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CN102180760B - Method for preparing benzene-free heptane solvent - Google Patents

Method for preparing benzene-free heptane solvent Download PDF

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CN102180760B
CN102180760B CN 201110070163 CN201110070163A CN102180760B CN 102180760 B CN102180760 B CN 102180760B CN 201110070163 CN201110070163 CN 201110070163 CN 201110070163 A CN201110070163 A CN 201110070163A CN 102180760 B CN102180760 B CN 102180760B
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heptane
removal
heavy
light
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CN102180760A (en
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张殿明
李荣忠
谢海鹰
朱彦斌
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Beijing Yanshan Jilian Petroleum Chemical Co ltd
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BEIJING YANSHAN JILIAN PETROLEUM CHEMICAL Co Ltd
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Abstract

本发明公开了一种制备无苯庚烷溶剂的方法,包括如下步骤:(1)脱除轻组分:己烷抽提后的切割油进入脱轻塔,从塔顶脱去轻组分,塔釜流出液为脱除轻组分后的粗庚烷;(2)脱除重组分:经步骤(1)脱除重组分后的粗庚烷进入脱重塔,从塔顶采集得到脱除重组分的粗庚烷,塔釜排出液为含中重组分的混合液;(3)催化加氢:将步骤(2)中脱除重组分后的粗庚烷经加氢反应器发生催化加氢反应将芳烃转化成烷烃,反应液经分离罐分离后的气体进入冷凝器进行冷凝,冷凝后的液体为无苯庚烷溶剂。本发明工艺简单,可工业化生产,庚烷收率达到80%以上,填补国内(环保)工业规模化生产无苯庚烷溶剂的空白;产生较好的经济效益和社会效益。The invention discloses a method for preparing a benzene-heptane-free solvent, which comprises the following steps: (1) removing light components: cutting oil after hexane extraction enters a light removal tower, and removes light components from the top of the tower, The effluent from the tower is the crude heptane after removing the light components; (2) Removing the heavy components: the crude heptane after the heavy components are removed in step (1) enters the heavy removal tower, and is collected from the top of the tower to remove The crude heptane of the heavy component, the liquid discharged from the tower kettle is a mixed liquid containing the medium and heavy component; (3) Catalytic hydrogenation: the crude heptane after removing the heavy component in step (2) is catalytically added to the hydrogenation reactor The hydrogen reaction converts aromatics into alkanes, and the gas separated from the reaction liquid by the separation tank enters the condenser for condensation, and the condensed liquid is a benzene-heptane-free solvent. The invention has a simple process, can be industrialized, and has a heptane yield of more than 80%, which fills the gap in domestic (environmental protection) industrial scale production of benzene-heptane-free solvents; and produces better economic and social benefits.

Description

一种制备无苯庚烷溶剂的方法A kind of method for preparing phenylheptane solvent

技术领域 technical field

本发明涉及一种制备无苯庚烷溶剂的方法,属于化工生产领域。 The invention relates to a method for preparing a benzene-heptane-free solvent, which belongs to the field of chemical production.

背景技术 Background technique

系列(环保)正庚烷溶剂,是一种应用极为广泛的工业溶剂。目前,我国只能少量生产含芳烃庚烷溶剂,随着石油化工、医药,食品工业的不断发展,这种工业级溶剂的某些性能已不能满足需要,开发系列(含量不同)环保绿色无苯正庚烷溶剂,增加产品品种,提高产品等级是我们企业一项刻不容缓的任务,这也是市场经济下提高企业竞争能力有效途径。 Series (environmentally friendly) n-heptane solvent, which is an extremely widely used industrial solvent. At present, my country can only produce a small amount of aromatic-containing heptane solvents. With the continuous development of petrochemical, pharmaceutical and food industries, some properties of this industrial-grade solvent can no longer meet the needs. The development of series (different content) environmental protection green benzene-free It is an urgent task for our company to increase product varieties and improve product grades for n-heptane solvents. This is also an effective way to improve the competitiveness of enterprises under the market economy.

发明内容 Contents of the invention

本发明要解决的技术问题是克服现有的缺陷,提供了一种工艺简单、可工业规模化生产、环保无苯的备无苯庚烷溶剂的方法。 The technical problem to be solved by the present invention is to overcome the existing defects and provide a method for preparing a benzene-heptane solvent with simple process, industrial scale production, environmental protection and benzene-free.

为了解决上述技术问题,本发明提供了如下的技术方案: In order to solve the problems of the technologies described above, the present invention provides the following technical solutions:

一种制备无苯庚烷溶剂的方法,以己烷抽提后的切割油为原料,包括如下步骤: A method for preparing solvent-free phenylheptane, using cutting oil after hexane extraction as raw material, comprising the steps of:

(1)脱除轻组分:己烷抽提后的切割油进入脱轻塔,使釜温维持在104±2℃,塔顶温度控制在98±2℃,从塔顶脱去轻组分,轻组分经冷凝器冷凝后一部分送至储罐,一部分送至塔顶回流,塔釜流出液为脱除轻组分后的粗庚烷; (1) Removal of light components: the cut oil after hexane extraction enters the light removal tower, maintains the temperature of the kettle at 104±2°C, controls the temperature at the top of the tower at 98±2°C, and removes the light components from the top of the tower , part of the light component is sent to the storage tank after being condensed by the condenser, and part of it is sent to the top of the tower to reflux, and the effluent from the tower kettle is crude heptane after removing the light component;

(2)脱除重组分:经步骤(1)脱除重组分后的粗庚烷进入脱重塔,控制塔釜温度132±2℃,塔顶温度120±2℃,从塔顶采集得到脱除重组分的粗庚烷,经冷凝器冷凝后一部分送至脱重塔塔顶作为回流,塔釜排出液为含中重组分的混合液; (2) Removal of heavy components: the crude heptane after removal of heavy components in step (1) enters the heavy removal tower, the temperature of the tower bottom is controlled at 132±2°C, and the temperature of the top of the tower is 120±2°C. The crude heptane that removes heavy components is sent to the top of the heavy removal tower as reflux after being condensed by the condenser, and the liquid discharged from the tower kettle is a mixed liquid containing medium and heavy components;

(3)催化加氢:将步骤(2)中脱除重组分后的粗庚烷经加氢反应器发生催化加氢反应将芳烃转化成烷烃,反应液经分离罐分离后的气体进入冷凝器进行冷凝,冷凝后的液体为无苯庚烷溶剂。 (3) Catalytic hydrogenation: The crude heptane after removal of heavy components in step (2) undergoes catalytic hydrogenation reaction in a hydrogenation reactor to convert aromatics into alkanes, and the gas separated from the reaction liquid by the separation tank enters the condenser Condensation is carried out, and the condensed liquid is a phenylheptane-free solvent.

步骤(3)中催化加氢反应采用NCG触媒作为催化剂。 The catalytic hydrogenation reaction in step (3) uses NCG catalyst as the catalyst.

进一步地,步骤(1)、步骤(2)中分别通过塔釜再沸器调节脱轻塔的塔釜的温度。 Further, in step (1) and step (2), the temperature of the tower still of the light removal tower is adjusted through the tower still reboiler respectively.

进一步地,步骤(1)中的原料己烷抽提后的切割油用脱轻塔塔釜流出液预热后再送至脱氢塔脱除轻组分。 Further, the cut oil extracted with hexane in step (1) is preheated with the effluent from the delightening tower and then sent to the dehydrogenation tower to remove light components.

进一步地,步骤(2)中通过脱重塔脱除的重组分送已烷生产车间作为生产已烷的原料。 Further, in step (2), the heavy weight removed by the deweighting tower is sent to the hexane production workshop as the raw material for hexane production.

本发明有益效果如下: The beneficial effects of the present invention are as follows:

己烷抽提后的切割油经初馏塔预处理得到的物料中正庚烷含量在25%以上,同时脱除组分中轻组分;再进一步对该物料经精馏塔处理,塔顶得到40%以上的系庚烷;该物料经精馏分离,得到质量分数为40%—90%的正庚烷,塔釜流出含中重组分混合液;经加氢反应器将芳烃转化成烷烃后,得到质量分数40—90%系列无苯庚烷溶剂成品,本发明工艺简单,可工业化生产,庚烷收率达到80%以上,填补国内(环保)工业规模化生产无苯庚烷溶剂的空白;产生较好的经济效益和社会效益。 The n-heptane content in the cut oil after hexane extraction is pretreated by the initial distillation tower is more than 25%, and the light components in the components are removed at the same time; the material is further processed by the rectification tower, and the top of the tower is obtained More than 40% is heptane; the material is separated by rectification to obtain n-heptane with a mass fraction of 40%-90%, and the mixed liquid containing medium and heavy components flows out from the tower; after the aromatics are converted into alkanes through a hydrogenation reactor , to obtain a series of benzene-heptane-free solvent products with a mass fraction of 40-90%. The process of the invention is simple and can be produced industrially. ; Generate better economic and social benefits.

附图说明 Description of drawings

附图用来提供对本发明的进一步理解,并且构成说明书的一部分,与本发明的实施例一起用于解释本发明,并不构成对本发明的限制。在附图中: The accompanying drawings are used to provide a further understanding of the present invention, and constitute a part of the description, and are used together with the embodiments of the present invention to explain the present invention, and do not constitute a limitation to the present invention. In the attached picture:

图1、图2是本发明制备无苯庚烷溶剂的方法的工艺流程图。 Fig. 1, Fig. 2 are the process flow diagrams of the method for preparing no-phenylheptane solvent of the present invention.

具体实施方式 Detailed ways

以下结合附图对本发明的优选实施例进行说明,应当理解,此处所描述的优选实施例仅用于说明和解释本发明,并不用于限定本发明。 The preferred embodiments of the present invention will be described below in conjunction with the accompanying drawings. It should be understood that the preferred embodiments described here are only used to illustrate and explain the present invention, and are not intended to limit the present invention.

实施例1Example 1

本发明中所述的制备无苯庚烷溶剂的方法生产庚烷时以已烷抽提后的切割油为原料,采用二塔精馏,一塔除轻组分,二塔脱除重组分,得到80%粗庚烷产品(含质量分数1%左右的甲苯),然后对含1%左右的甲苯粗庚烷进行在触媒作用下采用液相加氢脱除甲苯,得到80%(质量分数)的精庚烷产品。 The method for preparing benzene-free heptane solvent described in the present invention uses the cutting oil after hexane extraction as a raw material when producing heptane, adopts two towers for rectification, one tower removes light components, and the second tower removes heavy components, Obtain 80% crude heptane product (containing about 1% toluene by mass fraction), and then use liquid-phase hydrogenation to remove toluene to the crude heptane containing about 1% toluene under the action of catalyst to obtain 80% (mass fraction) of refined heptane products.

具体工艺流程如下:如图1、图2所示,图1中标号A、B、C、D的线条分别与图2中标号A、 B、C、D’的线条一一对应连接,已烷抽提后的切割油自原料罐11、12经换热器3用脱轻塔4塔底流出的塔釜液预热后,由进料泵801、802泵入脱轻塔4脱除低沸点的轻组分,塔顶蒸馏出的低沸点轻组分进入冷凝器61、62进行冷凝,未冷凝的尾气高空排放,冷凝后的轻组分进入回流罐7中,一部分轻组分经泵806泵送至储罐9中,一部分轻组分由回流泵805送回脱轻塔4塔顶回流,脱轻塔4塔釜温度控制104±2℃,塔顶温度控制在98±2℃,通过设置在脱轻塔4塔底的塔底再沸器5调节塔釜温度, 塔釜液用泵803、804泵送至脱重塔14中脱除重组分,脱重塔14釜温控制132±2℃,塔顶温度120±2℃,通过设置在塔底的塔底再沸器13调节釜温,塔顶蒸出物经冷凝器15、16冷却至40℃和20℃,分别流入回流罐24中,一部分粗庚烷使用泵812送回脱重塔14塔顶回流,一部分粗庚烷产品用泵813泵送至粗庚烷罐251、252、253中,釜液经塔釜换热器10冷却至50℃后,一部分经泵807泵送入塔底再沸器5用于调节塔内的温度,另一部分经泵808送入塔釜残液罐18中,经泵810、811输送至已烷生产车间作为石油醚产品。 The concrete technological process is as follows: as shown in Figure 1 and Figure 2, the lines of label A, B, C, D in Figure 1 are connected with the lines of label A, B, C, D' in Figure 2 in one-to-one correspondence respectively, and hexane After the extracted cutting oil is preheated from the raw material tanks 11 and 12 through the heat exchanger 3 and the tower still liquid flowing out from the bottom of the light removal tower 4, it is pumped into the light removal tower 4 by the feed pumps 801 and 802 to remove the low boiling point. The low-boiling light components distilled from the top of the tower enter the condensers 61 and 62 for condensation, the uncondensed tail gas is discharged at high altitude, the condensed light components enter the reflux tank 7, and a part of the light components pass through the pump 806 Pumped into the storage tank 9, a part of the light component is sent back to the top reflux of the light removal tower 4 by the reflux pump 805. The temperature of the bottom of the light removal tower 4 is controlled at 104±2°C, and the temperature at the top of the tower is controlled at 98±2°C. The tower bottom reboiler 5 that is arranged at the tower bottom of the light removal tower 4 adjusts the temperature of the tower kettle, and the tower kettle liquid is pumped to the weight removal tower 14 by pumps 803 and 804 to remove heavy components, and the temperature of the weight removal tower 14 is controlled at 132 ± 2°C, the temperature at the top of the tower is 120±2°C, the temperature of the kettle is adjusted through the bottom reboiler 13 installed at the bottom of the tower, and the distillate at the top of the tower is cooled to 40°C and 20°C by condensers 15 and 16, and flows into the reflux tank respectively In 24, a part of the crude heptane is sent back to the top of the weight removal tower 14 by pump 812 for reflux, and a part of the crude heptane product is pumped to the crude heptane tanks 251, 252, 253 by the pump 813, and the still liquid passes through the tower still heat exchanger After 10 is cooled to 50°C, a part is pumped into the tower bottom reboiler 5 through the pump 807 to adjust the temperature in the tower, and the other part is sent into the residual liquid tank 18 through the pump 808, and is transported to Hexane production workshop as petroleum ether product.

经脱轻塔4和脱重塔14两塔精馏后储存在粗庚烷罐251、252、253中的粗庚烷(粗庚烷中含质量分数1.2%的芳烃),用进料泵809将泵送到预热器17中,预热到140~150度,氢气由己烷车间2.8~3Mpa经减压到0.8~0.9Mpa再经流量调节到11.2NM3后与粗庚烷一起进入混合器26中充分混合后,进入加氢反应器19中,在CNG触媒的作用下,粗庚烷中芳烃加氢后转化成烷烃。反应液进入汽液分离罐20中分离后,液体经冷却器冷却后进入储罐中储中,气体经罐顶冷凝器后,进入冷却器,冷凝下来的液体溶剂油为含量80%(质量分数)的精庚烷,送至精庚烷产品罐中,不凝气体进入火炬总管。 The crude heptane stored in the crude heptane tanks 251, 252, and 253 after being rectified by the light removal tower 4 and the weight removal tower 14 (the crude heptane contains 1.2% aromatics by mass fraction) is fed by the feed pump 809 The pump is sent to the preheater 17, preheated to 140~150 degrees, the hydrogen is decompressed from 2.8~3Mpa in the hexane workshop to 0.8~0.9Mpa, and then the flow rate is adjusted to 11.2NM3, and then enters the mixer 26 together with the crude heptane After fully mixed in the crude heptane, it enters the hydrogenation reactor 19, and under the action of the CNG catalyst, the aromatics in the crude heptane are hydrogenated and converted into alkanes. After the reaction liquid enters the vapor-liquid separation tank 20 for separation, the liquid enters the storage tank after being cooled by the cooler, and the gas enters the cooler after passing through the tank top condenser, and the condensed liquid solvent oil has a content of 80% (mass fraction ) to the refined heptane product tank, and the non-condensable gas enters the flare header.

最后应说明的是:以上所述仅为本发明的优选实施例而已,并不用于限制本发明,尽管参照前述实施例对本发明进行了详细的说明,对于本领域的技术人员来说,其依然可以对前述各实施例所记载的技术方案进行修改,或者对其中部分技术特征进行等同替换。凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。 Finally, it should be noted that: the above is only a preferred embodiment of the present invention, and is not intended to limit the present invention. Although the present invention has been described in detail with reference to the foregoing embodiments, for those skilled in the art, it still The technical solutions recorded in the foregoing embodiments may be modified, or some technical features thereof may be equivalently replaced. Any modifications, equivalent replacements, improvements, etc. made within the spirit and principles of the present invention shall be included within the protection scope of the present invention.

Claims (5)

1.一种制备无苯庚烷溶剂的方法,其特征在于,以己烷抽提后的切割油为原料,包括如下步骤: 1. prepare a method for solvent-free phenylheptane, it is characterized in that, take the cutting oil after hexane extraction as raw material, comprise the steps: (1)脱除轻组分:己烷抽提后的切割油进入脱轻塔,使釜温维持在104±2℃,塔顶温度控制在98±2℃,从塔顶脱去轻组分,轻组分经冷凝器冷凝后一部分送到储罐,一部分送至塔顶回流,塔釜流出液为脱除轻组分后的粗庚烷; (1) Removal of light components: the cut oil after hexane extraction enters the light removal tower, maintains the temperature of the kettle at 104±2°C, controls the temperature at the top of the tower at 98±2°C, and removes the light components from the top of the tower , part of the light component is sent to the storage tank after being condensed by the condenser, and part of it is sent to the top of the tower for reflux, and the effluent from the tower kettle is the crude heptane after removing the light component; (2)脱除重组分:经步骤(1)脱除轻组分后的粗庚烷进入脱重塔,控制塔釜温度132±2℃,塔顶温度120±2℃,从塔顶采集得到脱除重组分的粗庚烷,经冷凝器冷凝后一部分送至脱重塔塔顶作为回流,塔釜排出液为含中重组分的混合液; (2) Removal of heavy components: the crude heptane after removal of light components in step (1) enters the weight removal tower, the temperature of the tower bottom is controlled at 132±2°C, and the temperature of the top of the tower is 120±2°C, collected from the top of the tower The crude heptane from which heavy components have been removed is condensed by a condenser and partly sent to the top of the weight removal tower as reflux, and the liquid discharged from the tower kettle is a mixed liquid containing medium and heavy components; (3)催化加氢:将步骤(2)中脱除重组分后的粗庚烷经加氢反应器发生催化加氢反应将芳烃转化烷烃,反应液经分离罐分离后的气体进入冷凝器进行冷凝,冷凝后的液体为无苯庚烷溶剂。 (3) Catalytic hydrogenation: The crude heptane after removal of heavy components in step (2) is subjected to a catalytic hydrogenation reaction in a hydrogenation reactor to convert aromatics into alkanes, and the gas separated from the reaction liquid by the separation tank enters the condenser for further processing. Condensate, and the condensed liquid is a benzene-heptane-free solvent. 2.根据权利要求1所述的制备无苯庚烷溶剂的方法,其特征在于,步骤(3)中催化加氢反应采用NCG触媒作为催化剂。 2. the method for preparing no-phenylheptane solvent according to claim 1, is characterized in that, catalytic hydrogenation reaction adopts NCG catalyst as catalyzer in step (3). 3.根据权利要求1所述的制备无苯庚烷溶剂的方法,其特征在于,步骤(1)、步骤(2)中分别通过塔釜再沸器调节脱轻塔或脱重塔的塔釜的温度。 3. the method for preparing benzene-heptane-free solvent according to claim 1, is characterized in that, in step (1), step (2), adjust the tower still of light removal tower or heavy removal tower by tower still reboiler respectively temperature. 4.根据权利要求1所述的制备无苯庚烷溶剂的方法,其特征在于,步骤(1)中的原料己烷抽提后的切割油用脱轻塔塔釜流出液预热后再送至脱轻塔脱除轻组分。 4. the method for preparing benzene-heptane-free solvent according to claim 1 is characterized in that, the cutting oil after the extraction of raw material hexane in step (1) is sent to The light removal tower removes light components. 5.根据权利要求1所述的制备无苯庚烷溶剂的方法,其特征在于,步骤(2)中通过脱重塔脱除的重组分送己烷生产车间作为生产己烷的原料。 5. The method for preparing benzene-heptane-free solvent according to claim 1, characterized in that, in step (2), the heavy fraction removed by the weight removal tower is sent to the hexane production workshop as the raw material for hexane production.
CN 201110070163 2011-03-23 2011-03-23 Method for preparing benzene-free heptane solvent Expired - Fee Related CN102180760B (en)

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