～200，原料进料位置为理论板40～120，萃取剂进料位置为理论板5～30，溶剂比5～15，回流比3～12。The operating pressure at the top of the extractive distillation tower is 70-100KPa, the temperature of the tower kettle is 220-280°C, the number of theoretical plates is 100-200, the feeding position of the raw material is 40-120 theoretical plates, and the feeding position of the extractant is 5-200 theoretical plates. 30, solvent ratio 5-15, reflux ratio 3-12.
所述溶剂回收塔塔顶操作压力70～100KPa，塔釜温度260～300℃，理论板数30～100，进料位置为理论板8～32，回流比5～20。The operating pressure at the top of the solvent recovery tower is 70-100KPa, the temperature of the tower kettle is 260-300°C, the number of theoretical plates is 30-100, the feeding position is 8-32 theoretical plates, and the reflux ratio is 5-20.
本发明通过对系统进行减压梯级精馏，降低了混合C9芳烃溶剂油原料液中混合物的沸点，增大了各组分之间的相对挥发度，降低了分离难度，提高了产品收率；过程采用差压热耦合精馏也降低了过程的能耗。本发明的精密压差热耦合萃取精馏相对于传统的精馏分离工艺，过程总能耗降低约30～50％。The present invention reduces the boiling point of the mixture in the mixed C9 aromatic hydrocarbon solvent oil raw material liquid by performing vacuum step rectification on the system, increases the relative volatility between each component, reduces the difficulty of separation, and improves the product yield ; Process using differential pressure thermal coupling rectification also reduces the energy consumption of the process. Compared with the traditional rectification and separation process, the precision differential pressure thermal coupling extractive distillation of the present invention reduces the total energy consumption of the process by about 30-50%.
本发明的优点是：The advantages of the present invention are:
(1)本发明采用精密压差热耦合萃取精馏设计，通过减压梯级精馏降低了分离难度及能耗。(1) The present invention adopts the design of precise differential pressure thermal coupling extraction and rectification, and reduces the separation difficulty and energy consumption through vacuum cascade rectification.
(2)本发明提出一种新型的萃取精馏工艺，采用新型的环丁砜/二甲基亚砜(质量比10～5:1)做混合萃取剂，可以进一步提高连三甲苯的纯度(≥99wt％)，减压操作进一步提高了连三甲苯的收率(92～95％之间)。(2) The present invention proposes a novel extraction and rectification process, adopting novel sulfolane/dimethyl sulfoxide (mass ratio 10～5:1) as a mixed extraction agent, which can further improve the purity of trimethylbenzene (≥99wt %), the decompression operation has further improved the yield of trimethylbenzene (between 92～95%).
(3)本发明采用集成精密压差热耦合梯级减压蒸馏工艺，可以大幅度降低能耗，较传统精馏工艺节能约30～50％。(3) The present invention adopts an integrated precision differential pressure thermal coupling cascade vacuum distillation process, which can greatly reduce energy consumption, and save energy by about 30-50% compared with traditional rectification processes.
附图说明Description of drawings
图1为本发明一种高纯连三甲苯提纯方法的流程示意图。Fig. 1 is a schematic flow sheet of a high-purity parathylene purification method of the present invention.
其中：in:
说明：T1预脱轻塔；T2预脱重塔；T3萃取精馏塔；T4溶剂回收塔；E1预脱轻塔再沸器；E2预脱重塔再沸器；E3萃取精馏塔再沸器；1待提纯的混合C9原料；2脱除的轻组分物流；3脱轻后混合C9物流；4预脱重塔塔顶气相物流；5经预脱轻塔再沸器换热后的塔顶冷凝液；6浓缩的连三甲苯物流；7脱除的重组分物流；8萃取精馏塔塔顶气相物流；9经预脱重塔再沸器换热后的塔顶冷凝液；10循环溶剂物流；11高纯连三甲苯产品；12萃取剂及茚满等重组分物流；13溶剂回收塔塔顶气相物流；14经萃取精馏塔再沸器换热后的塔顶冷凝液；15茚满及重组分物流；16回收的萃取剂；17补充的新鲜萃取剂。Description: T1 pre-light removal tower; T2 pre-weight removal tower; T3 extractive distillation tower; T4 solvent recovery tower; E1 pre-light removal tower reboiler; E2 pre-weight removal tower reboiler; E3 extractive distillation tower reboiler 1 mixed C 9 raw material to be purified; 2 light component stream removed; 3 mixed C 9 stream after light removal; 4 gas phase stream at the top of the pre-light removal tower; 5 heat exchange through the pre-light removal tower reboiler 6. Concentrated trimethylbenzene stream; 7. Removed heavy component stream; 8. Extraction and rectification column overhead gas phase stream; 10 circulating solvent stream; 11 high-purity trimethylbenzene product; 12 heavy component streams such as extractant and indane; 13 solvent recovery tower overhead gas phase stream; 14 tower top condensate after heat exchange by extractive distillation tower reboiler; 15 Indane and heavy fraction stream; 16 Recovered extractant; 17 Supplementary fresh extractant.
具体实施方式detailed description
下面结合本发明实施例中的附图，对本发明实施例中的技术方案进行清楚、完整地描述，显然，所描述的实施例仅仅是本发明一部分实施例，而不是全部的实施例。The technical solutions in the embodiments of the present invention will be clearly and completely described below in conjunction with the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only some of the embodiments of the present invention, not all of them.
一种从混合C9芳烃溶剂油中提取高纯连三甲苯的流程，包括原料预处理和萃取精馏两部分，涉及预脱轻塔T1、预脱重塔T2、萃取精馏塔T3和溶剂回收塔T4。其中原料预处理部分包括预脱轻塔T1和预脱重塔T2，萃取精馏部分包括萃取精馏塔T3和溶剂回收塔T4。预脱轻塔T1的目的是脱除原料中比连三甲苯沸点低的组分；预脱重塔T2的目的是脱除比茚满沸点高的组分；萃取精馏塔T3的目的是增大连三甲苯和茚满的相对挥发度，脱除茚满，得到连三甲苯产品；溶剂回收塔T4的目的是回收萃取剂。A process for extracting high-purity parathylene from mixed C9 aromatic solvent oil, including two parts: raw material pretreatment and extractive distillation, involving pre-delightening tower T1, pre-deweighting tower T2, extractive distillation tower T3 and solvent recovery tower T4. The raw material pretreatment part includes a pre-lightening tower T1 and a pre-lightening tower T2, and the extractive distillation part includes an extractive distillation tower T3 and a solvent recovery tower T4. The purpose of the pre-delightening tower T1 is to remove components with a lower boiling point than trimethylbenzene in the raw material; the purpose of the pre-deweighting tower T2 is to remove components with a higher boiling point than indane; the purpose of the extractive distillation tower T3 is to increase The relative volatility of trimethylbenzene and indan in Dalian, remove indan, and obtain the trimethylbenzene product; the purpose of the solvent recovery tower T4 is to recover the extractant.
本发明的装置如图1所示：Device of the present invention is as shown in Figure 1:
待提纯的混合C9原料1的进料管线与预脱轻塔T1中部连接，脱除的轻组分物流2的管线与预脱轻塔T1塔顶相连接，脱轻后混合C9物流3的管线与预脱重塔T2中部连接，预脱轻塔T1塔釜设置预脱轻塔再沸器E1；预脱重塔塔顶气相物流4的管线与预脱轻塔再沸器E1相连接，经预脱轻塔再沸器换热后的塔顶冷凝液5的管线与预脱重塔T2塔顶相连接，经预脱重塔T2浓缩的连三甲苯物流6的管线与萃取精馏塔T3相连接，预脱重塔T2塔釜连接脱除的重组分物流7的管线，预脱重塔T2塔釜设置预脱重塔再沸器E2；萃取精馏塔塔顶气相物流8的管线与预脱重塔再沸器E2相连接，经预脱重塔再沸器换热后的塔顶冷凝液9的管线与萃取精馏塔T3顶部相连接，循环溶剂物流10的管线与萃取精馏塔T3上部相连接，萃取精馏塔T3塔顶连接高纯连三甲苯产品11的管线，萃取剂及茚满等重组分物流12的管线与溶剂回收塔T4相连接，萃取精馏塔T3塔釜设置萃取精馏塔再沸器E3；溶剂回收塔塔顶气相物流13的管线与萃取精馏塔再沸器E3相连接，经萃取精馏塔再沸器换热后的塔顶冷凝液14的管线与溶剂回收塔T4顶部相连接，茚满及重组分物流15的管线与溶剂回收塔T4塔顶相连，回收的萃取剂16的管线与溶剂回收塔T4塔釜相连接。The feed line of the mixed C9 raw material 1 to be purified is connected to the middle part of the pre-light removal tower T1, and the pipeline of the removed light component stream 2 is connected to the top of the pre-light removal tower T1, and the mixed C9 stream 3 is removed after light removal The pipeline is connected to the middle part of the pre-delightening tower T2, and the pre-delightening tower reboiler E1 is set in the bottom of the pre-delightening tower T1; , the pipeline of the tower top condensate 5 after the heat exchange of the pre-light removal tower reboiler is connected with the pre-weight removal tower T2 tower top, and the pipeline of the trimethylbenzene stream 6 concentrated through the pre-weight removal tower T2 is connected with the extractive distillation The tower T3 is connected, and the pipeline of the heavy component stream 7 that is connected to the pre-weight removal tower T2 tower kettle is removed, and the pre-weight removal tower T2 tower kettle is provided with a pre-weight removal tower reboiler E2; The pipeline is connected with the pre-deweighting tower reboiler E2, the pipeline of the overhead condensate 9 after the heat exchange of the pre-deweighting tower reboiler is connected with the top of the extractive distillation tower T3, and the pipeline of the circulating solvent stream 10 is connected with the extraction The upper part of the rectification tower T3 is connected, the top of the extractive distillation tower T3 is connected to the pipeline of the high-purity trimethylbenzene product 11, the pipeline of the heavy component stream 12 such as extractant and indane is connected to the solvent recovery tower T4, and the extractive distillation tower T3 tower The kettle is provided with an extractive distillation tower reboiler E3; the pipeline of the solvent recovery tower overhead gas stream 13 is connected with the extractive distillation tower reboiler E3, and the tower top condensate 14 after the heat exchange of the extractive distillation tower reboiler is The pipeline of is connected with the top of the solvent recovery tower T4, the pipeline of indane and heavy component flow 15 is connected with the top of the solvent recovery tower T4, and the pipeline of the extractant 16 recovered is connected with the bottom of the solvent recovery tower T4.
整个流程采用过程集成精密压差热耦合设计，即高压塔塔顶给低压塔塔釜提供再沸热量，既降低了过程的能耗又节省了设备投资，最大限度的降低整个流程的设备投资和操作费用。The entire process adopts a process-integrated precision differential pressure thermal coupling design, that is, the top of the high-pressure column provides reboiling heat to the bottom of the low-pressure column, which not only reduces the energy consumption of the process but also saves equipment investment, and minimizes the equipment investment and cost of the entire process. operating costs.
预脱重塔T2塔顶为预脱轻塔T1塔底供热，萃取精馏塔T3塔顶为预脱重塔T2塔底供热，溶剂回收塔T4塔顶为萃取精馏塔T3塔底供热，溶剂回收塔T4用蒸汽供热。The top of the pre-deweighting tower T2 supplies heat to the bottom of the pre-delightening tower T1, the top of the extractive distillation tower T3 supplies heat to the bottom of the pre-deweighting tower T2, and the top of the solvent recovery tower T4 serves as the bottom of the extractive distillation tower T3 For heat supply, the solvent recovery tower T4 uses steam for heat supply.
物料流程如下：The material flow is as follows:
待提纯的混合C9原料1进入预脱轻塔T1的中部，脱去大部分的轻组分并损失少量的连三甲苯(物流2)，预脱轻塔再沸器E1利用预脱重塔塔顶气相物流4冷凝做为热源，经预脱轻塔再沸器换热后的塔顶冷凝液5回到预脱重塔T2部分作为回流，部分采出；预脱轻塔T1塔釜脱轻后混合C9物流3进入预脱重塔T2的中部，脱去大部分的重组分并损失少量的连三甲苯(物流7)，预脱重塔再沸器E2利用萃取精馏塔塔顶气相物流8冷凝作为热源，经预脱重塔再沸器换热后的塔顶冷凝液9回到萃取精馏塔T3部分作为回流，部分采出；预脱重塔T2塔顶浓缩的连三甲苯物流6进入萃取精馏塔T3中部，循环溶剂物流10在萃取精馏塔T3上部加入，经萃取精馏脱除茚满，萃取精馏塔T3塔顶得到高纯连三甲苯产品(物流11)，萃取精馏塔再沸器E3利用溶剂回收塔塔顶气相物流13冷凝作为热源，经萃取精馏塔再沸器换热后的塔顶冷凝液14回到溶剂回收塔T4部分作为回流，部分采出；萃取剂及茚满等重组分物流12进入溶剂回收塔T4，溶剂回收塔T4塔顶得到茚满及重组分(物流15)，塔底得到回收的萃取剂(物流16)并返回萃取精馏塔T3，补充的新鲜萃取剂由物流17实现。The mixed C9 raw material 1 to be purified enters the middle part of the pre-light removal tower T1, and most of the light components are removed and a small amount of trimethylbenzene (stream 2) is lost. The pre-light removal tower reboiler E1 utilizes the pre-light removal tower The tower top gas phase stream 4 is condensed as a heat source, and the tower top condensate 5 after heat exchange in the pre-light removal tower reboiler is returned to the pre-light removal tower T2 part as reflux, and partly extracted; Mixed C 9 stream 3 enters the middle part of pre-deweighting tower T2 after light, removes most of the heavy components and loses a small amount of trimethylbenzene (stream 7), and the pre-deweighting tower reboiler E2 utilizes the top of the extractive distillation tower The gaseous phase stream 8 is condensed as a heat source, and the tower top condensate 9 after the heat exchange of the pre-deweighting tower reboiler is returned to the extractive distillation tower T3 part as reflux, and partly extracted; The toluene stream 6 enters the middle part of the extractive distillation tower T3, and the circulating solvent stream 10 is added in the upper part of the extractive distillation tower T3, and the indane is removed through extractive distillation, and the high-purity trimethylbenzene product (stream 11) is obtained at the top of the extractive distillation tower T3, The reboiler E3 of the extractive distillation tower utilizes the condensation of the gas phase stream 13 at the top of the solvent recovery tower as a heat source, and the condensate 14 at the top of the tower after heat exchange in the reboiler of the extractive distillation tower is returned to the solvent recovery tower T4 partly as reflux, and partly recovered heavy component flow 12 such as extractant and indane enters solvent recovery tower T4, and solvent recovery tower T4 tower top obtains indane and heavy component (streamline 15), and the extraction agent (streamline 16) that obtains reclaiming at the bottom of the tower also returns extraction essence Distillation column T3, supplemented fresh extractant is realized by stream 17.
本发明为了较好的匹配各塔之间的热量，控制预脱轻塔T1塔顶操作压力5～30KPa，塔釜操作温度80～140℃，理论板数30～150，进料位置10～70(理论板)，回流比20～70；预脱重塔T2塔顶操作压力20～90KPa，塔釜操作温度120～190℃，理论板数40～150，进料位置20～80(理论板)，回流比4～40；萃取精馏塔T3塔顶操作压力70～100KPa，塔釜温度220～280℃，理论板数100～200，原料进料位置40～120(理论板)，萃取剂进料位置5～30(理论板)，溶剂比5～15，回流比3～12；溶剂回收塔T4塔顶操作压力70～100KPa，塔釜温度260～300℃，理论板数30～100，进料位置8～32(理论板)，回流比5～20。In order to better match the heat between the towers, the present invention controls the operating pressure at the top of the pre-light removal tower T1 to be 5-30KPa, the operating temperature of the tower kettle is 80-140°C, the number of theoretical plates is 30-150, and the feeding position is 10-70 (theoretical plate), reflux ratio 20-70; pre-weight removal tower T2 top operating pressure 20-90KPa, tower kettle operating temperature 120-190°C, theoretical plate number 40-150, feed position 20-80 (theoretical plate) , reflux ratio 4-40; extractive distillation column T3 tower top operating pressure 70-100KPa, tower still temperature 220-280 ℃, theoretical plate number 100-200, raw material feeding position 40-120 (theoretical plate), extractant feed The material position is 5-30 (theoretical plate), the solvent ratio is 5-15, and the reflux ratio is 3-12; the operating pressure at the top of the solvent recovery tower T4 is 70-100KPa, the temperature of the tower kettle is 260-300°C, and the number of theoretical plates is 30-100. Feed position 8-32 (theoretical plate), reflux ratio 5-20.
实施例一：Embodiment one:
原料进料量为1000kg/h，环丁砜/二甲基亚砜质量比为10:1，进料组成如下表所示：The raw material feed rate is 1000kg/h, the mass ratio of sulfolane/dimethyl sulfoxide is 10:1, and the feed composition is shown in the following table:
工艺条件如下：The process conditions are as follows:
上述工艺条件下生产的连三甲苯产品纯度为99.2％，产品回收率为：93.9％。The purity of the trimethylbenzene product produced under the above process conditions is 99.2%, and the product recovery rate is 93.9%.
实施例二：Embodiment two:
原料进料量为1200kg/h，环丁砜/二甲基亚砜质量比为8:1，进料组成如下表所示：The raw material feed rate is 1200kg/h, the mass ratio of sulfolane/dimethyl sulfoxide is 8:1, and the feed composition is shown in the following table:
工艺条件如下：The process conditions are as follows:
上述工艺条件下生产的连三甲苯产品纯度为99.3％，产品回收率为：94.4％。The purity of the trimethylbenzene product produced under the above process conditions is 99.3%, and the product recovery rate is 94.4%.
实施例三：Embodiment three:
原料进料量为1200kg/h，环丁砜/二甲基亚砜质量比为5:1，进料组成如下表所示：The raw material feed rate is 1200kg/h, the mass ratio of sulfolane/dimethyl sulfoxide is 5:1, and the feed composition is shown in the table below:
工艺条件如下：The process conditions are as follows:
上述工艺条件下生产的连三甲苯产品纯度为99.5％，产品回收率为：92.8％。The purity of the trimethylbenzene product produced under the above process conditions is 99.5%, and the product recovery rate is 92.8%.
本发明公开和提出的一种高纯连三甲苯的提纯方法，本领域技术人员可通过借鉴本文内容，适当改变条件路线等环节实现，尽管本发明的方法和制备技术已通过较佳实施例子进行了描述，相关技术人员明显能在不脱离本发明内容、精神和范围内对本文所述的方法和技术路线进行改动或重新组合，来实现最终的制备技术。特别需要指出的是，所有相类似的替换和改动对本领域技术人员来说是显而易见的，他们都被视为包括在本发明精神、范围和内容中。A kind of purification method of high-purity parathylene disclosed and proposed by the present invention can be realized by those skilled in the art by referring to the content of this article and appropriately changing the conditions and routes, although the method and preparation technology of the present invention have been described through preferred implementation examples Therefore, those skilled in the art can obviously modify or recombine the methods and technical routes described herein without departing from the content, spirit and scope of the present invention, so as to realize the final preparation technology. In particular, it should be pointed out that all similar substitutions and modifications will be obvious to those skilled in the art, and they are all considered to be included in the spirit, scope and content of the present invention.
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| CN116143578A (en) * | 2023-02-17 | 2023-05-23 | 中国天辰工程有限公司 | A solvent recovery process and system for butadiene oligomerization reaction |
| CN116143578B (en) * | 2023-02-17 | 2025-03-21 | 中国天辰工程有限公司 | A butadiene oligomerization reaction solvent recovery process and system |
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