CN1125008C - Process for recovering arylhydrocarbon by combination of extracting distillation with liquid-liquid extraction - Google Patents
Process for recovering arylhydrocarbon by combination of extracting distillation with liquid-liquid extraction Download PDFInfo
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- 238000000034 method Methods 0.000 title claims abstract description 73
- 238000000638 solvent extraction Methods 0.000 title claims abstract description 62
- 238000000622 liquid--liquid extraction Methods 0.000 title claims abstract description 61
- 238000004821 distillation Methods 0.000 title claims abstract description 26
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims abstract description 222
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 claims abstract description 57
- 238000000895 extractive distillation Methods 0.000 claims abstract description 56
- 239000000203 mixture Substances 0.000 claims abstract description 28
- 229930195733 hydrocarbon Natural products 0.000 claims abstract description 19
- 150000002430 hydrocarbons Chemical class 0.000 claims abstract description 19
- 239000004215 Carbon black (E152) Substances 0.000 claims abstract description 17
- 239000002904 solvent Substances 0.000 claims description 121
- 238000011084 recovery Methods 0.000 claims description 44
- 150000004945 aromatic hydrocarbons Chemical class 0.000 claims description 30
- 238000000605 extraction Methods 0.000 claims description 22
- 238000005194 fractionation Methods 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 10
- HXJUTPCZVOIRIF-UHFFFAOYSA-N sulfolane Chemical group O=S1(=O)CCCC1 HXJUTPCZVOIRIF-UHFFFAOYSA-N 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 5
- 239000002994 raw material Substances 0.000 abstract description 26
- 125000003118 aryl group Chemical group 0.000 abstract description 22
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 abstract description 21
- 239000008096 xylene Substances 0.000 abstract description 15
- 238000005265 energy consumption Methods 0.000 abstract description 8
- 238000004508 fractional distillation Methods 0.000 abstract 1
- 238000007670 refining Methods 0.000 abstract 1
- 239000006184 cosolvent Substances 0.000 description 11
- 238000010992 reflux Methods 0.000 description 7
- 238000000926 separation method Methods 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 5
- 238000000197 pyrolysis Methods 0.000 description 5
- 230000008929 regeneration Effects 0.000 description 5
- 238000011069 regeneration method Methods 0.000 description 5
- 239000007789 gas Substances 0.000 description 4
- 229940078552 o-xylene Drugs 0.000 description 4
- 238000004064 recycling Methods 0.000 description 4
- 230000000694 effects Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- FYGHSUNMUKGBRK-UHFFFAOYSA-N 1,2,3-trimethylbenzene Chemical compound CC1=CC=CC(C)=C1C FYGHSUNMUKGBRK-UHFFFAOYSA-N 0.000 description 2
- URLKBWYHVLBVBO-UHFFFAOYSA-N Para-Xylene Chemical group CC1=CC=C(C)C=C1 URLKBWYHVLBVBO-UHFFFAOYSA-N 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- 239000011280 coal tar Substances 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- IVSZLXZYQVIEFR-UHFFFAOYSA-N m-xylene Chemical group CC1=CC=CC(C)=C1 IVSZLXZYQVIEFR-UHFFFAOYSA-N 0.000 description 2
- LCEDQNDDFOCWGG-UHFFFAOYSA-N morpholine-4-carbaldehyde Chemical compound O=CN1CCOCC1 LCEDQNDDFOCWGG-UHFFFAOYSA-N 0.000 description 2
- UOHMMEJUHBCKEE-UHFFFAOYSA-N prehnitene Chemical compound CC1=CC=C(C)C(C)=C1C UOHMMEJUHBCKEE-UHFFFAOYSA-N 0.000 description 2
- 150000003457 sulfones Chemical class 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- 150000003738 xylenes Chemical class 0.000 description 2
- WKFQMDFSDQFAIC-UHFFFAOYSA-N 2,4-dimethylthiolane 1,1-dioxide Chemical compound CC1CC(C)S(=O)(=O)C1 WKFQMDFSDQFAIC-UHFFFAOYSA-N 0.000 description 1
- PPDFQRAASCRJAH-UHFFFAOYSA-N 2-methylthiolane 1,1-dioxide Chemical compound CC1CCCS1(=O)=O PPDFQRAASCRJAH-UHFFFAOYSA-N 0.000 description 1
- 150000001335 aliphatic alkanes Chemical class 0.000 description 1
- 125000003545 alkoxy group Chemical group 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 125000003710 aryl alkyl group Chemical group 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 150000001924 cycloalkanes Chemical class 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 150000002334 glycols Chemical class 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 125000004435 hydrogen atom Chemical class [H]* 0.000 description 1
- 238000006317 isomerization reaction Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000463 material Substances 0.000 description 1
- 231100000989 no adverse effect Toxicity 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
Description
本发明为一种抽提蒸馏-液液抽提组合工艺，适用于从烃类混合物中回收高纯度芳烃产品。The invention is an extractive distillation-liquid-liquid extraction combined process, which is suitable for recovering high-purity aromatic products from hydrocarbon mixtures.
目前，从催化重整油或裂解加氢汽油等烃类混合物中分离芳烃的传统方法主要有液液抽提法和抽提蒸馏法。液液抽提工艺能以较高收率获得高纯度苯、甲苯和二甲苯(BTX)产品。但现有的液液抽提工艺适于处理芳含30～70重％的原料。对于芳含大于75重％甚至达到80～90重％的原料则易出现原料与溶剂混溶的现象，需要用大量非芳烃产品与原料混兑使芳烃含量降至70重％以维持抽提塔的正常操作，而原料混兑降低了过程的分离效率、装置处理能力，也增加了过程的能耗，有时还会因混兑不均匀出现操作不稳。而抽提蒸馏是利用溶剂对烃类各组分相对挥发度影响的不同而从烃类混合物中分离芳烃的方法，无须进行原料混兑。较适于从窄馏份油中回收单一芳烃产品，而难以在同一个抽提蒸馏系列中同时获得高纯度的BTX产品。一般而言，抽提蒸馏工艺较之液液抽提工艺的芳烃收率为低，两种处理方法各有所长，并具有一定的互补性，所以将二者结合在一起的组合工艺得到发展。At present, the traditional methods for separating aromatics from hydrocarbon mixtures such as catalytic reformed oil or pyrolysis hydrogenated gasoline mainly include liquid-liquid extraction and extractive distillation. The liquid-liquid extraction process can obtain high-purity benzene, toluene and xylene (BTX) products in a relatively high yield. However, the existing liquid-liquid extraction process is suitable for processing raw materials with an aromatic content of 30-70% by weight. For raw materials with an aromatic content greater than 75% by weight or even 80-90% by weight, miscibility of raw materials and solvents is likely to occur, and a large amount of non-aromatic products and raw materials need to be mixed to reduce the content of aromatics to 70% by weight to maintain the extraction tower. The normal operation of the process, but the mixing of raw materials reduces the separation efficiency of the process, the processing capacity of the device, and also increases the energy consumption of the process, and sometimes the operation is unstable due to uneven mixing. Extractive distillation is a method of separating aromatics from hydrocarbon mixtures by using the difference in the influence of solvents on the relative volatility of each component of hydrocarbons, without the need for raw material mixing. It is more suitable for recovering a single aromatic product from narrow fraction oil, but it is difficult to obtain high-purity BTX product in the same extractive distillation series at the same time. Generally speaking, the yield of aromatics in the extractive distillation process is lower than that of the liquid-liquid extraction process. The two treatment methods have their own strengths and have certain complementarities. Therefore, the combined process combining the two has been developed. .
US3723256提出了一种抽提蒸馏-液液抽提的组合工艺。其做法是先将原料进行预分馏，切割成苯馏份和C8芳烃馏份。苯馏份进入抽提蒸馏段，得到含苯和溶剂的第一物流和第一非芳烃馏份。C8芳烃馏份进入液液抽提段得到含芳烃的溶剂萃取相和含非芳烃的抽余相，所得抽提相再进入汽提段进行处理，得到含芳烃和溶剂的第二馏份以及第二非芳烃馏份。将上述处理得到的第一和第二非芳烃馏份再返回液液抽提段，将含芳烃的第二馏份和含苯的第一馏份引入溶剂回收段，分离溶剂和芳烃，其中回收溶剂分两股从回收段的不同位置引出，其中的一股流入抽提蒸馏段，另一股流入液液抽提段。该方法将抽提蒸馏和液液抽提工艺结合，并采用一个溶剂回收塔，较适于处理芳含大于75重％的原料，同时以较高收率获得高纯BTX。但该法适用于新建装置，且操作能耗未有显著降低，不适用于对炼厂中现有的液液抽提装置进行大幅度扩能改造。US3723256 proposes a combined process of extractive distillation-liquid-liquid extraction. The method is to pre-fractionate the raw materials and cut them into benzene fractions and C 8 aromatic fractions. The benzene fraction enters the extractive distillation section to obtain a first stream containing benzene and solvent and a first non-aromatic fraction. The C8 aromatic fraction enters the liquid-liquid extraction section to obtain an aromatic-containing solvent extraction phase and a non-aromatic-containing raffinate phase, and the resulting extraction phase enters a stripping section for processing to obtain a second fraction containing aromatics and a solvent and Second non-aromatic fraction. Return the first and second non-aromatic fractions obtained from the above treatment to the liquid-liquid extraction section, introduce the second fraction containing aromatics and the first fraction containing benzene into the solvent recovery section, separate the solvent and aromatics, and recover The solvent is drawn from different positions in the recovery section in two streams, one of which flows into the extraction distillation section, and the other flows into the liquid-liquid extraction section. The method combines extractive distillation and liquid-liquid extraction technology, and adopts a solvent recovery tower, which is more suitable for processing raw materials with an aromatic content of more than 75% by weight, and simultaneously obtains high-purity BTX with a relatively high yield. However, this method is suitable for new equipment, and the operating energy consumption has not been significantly reduced, and it is not suitable for large-scale expansion and transformation of the existing liquid-liquid extraction equipment in the refinery.
US3844902提出的抽提蒸馏-液液抽提组合工艺将预分馏与抽提蒸馏合并在一个抽提蒸馏塔中进行，即在抽提蒸馏过程中将原料分离成重质芳烃和轻芳烃两种物流，再用抽提蒸馏法将重质芳烃与非芳组分分离，然后含重质芳烃的溶剂进溶剂回收塔以使重质芳烃与溶剂分离，在回收塔顶得到甲苯和二甲苯的混合物，回收溶剂再返回抽提蒸馏塔。抽提蒸馏过程产生的非芳烃和轻芳烃冷却后进入抽提塔进行液液抽提，塔顶得非芳烃，塔底富含芳烃的溶剂则经汽提塔、溶剂回收塔得到轻芳烃，轻芳烃为苯和甲苯的混合物。由于不设预分馏，直接在抽提蒸馏塔中将轻质芳烃与重质芳烃分离，在此过程中大量的轻质芳烃需要经过蒸馏排出抽提蒸馏塔，然后再进入液液抽提进行液相抽提，再经过汽提蒸馏和溶剂回收等蒸馏处理才能得到纯芳烃产品，且仍为混合物，要得到纯苯还需进一步的精馏。显然上述工艺操作需要多次蒸发轻质芳烃，较适于处理轻芳烃含量低而重芳烃含量高的原料。对于裂解加氢汽油及煤焦油这类轻芳烃含量很高的原料，由于需对轻芳烃进行多次蒸发及使用液液抽提分离轻芳烃，将造成操作能耗的增加。The extractive distillation-liquid-liquid extraction combined process proposed by US3844902 combines pre-fractionation and extractive distillation in an extractive distillation tower, that is, the raw material is separated into two streams of heavy aromatics and light aromatics during the extractive distillation process , and then use extractive distillation to separate heavy aromatics from non-aromatic components, then the solvent containing heavy aromatics enters the solvent recovery tower to separate heavy aromatics from the solvent, and a mixture of toluene and xylene is obtained at the top of the recovery tower, The recovered solvent is returned to the extractive distillation column. The non-aromatics and light aromatics produced in the extractive distillation process are cooled and enter the extraction tower for liquid-liquid extraction. The non-aromatics are obtained at the top of the tower, and the solvent rich in aromatics at the bottom of the tower is passed through the stripping tower and the solvent recovery tower to obtain light aromatics. Aromatics are mixtures of benzene and toluene. Since there is no pre-fractionation, the light aromatics are directly separated from the heavy aromatics in the extractive distillation tower. In this process, a large amount of light aromatics need to be distilled out of the extractive distillation tower, and then enter the liquid-liquid extraction for liquid extraction. Phase extraction, and then distillation treatment such as stripping distillation and solvent recovery can obtain pure aromatic products, and they are still mixtures. Further rectification is required to obtain pure benzene. Apparently, the above-mentioned process requires repeated evaporation of light aromatics, which is more suitable for processing raw materials with low content of light aromatics and high content of heavy aromatics. For raw materials with a high content of light aromatics such as pyrolysis hydrogenated gasoline and coal tar, the operation energy consumption will increase due to the need to evaporate the light aromatics multiple times and use liquid-liquid extraction to separate the light aromatics.
本发明的目的是提供一种能够直接分离得到纯苯，并能同时回收甲苯和二甲苯的抽提蒸馏-液液抽提组合工艺。该工艺能耗、物耗较低，芳烃收率高。The purpose of the present invention is to provide a kind of extractive distillation-liquid-liquid extraction combination process that can directly separate and obtain pure benzene, and can recover toluene and xylene at the same time. The process has low energy consumption and material consumption and high yield of aromatics.
本发明利用同一芳烃选择性溶剂在抽提蒸馏和液液抽提中的选择性不同的特点，采用抽提蒸馏-液液抽提组合工艺对原料中轻馏份和重馏份分别进行抽提蒸馏和液液抽提处理。在抽提蒸馏单元溶剂回收塔塔顶直接获得合格苯产品，在液液抽提单元回收塔处获得高纯度的甲苯和苯。The present invention utilizes the characteristics of different selectivities of the same aromatic hydrocarbon selective solvent in extractive distillation and liquid-liquid extraction, and adopts the combination process of extractive distillation-liquid-liquid extraction to extract light fractions and heavy fractions in raw materials respectively. Distillation and liquid-liquid extraction processing. Qualified benzene products are directly obtained at the top of the solvent recovery tower of the extraction and distillation unit, and high-purity toluene and benzene are obtained at the recovery tower of the liquid-liquid extraction unit.
本发明所述的方法包括如下步骤：Method of the present invention comprises the steps:
(1)将烃类混合物进行预分馏，得到苯浓度为60.0～95.0重％的第一馏份和苯浓度为0.5～30.0重％的第二馏份；(1) Pre-fractionating the hydrocarbon mixture to obtain a first fraction with a benzene concentration of 60.0 to 95.0% by weight and a second fraction with a benzene concentration of 0.5 to 30.0% by weight;
(2)将第一馏份送入抽提蒸馏塔，用芳烃选择性溶剂溶解其中的苯得到富含苯的溶剂，将该富含苯的溶剂送入抽提蒸馏溶剂回收塔使芳烃选择性溶剂与苯分离，从该回收塔底得到的贫溶剂返回抽提蒸馏塔顶；(2) Send the first fraction into the extractive distillation tower, dissolve the benzene therein with the aromatic hydrocarbon selective solvent to obtain a solvent rich in benzene, send the solvent rich in benzene into the extractive distillation solvent recovery tower to make the aromatic hydrocarbon selective The solvent is separated from benzene, and the lean solvent obtained from the bottom of the recovery tower is returned to the top of the extraction distillation tower;
(3)将所述的第二馏份和(2)步中抽提蒸馏塔顶排出的抽余油混合后送入液液抽提塔，用芳烃选择性溶剂溶解其中的芳烃得到富含芳烃的溶剂，将富含芳烃的溶剂送入汽提塔，汽提塔上部排出的物流，即回流芳烃返回液液抽提塔，汽提塔下部排出的含芳烃的溶剂进入液液抽提溶剂回收塔，在该回收塔顶部得到纯芳烃，回收塔底排出的贫溶剂返回液液抽提塔顶。(3) After mixing the raffinate oil discharged from the top of the extractive distillation tower in the second cut and (2) step, it is sent into the liquid-liquid extraction tower, and the aromatic hydrocarbons therein are dissolved with an aromatic hydrocarbon selective solvent to obtain rich aromatic hydrocarbons The solvent rich in aromatics is sent to the stripping tower, and the stream discharged from the upper part of the stripping tower, that is, the reflux aromatics returns to the liquid-liquid extraction tower, and the aromatics-containing solvent discharged from the lower part of the stripping tower enters the liquid-liquid extraction solvent for recovery Tower, the pure aromatics are obtained at the top of the recovery tower, and the poor solvent discharged from the bottom of the recovery tower is returned to the top of the liquid-liquid extraction tower.
所述方法中，预分馏分出的第一馏份主要为含有非芳烃的苯馏份；第二馏份主要为苯和甲苯的混合馏份，其中苯的含量较少，预分馏分出的重组分从体系中排出，主要为含二甲苯的物质，可用作碳八芳烃异构化原料。In the method, the first cut out of the pre-fractionation is mainly the benzene cut containing non-aromatics; the second cut is mainly the mixed cut of benzene and toluene, wherein the content of benzene is less, and the pre-fractionation out Heavy components are discharged from the system, mainly xylene-containing substances, which can be used as raw materials for isomerization of C8 aromatics.
上述预分馏的操作条件最好控制在使所得第一馏份中苯浓度为70.0～95.0重％；第二馏份中苯浓度为0.5～15.0重％，最好为2.0～10.0重％。The operating conditions of the above-mentioned pre-fractionation are preferably controlled so that the benzene concentration in the obtained first fraction is 70.0-95.0% by weight; the benzene concentration in the second fraction is 0.5-15.0% by weight, preferably 2.0-10.0% by weight.
为增加环丁砜对非芳烃的溶解能力，提高抽提蒸馏过程中的苯回收率和缓和溶剂回收的操作苛刻度，本发明在步骤(2)所述的抽提蒸馏中，在芳烃选择性溶剂中加入C8～C10的芳烃作为助溶剂。助溶剂选自C8～C10芳烃中的任意一种或它们的混合物，如对二甲苯、邻二甲苯、间二甲苯、三甲苯或四甲苯，优选的助溶剂为二甲苯。所述助溶剂在芳烃选择性溶剂中的含量为0.1～15.0重％，最好为3.0～8.0重％。In order to increase the solubility of sulfolane to non-aromatic hydrocarbons, improve the operating severity of benzene recovery rate and ease solvent recovery in the extractive distillation process, the present invention in the extractive distillation described in step (2), in the aromatic hydrocarbon selective solvent C 8 -C 10 aromatic hydrocarbons are added as auxiliary solvents. The co-solvent is selected from any one of C 8 -C 10 aromatic hydrocarbons or a mixture thereof, such as p-xylene, o-xylene, m-xylene, trimethylbenzene or tetramethylbenzene, and the preferred co-solvent is xylene. The content of the auxiliary solvent in the aromatic hydrocarbon selective solvent is 0.1-15.0% by weight, preferably 3.0-8.0% by weight.
本发明方法所用烃类混合物中芳烃的含量为60.0～98.0重％，最好是选用苯含量为30.0～90.0重％的烃类混合物。The content of aromatics in the hydrocarbon mixture used in the method of the present invention is 60.0-98.0% by weight, preferably a hydrocarbon mixture with a benzene content of 30.0-90.0% by weight.
本发明方法将烃类混合物经过预分馏分成两个馏份后，将第一馏份进行抽提蒸馏操作，抽提蒸馏操作产生的非芳烃组份，即抽余油与第二馏份混合后进行液液抽提操作。抽提蒸馏与液液抽提操作所使用的溶剂为同一种物质，但各自独立，互不相混用，这样液液抽提操作溶剂中可含有微量水以提高分离效率，适宜的水含量为0.3～1.0重％。抽提蒸馏溶剂中不含水，以避免影响向纯苯的质量以及溶剂溶解性降低导致的芳烃分离效率变差。In the method of the present invention, after the hydrocarbon mixture is pre-fractionated into two fractions, the first fraction is subjected to an extractive distillation operation, and the non-aromatic components produced by the extractive distillation operation, that is, after the raffinate is mixed with the second fraction Perform liquid-liquid extraction. The solvent used in extractive distillation and liquid-liquid extraction is the same substance, but they are independent and not mixed with each other. In this way, the liquid-liquid extraction solvent can contain a small amount of water to improve the separation efficiency. The suitable water content is 0.3 ~1.0% by weight. The extractive distillation solvent does not contain water, so as to avoid affecting the quality of pure benzene and reducing the solubility of the solvent to reduce the separation efficiency of aromatics.
本发明所用的芳烃选择性溶剂可选自砜类、甘醇类或N-甲酰基吗啉，所述的砜类具有的通式表达式为：式中R1、R2、R3、R4分别选自氢、C1～C10的烷基、C7～C12的芳烷基、C1～C8的烷氧基。较为优选的溶剂是环丁砜、2-甲基环丁砜或2，4-二甲基环丁砜，最为优选的溶剂为环丁砜。The aromatic hydrocarbon selective solvent used in the present invention can be selected from sulfones, glycols or N-formylmorpholine, and the general formula expression that described sulfones have is: In the formula, R 1 , R 2 , R 3 , and R 4 are respectively selected from hydrogen, C 1 -C 10 alkyl, C 7 -C 12 aralkyl, and C 1 -C 8 alkoxy. The more preferred solvent is sulfolane, 2-methylsulfolane or 2,4-dimethylsulfolane, and the most preferred solvent is sulfolane.
下面的附图有利于对本发明的进一步理解。The following drawings are helpful for further understanding of the present invention.
图1为本发明组合工艺的流程示意图。Figure 1 is a schematic flow diagram of the combined process of the present invention.
图2为采用抽提蒸馏工艺回收苯的流程示意图。Figure 2 is a schematic flow chart of recovering benzene by extractive distillation process.
由图1可知，烃类混合物经管线1从中下部进入预分馏塔2，预分馏塔2可选用一个普通蒸馏塔，在塔顶得到含苯的第一馏份，在塔中部得到含少量苯的第二馏份，塔底得混合二甲苯；预分馏也可采用两个蒸馏塔相互串连，串连的塔一个为苯馏份切割塔，另一个为脱庚烷塔，这样则在苯馏份切割塔塔顶获得含苯的第一馏份，在脱庚烷塔塔顶获得含少量苯的第二馏份，塔底获得混合二甲苯。预分馏分出的混合二甲苯经管线15排出装置。As can be seen from Fig. 1, the hydrocarbon mixture enters the pre-fractionation tower 2 from the middle and lower part through the pipeline 1, and the pre-fractionation tower 2 can be selected as a common distillation tower to obtain the first fraction containing benzene at the top of the tower, and obtain the fraction containing a small amount of benzene in the middle of the tower. The second distillate, mixed xylene at the bottom of the tower; pre-fractionation can also adopt two distillation towers connected in series, one of the towers connected in series is a benzene fraction cutting tower, and the other is a deheptanizer, so that in the benzene distillation The first fraction containing benzene is obtained at the top of the cutting tower, the second fraction containing a small amount of benzene is obtained at the top of the deheptanizer, and the mixed xylenes are obtained at the bottom of the tower. The pre-fractionated mixed xylenes are discharged from the unit through line 15.
预分馏塔2塔顶蒸出的含苯的气相第一馏份由管线3排出，经冷凝后由中部进入抽提蒸馏塔4，芳烃选择性溶剂由管线10从塔顶进入抽提蒸馏塔4，塔顶轻组分主要为非芳烃组分，由管线6排出，塔底富溶剂经管线8由中部进入抽提蒸馏溶剂回收塔9。该回收塔9塔顶气相经冷凝器11冷凝后进入贮罐12，不凝性气体由管线14排出，苯产品从贮罐12排出，一部分回流入回收塔9，另一部分由管线13排出，回收塔9塔底得到的贫溶剂由管线10返回抽提蒸馏塔4顶部。The first fraction of the benzene-containing gas phase evaporated from the top of the pre-fractionation tower 2 is discharged from the pipeline 3, and enters the extraction distillation tower 4 from the middle after being condensed, and the aromatic hydrocarbon selective solvent enters the extraction distillation tower 4 from the tower top through the pipeline 10 , the light components at the top of the tower are mainly non-aromatic components, which are discharged from the pipeline 6, and the rich solvent at the bottom of the tower enters the extractive distillation solvent recovery tower 9 through the middle part through the pipeline 8. The gas phase at the top of the recovery tower 9 enters the storage tank 12 after being condensed by the condenser 11, the non-condensable gas is discharged from the pipeline 14, the benzene product is discharged from the storage tank 12, part of it flows back into the recovery tower 9, and the other part is discharged through the pipeline 13 for recovery. The lean solvent obtained at the bottom of column 9 is returned to the top of extractive distillation column 4 through line 10 .
预分馏塔2侧线切割得到的第二馏份，主要为含少量苯的甲苯馏份，由抽提蒸馏塔侧线5排出，与抽提蒸馏塔顶管线6排出的非芳烃组分混合后经管线7进入液液抽提塔16的中下部，液液抽提的抽余相，主要为非芳烃物质由塔顶管线30排出，抽提相为含芳烃的溶剂，由塔底部排出经管线17送入汽提塔18的顶部，经过汽提蒸馏，气相组分经冷凝后由管线19排出进入贮罐20，再从贮罐20排出作为回流芳烃经管线21返回至液液抽提塔16的底部，以进一步回收该物流中所含有的芳烃。汽提塔18底部排出的含芳烃的富溶剂经管线22进入液液抽提溶剂回收塔23的中部，该回收塔23顶部排出的物流，经冷凝器25冷却后进入贮罐26，从贮罐26排出的流出物为甲苯及少量苯的纯芳烃，一部分由管线28回流入回收塔23，另一部分由管线29排出系统。由管线29排出的纯芳烃可经过进一步精馏分离苯和甲苯，图1中未标出。由回收塔23底部排出的贫溶剂经管线24返回液液抽提塔的顶部循环利用。The second fraction obtained by cutting the side line of the pre-fractionation tower 2 is mainly the toluene fraction containing a small amount of benzene, which is discharged from the side line 5 of the extractive distillation tower, mixed with the non-aromatic components discharged from the overhead line 6 of the extractive distillation tower, and then passed through the pipeline 7 enters the middle and lower part of the liquid-liquid extraction tower 16, the raffinate phase of the liquid-liquid extraction is mainly non-aromatic substances and is discharged from the tower top pipeline 30, and the extraction phase is a solvent containing aromatic hydrocarbons, which is discharged from the bottom of the tower and sent through the pipeline 17. Enter the top of the stripping tower 18, after stripping and distillation, the gas phase components are discharged from the pipeline 19 into the storage tank 20 after being condensed, and then discharged from the storage tank 20 as reflux aromatics and return to the bottom of the liquid-liquid extraction tower 16 through the pipeline 21 , to further recover the aromatics contained in this stream. The rich solvent containing aromatics discharged from the bottom of the stripping tower 18 enters the middle part of the liquid-liquid extraction solvent recovery tower 23 through the pipeline 22, and the stream discharged from the top of the recovery tower 23 enters the storage tank 26 after being cooled by the condenser 25, and is discharged from the storage tank The effluent discharged from 26 is pure aromatics of toluene and a small amount of benzene, a part flows back into the recovery tower 23 through the pipeline 28, and the other part is discharged from the system through the pipeline 29. The pure aromatics discharged from line 29 can be further rectified to separate benzene and toluene, not shown in FIG. 1 . The lean solvent discharged from the bottom of the recovery tower 23 is returned to the top of the liquid-liquid extraction tower through the pipeline 24 for recycling.
上述流程中，抽提蒸馏溶剂回收塔9底部回收的贫溶剂应有一部分送溶剂再生塔再生，另一部分返回抽提蒸馏塔2顶循环利用。同样，液液抽提溶剂回收塔23底部回收的贫溶剂也应有一部分送溶剂再生塔再生，另一部分返回液液抽提塔16顶部循环利用。所述的溶剂再生操作是本领域技术人员所熟知的，图1中未标出。In the above process, part of the poor solvent recovered from the bottom of the extractive distillation solvent recovery tower 9 should be sent to the solvent regeneration tower for regeneration, and the other part should be returned to the top of the extractive distillation tower 2 for recycling. Similarly, part of the poor solvent recovered at the bottom of the liquid-liquid extraction solvent recovery tower 23 should be sent to the solvent regeneration tower for regeneration, and the other part should be returned to the top of the liquid-liquid extraction tower 16 for recycling. The solvent regeneration operation is well known to those skilled in the art, and is not shown in FIG. 1 .
在应用本发明所述的组合工艺时，各塔操作参数为：预分馏塔2为常压蒸馏操作，其塔顶温度控制在70～85℃，塔底温度控制在105～155℃，塔侧线第二馏份引出口的温度为90～120℃。抽提蒸馏塔4塔顶操作压力为0.1～0.3MPa，溶剂与第一馏份质量流量之比，即溶剂比控制在2.0～5.5，溶剂入塔温度为80～130℃，为提高分离效率溶剂中最好含0.1～15.0重％，优选含3.0～8.0重％的C8～C10芳烃作为助溶剂。抽提蒸馏溶剂回收塔9塔顶操作压力为0.040～0.1MPa，富溶剂入塔温度125～180℃。液液抽提塔16中溶剂与第二馏份质量流量比为3.0～5.0，回流芳烃与第二馏份质量流量之比为0.5～0.8，液液抽提溶剂含水量为0.3～0.8重％，入塔温度为60～100℃，塔顶操作压力控制在0.7～0.8MPa。进入汽提塔18的富溶剂入塔温度为100～120℃，汽提塔18底部操作压力控制在0.18～0.35MPa，该塔中溶剂与芳烃质量流量之比为0.5～0.7。液液抽提溶剂回收塔23中汽提水与溶剂量之比为0.020～0.040，塔底操作压力为0.06～0.09MPa，塔底操作温度165～180℃。When applying the combined process described in the present invention, the operating parameters of each tower are: the pre-fractionation tower 2 is an atmospheric distillation operation, the tower top temperature is controlled at 70-85°C, the tower bottom temperature is controlled at 105-155°C, and the tower side line The temperature of the second fraction outlet is 90-120°C. The operating pressure at the top of the extractive distillation tower 4 is 0.1-0.3 MPa, the ratio of the mass flow rate of the solvent to the first fraction, that is, the solvent ratio is controlled at 2.0-5.5, and the temperature of the solvent entering the tower is 80-130°C. In order to improve the separation efficiency, the solvent It is best to contain 0.1-15.0% by weight, preferably 3.0-8.0% by weight, of C 8 -C 10 aromatic hydrocarbons as co-solvents. The operating pressure at the top of the extraction distillation solvent recovery tower 9 is 0.040-0.1 MPa, and the temperature of the rich solvent entering the tower is 125-180°C. The mass flow ratio of the solvent to the second fraction in the liquid-liquid extraction tower 16 is 3.0-5.0, the mass flow ratio of the reflux aromatics to the second fraction is 0.5-0.8, and the water content of the liquid-liquid extraction solvent is 0.3-0.8% by weight , The temperature entering the tower is 60-100°C, and the operating pressure at the top of the tower is controlled at 0.7-0.8 MPa. The temperature of the rich solvent entering the stripping tower 18 is 100-120° C., the operating pressure at the bottom of the stripping tower 18 is controlled at 0.18-0.35 MPa, and the mass flow ratio of the solvent to aromatics in the tower is 0.5-0.7. The ratio of stripping water to solvent in the liquid-liquid extraction solvent recovery tower 23 is 0.020-0.040, the operating pressure at the bottom of the tower is 0.06-0.09 MPa, and the operating temperature at the bottom of the tower is 165-180°C.
本发明方法适合于从含苯30重％以上的高苯含量的烃类混合物中回收BTX。特别适用于从裂解加氢汽油、煤焦油等原料中回收芳烃，并可直接得到苯产品。The method of the invention is suitable for recovering BTX from the hydrocarbon mixture with high benzene content containing more than 30% by weight of benzene. It is especially suitable for recovering aromatics from raw materials such as pyrolysis hydrogenated gasoline and coal tar, and can directly obtain benzene products.
本发明提出的组合工艺在常规的液液抽提工艺中增设抽提蒸馏单元，仅需增加少量设备即可将其改造成适于从高苯含量的烃类中回收BTX的装置。在组合工艺中，由于抽提蒸馏单元的存在，液液抽提单元的负荷大大降低，苯和水的蒸发量减少，因此可大幅度降低能耗，同时降低溶剂耗量。本发明的组合工艺可同时回收苯、甲苯和二甲苯，与单纯的液液抽提工艺或与USP3844902公开的组合工艺相比，可在保证产品纯度和芳烃收率的情况下，进一步降低能耗。The combination process proposed by the present invention adds an extraction distillation unit to the conventional liquid-liquid extraction process, and only needs to add a small amount of equipment to transform it into a device suitable for recovering BTX from hydrocarbons with high benzene content. In the combined process, due to the existence of the extractive distillation unit, the load of the liquid-liquid extraction unit is greatly reduced, and the evaporation of benzene and water is reduced, so the energy consumption can be greatly reduced, and the solvent consumption can be reduced at the same time. The combined process of the present invention can recover benzene, toluene and xylene at the same time. Compared with the simple liquid-liquid extraction process or the combined process disclosed in USP3844902, it can further reduce energy consumption while ensuring product purity and aromatics yield .
下面通过实例进一步说明本发明，但本发明并不限于此。The present invention is further illustrated by examples below, but the present invention is not limited thereto.
实例中抽提蒸馏塔、抽提蒸馏溶剂回收塔、液液抽提塔、汽提塔、液液抽提溶剂回收塔的设计及操作根据原料组成及处理量由过程模拟软件计算给出。The design and operation of extractive distillation tower, extractive distillation solvent recovery tower, liquid-liquid extraction tower, stripping tower, and liquid-liquid extraction solvent recovery tower are calculated by process simulation software according to raw material composition and processing capacity.
实例1Instance 1
本实例采用本发明组合工艺从烃类混合物中同时回收BTX。This example adopts the combined process of the present invention to simultaneously recover BTX from the hydrocarbon mixture.
以裂解加氢汽油为原料，环丁砜为溶剂，采用本发明的组合工艺同时回收BTX。所用原料组成、预分馏后第一馏份和第二馏份组成及流量见表1，各塔操作条件见表2，回收产品质量及装置总消耗指标见表3。Using pyrolysis hydrogenated gasoline as raw material and sulfolane as solvent, BTX is simultaneously recovered by adopting the combined process of the present invention. The composition of the raw materials used, the composition and flow rate of the first fraction and the second fraction after pre-fractionation are shown in Table 1, the operating conditions of each tower are shown in Table 2, and the quality of recovered products and the total consumption index of the device are shown in Table 3.
实例2Example 2
本实例按照实例1的组合工艺方法从裂解加氢汽油中回收BTX。不同的是在抽提蒸馏溶剂中加入邻二甲苯作为助溶剂，邻二甲苯在溶剂中的含量为4.5重％。各塔操作条件见表2，回收产品质量及消耗指标见表3。This example reclaims BTX from pyrolysis hydrogenated gasoline according to the combined process method of Example 1. The difference is that o-xylene is added as a co-solvent in the extraction and distillation solvent, and the content of o-xylene in the solvent is 4.5% by weight. The operating conditions of each tower are shown in Table 2, and the recovered product quality and consumption indicators are shown in Table 3.
由表2可知，在抽提蒸馏溶剂中加入助溶剂后，抽提蒸馏塔的操作压力和温度得到缓和。液液抽提塔的进料量降低，液液抽提单元负荷因之下降。由表3数据可知，加入助溶剂对回收产品质量无不良影响。It can be known from Table 2 that after adding a co-solvent to the extractive distillation solvent, the operating pressure and temperature of the extractive distillation tower are eased. The feed rate of the liquid-liquid extraction tower is reduced, and the load of the liquid-liquid extraction unit is therefore reduced. From the data in Table 3, it can be seen that the addition of co-solvent has no adverse effect on the quality of the recovered product.
对比例1Comparative example 1
采用常规的液液抽提工艺回收芳烃，即先采用预分馏塔将原料分离成二甲苯含量为0.1重％的第一馏份和二甲苯含量为99.0重％的第二馏份，然后将第二馏份排出体系，第一馏份送入液液抽提塔，经过抽提、汽提和溶剂回收步骤得到高纯度的苯和甲苯。液液抽提工艺所用原料同实例1，各塔操作条件及回收芳烃质量分别见表2、表3。Aromatics is recovered by a conventional liquid-liquid extraction process, that is, a pre-fractionator is used to separate the raw material into a first fraction with a xylene content of 0.1% by weight and a second fraction with a xylene content of 99.0% by weight, and then the second fraction with a xylene content of 99.0% by weight The second fraction is discharged from the system, the first fraction is sent to the liquid-liquid extraction tower, and high-purity benzene and toluene are obtained through the steps of extraction, stripping and solvent recovery. The raw materials used in the liquid-liquid extraction process are the same as in Example 1, and the operating conditions of each tower and the quality of recovered aromatics are shown in Table 2 and Table 3, respectively.
由表2、表3数据对比可知，本发明组合工艺的抽提蒸馏塔的溶剂比及操作温度条件适中，液液抽提部分的操作条件与单纯的液液抽提工艺基本一致。在产品质量及芳烃回收率相当的情况下，组合工艺的能耗大幅度降低，特别是蒸汽消耗可比单纯液液抽提工艺下降22％以上，抽提溶剂耗量也相应降低。From the comparison of the data in Table 2 and Table 3, it can be seen that the solvent ratio and operating temperature conditions of the extraction distillation tower of the combined process of the present invention are moderate, and the operating conditions of the liquid-liquid extraction part are basically consistent with the simple liquid-liquid extraction process. In the case of equivalent product quality and aromatics recovery rate, the energy consumption of the combined process is greatly reduced, especially the steam consumption can be reduced by more than 22% compared with the simple liquid-liquid extraction process, and the extraction solvent consumption is also reduced accordingly.
实例3Example 3
本实例说明在抽提蒸馏溶剂中加入助溶剂的效果。This example illustrates the effect of adding a co-solvent to an extractive distillation solvent.
采用图2所示的抽提蒸馏流程回收苯。图2中烃原料由管线1进入预分馏塔2，塔顶分馏出的苯含量为86.0重％的第一馏份由管线3进入抽提蒸馏塔4，塔底的苯含量为0.5重％的第二馏份由管线15排出体系。第一馏份经过抽提蒸馏后，非芳烃由管线6排出，含苯的富溶剂从塔底排出经管线8送至溶剂回收塔9，回收塔顶流出物经冷凝器11冷却后进入贮罐12，其中轻组分由管线14排出，苯产品由管线13排出，塔底贫溶剂由管线10送回抽提蒸馏塔顶循环利用。所述流程中各塔操作条件同组合工艺中的抽提蒸馏部分。The extractive distillation process shown in Figure 2 is used to recover benzene. Among Fig. 2, the hydrocarbon raw material enters the pre-fractionating tower 2 from the pipeline 1, and the first fraction with a benzene content of 86.0% by weight enters the extractive distillation tower 4 through the pipeline 3, and the benzene content at the bottom of the tower is 0.5% by weight. The second fraction exits the system via line 15. After the first fraction is extracted and distilled, the non-aromatic hydrocarbons are discharged from the pipeline 6, and the rich solvent containing benzene is discharged from the bottom of the tower and sent to the solvent recovery tower 9 through the pipeline 8, and the recovered tower top effluent is cooled by the condenser 11 and then enters the storage tank 12, wherein the light components are discharged from the pipeline 14, the benzene product is discharged from the pipeline 13, and the poor solvent at the bottom of the tower is sent back to the top of the extractive distillation tower for recycling through the pipeline 10. The operating conditions of each tower in the flow process are the same as the extractive distillation part in the combined process.
采用实例1所述的裂解加氢汽油为原料，以环丁砜为溶剂，溶剂中含6.0重％的助溶剂邻二甲苯，用图2所示的抽提蒸馏工艺回收单一的苯产品。分离效果见表4。表4中同时列出了与本实例流程及操作条件相同，但不含助溶剂的对比例2的分离效果数据。Adopt the cracking hydrogenated gasoline described in example 1 as raw material, take sulfolane as solvent, contain 6.0% by weight co-solvent o-xylene in the solvent, reclaim single benzene product with the extractive distillation process shown in Fig. 2. The separation effect is shown in Table 4. Table 4 also lists the separation effect data of Comparative Example 2 that is the same as the flow process and operating conditions of this example, but does not contain a cosolvent.
由表4可知，在抽提蒸馏溶剂中加入助溶剂后，贫溶剂的苯含量和抽余油中的苯含量均有显著下降，特别是抽余油中的苯含量降到1.0重％以下。It can be seen from Table 4 that after adding co-solvent to the extractive distillation solvent, the benzene content of the poor solvent and the benzene content in the raffinate all have a significant decrease, especially the benzene content in the raffinate drops below 1.0% by weight.
表1
表3
*指包括预分馏、抽提、产品精馏在内的全过程工艺消耗。表4
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| CN113943586A (en) * | 2020-07-17 | 2022-01-18 | 中国石油天然气集团有限公司 | Method for removing aromatic hydrocarbon in straight-run naphtha |
| CN111995490A (en) * | 2020-09-03 | 2020-11-27 | 唐山旭阳化工有限公司 | Hydrogenated oil separation equipment and method |
| CN117343758B (en) * | 2022-06-28 | 2025-05-13 | 中国石油化工股份有限公司 | Method for separating aromatic hydrocarbon from gasoline C6+ fraction |
| CN115193082B (en) * | 2022-09-16 | 2022-12-30 | 旭阳工程有限公司 | Crude benzene hydrofining separation process |
-
2000
- 2000-02-01 CN CN 00100477 patent/CN1125008C/en not_active Expired - Lifetime
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103305260A (en) * | 2012-03-16 | 2013-09-18 | 中国石油化工股份有限公司 | System and method for reducing viscosity of quenching oil of ethylene unit |
| CN103305260B (en) * | 2012-03-16 | 2015-10-07 | 中国石油化工股份有限公司 | A kind of system and method reducing ethylene unit quenching oil viscosity |
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| CN1262264A (en) | 2000-08-09 |
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