CN103193595B - Ethylene glycol rectification device system and rectification technique in industry of producing ethylene glycol by synthesis gas - Google Patents
Ethylene glycol rectification device system and rectification technique in industry of producing ethylene glycol by synthesis gas Download PDFInfo
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- CN103193595B CN103193595B CN201310091229.6A CN201310091229A CN103193595B CN 103193595 B CN103193595 B CN 103193595B CN 201310091229 A CN201310091229 A CN 201310091229A CN 103193595 B CN103193595 B CN 103193595B
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Abstract
The invention discloses an ethylene glycol rectification device system in industry of producing ethylene glycol by synthesis gas. The ethylene glycol rectification device system comprises a primary dealcoholization tower, a secondary dealcoholization tower, an ethylene glycol refining tower, wherein the primary dealcoholization tower is connected with a hydrogenation reaction product tank by a pipeline, the secondary dealcoholization tower is connected with the primary dealcoholization tower by a pipeline, the ethylene glycol refining tower is connected with the secondary dealcoholization tower, an ethanol removal tower and a butylenes glycol removal tower which are connected by a pipeline are arranged on the pipeline between the secondary dealcoholization tower and the ethylene glycol refining tower, the top of the ethanol removal tower is connected with an ethanol tank, and the top of the butylenes glycol removal tower is connected with the butylenes glycol tank. The invention further discloses a rectification technique in industry of producing ethylene glycol by synthesis gas. According to the ethylene glycol rectification device system in industry of producing ethylene glycol by synthesis gas, the steam consumption can be reduced, the energy consumption can be saved, the purity of the methanol can be improved, the output of premium grade products can be increased, the production cost can be greatly lowered, and the enterprise benefits can be increased.
Description
Technical field
The present invention relates to ethylene glycol rectifier unit system and rectification process in the industry of synthetic gas preparing ethylene glycol.
Background technology
Ethylene glycol (EG) has another name called glycol, ethylene glycol, is a kind of important basic petrochemical organic raw material, mainly for the production of trevira, and frostproofer, unsaturated polyester resin, lubricant, softening agent nonionogenic tenside and explosive etc.At present, the method for domestic and international synthesizing glycol can be divided into petroleum law production technique and non-petroleum method production technique.
Petroleum law produces ethylene glycol technique with ethene and oxygen for raw material, and ethane via epoxyethane finally obtains ethylene glycol.At present, domestic and international large-scale ethylene glycol is produced and is all adopted this method, and this method relative skill is ripe, application is comparatively extensive.But it is comparatively large that this method this method affects fluctuation by International Petroleum Price, and in production process, water loss is excessive, is not suitable for water resources shortage area, and catalyst technology is comparatively strong to external dependency, and product by product is also more, and product recovery rate is only 88%.
Non-petroleum method production technique with coal or Sweet natural gas for raw material, after obtaining synthetic gas by methods such as Coal Chemical Industries, by direct synthesis technique or indirect synthesis technique finally obtained ethylene glycol.Direct synthesis technique is by synthetic gas one-step synthesis ethylene glycol, it is a kind of simple effective method, but this method needs very high synthesis pressure that catalyzer just can be made at high temperature to have very high activity, therefore requires higher at controlling technical method, not yet realizes industrialization at present.Synthetic gas indirect synthesis glycol method can be divided into again methyl alcohol formaldehyde synthesis method and barkite synthesis method.Wherein methyl alcohol formaldehyde method is with synthetic gas first synthesizing methanol, formaldehyde, the indirect method of resynthesis ethylene glycol, and concrete research direction can be divided into following direction again: (1) methanol dehydrogenation dimerization method; (2) dme oxidative coupling method; (3) oxyacetic acid method; (4) stiasny method; (5) formaldehyde hydroformylation method; (6) formaldehyde and methyl-formiate coupling method, but above several research direction only rests on laboratory stage at present, same and unrealized heavy industrialization.
Compared with above-mentioned coal-ethylene glycol method, barkite synthesis method (also known as oxidative coupling method) is current industrialized synthetic method, according to the resource situation of China's " oil-poor, rich coal, weak breath ", this method is Material synthesis ethylene glycol with coal, has strategic importance always and economic implications.The main raw material of barkite synthesis method is NO, CO, O2, H2, alcohols etc.Reaction principle is that NO and O2 reaction generates N2O3, N2O3 and reacts with methyl alcohol and generate methyl nitrite, obtains oxalate diester, then produce ethylene glycol through shortening under Pd catalyst action with CO oxidative coupling.This production technique by esterification, carbonylation, hydrogenation and purifying ethylene glycol totally four operations form.
Rectifying job number rectification process route (see accompanying drawing 1) in used synthetic gas preparing ethylene glycol commercial process point three towers, one-level dealcoholize column 1 and secondary dealcoholize column 2 adopt 25kg steam and adopt be negative pressure distillation operation, three towers also adopt negative pressure to carry out rectifying, the ethylene glycol solution that hydrogenation job number hydrogenation reaction generates, enter into rectifying job number, be introduced into one-level dealcoholize column 1, overhead extraction light constituent methyl alcohol, methyl alcohol turns back to methanol tank 7; The mixed solution containing ethylene glycol at the bottom of tower enters into secondary dealcoholize column 2; Secondary dealcoholize column overhead extraction mixed solution, enters methanol tank 7; Tower reactor ethylene glycol mixture enters into purifying ethylene glycol tower 5, and overhead extraction is containing the butyleneglycol mixed solution of ethylene glycol, and enter into defective ethylene glycol tank 12, tower reactor obtains salable product ethylene glycol, enters finished pot 13.Owing to carrying out rectifying under adopting high pressure 25kg steam and still containing the impurity such as more ethanol and butyleneglycol in ethylene glycol after three-tower rectification, the rectifying job number rectification process thus in used synthetic gas preparing ethylene glycol course of industrialization exists the problems such as energy consumption is high, top grade product yield poorly.
Summary of the invention
The object of this invention is to provide one and effectively can improve ethylene glycol top grade product output, greatly reduce production cost, improve ethylene glycol rectifier unit system in the synthetic gas preparing ethylene glycol industry of the performance of enterprises.
Ethylene glycol rectifier unit system in synthetic gas preparing ethylene glycol of the present invention industry, comprise the one-level dealcoholize column be connected by pipeline with hydrogenation reaction products pot, the secondary dealcoholize column being connected one-level dealcoholize column by pipeline and the purifying ethylene glycol tower connecting secondary dealcoholize column, described secondary dealcoholize column with the pipeline between purifying ethylene glycol tower is provided with the de-ethanol tower and de-butyleneglycol tower that are connected by pipeline, the tower top of described de-ethanol tower connects Ethanol tank, and the tower top of described de-butyleneglycol tower connects butyleneglycol tank.
The entrance of described de-ethanol tower is connected with the outlet of secondary dealcoholize column, and the outlet of described de-butyleneglycol tower is connected with the entrance of purifying ethylene glycol tower.
The tower top of described purifying ethylene glycol tower connects at the bottom of ethylene glycol salable product tank, still and connects ethylene glycol top grade product tank.
Described ethylene glycol salable product tank is connected to the entrance of de-butyleneglycol tower by return pipeline.
Ethylene glycol rectification process in synthetic gas preparing ethylene glycol of the present invention industry, comprises the steps:
A), the ethylene glycol mixture of hydrogenation job number hydrogenator generation, enter into rectifying job number, be introduced into one-level dealcoholize column, open the cut of 3-5kg steam atmospheric distillation from overhead extraction 65 DEG C-75 DEG C, enter into methanol tank, the mixed solution containing ethylene glycol at the bottom of tower enters into secondary dealcoholize column;
B), open the rectifying under vacuum tightness-0.04 ~-0.05MPa of 3-5kg steam and, from the cut of secondary dealcoholize column overhead extraction 42 DEG C-48 DEG C, also enter methanol tank, secondary dealcoholize column tower reactor ethylene glycol mixture enters into de-ethanol tower;
C), open the rectifying under vacuum tightness-0.04 ~-0.05MPa of 3-5kg steam and, from the cut of de-ethanol tower overhead extraction 72-78 DEG C, collect Ethanol tank, de-ethanol tower tower reactor mixed solution enters de-butyleneglycol tower;
D), under vacuum tightness-0.04 ~-0.05MPa rectifying from the cut of de-butyleneglycol column overhead extraction 145-150 DEG C, collect butyleneglycol tank, de-butyleneglycol tower tower reactor ethylene glycol liquid enters into purifying ethylene glycol tower and refines;
E), under vacuum tightness-0.04 ~-0.05MPa rectifying from the ethylene glycol of purifying ethylene glycol column overhead extraction 132-133 DEG C, collect salable product tank, and by a part of salable product ethylene glycol, return to de-butyleneglycol tower, the top grade product ethylene glycol of tower reactor extraction 142-143 DEG C, collects top grade product tank.
Rectifier unit system of the present invention adopts two-stage dealcoholize column to carry out Methanol Recovery and has additional de-ethanol tower and reclaims ethanol and de-butyleneglycol tower to collect butyleneglycol, the higher ethanol of purity and butyleneglycol can be collected with additional income, reduce costs, a salable product ethylene glycol part from the extraction of purifying ethylene glycol column overhead is returned to de-butyleneglycol tower simultaneously, improve top grade product output, also effectively reduce manufacturing cost, improve the performance of enterprises.Concrete being of beneficial effect of rectification process of the present invention:
(1) top grade product output can be improved, greatly reduce manufacturing cost, improve the performance of enterprises.
(2) one-level dealcoholize column 1, adopts atmospheric operation, cancels original steam 25kg, adopts 3kg steam, collects the most of methyl alcohol in mixed solution, not only energy efficient, and the purity that can improve methyl alcohol.Original one-level dealcoholysis is negative-pressure operation, and the present invention adopts atmospheric operation also can save the energy consumption of negative-pressure operation vacuum pump.
(3) secondary dealcoholize column 2, adopts rough vacuum operation, adopts away methyl alcohol a small amount of in mixed solution, use 25kg steam instead 3kg steam, reduce steam consumption, saved manufacturing cost.
(4) de-ethanol tower 3, adopts rough vacuum operation, reduces vapor pressure, saved energy consumption, the ethanol in overhead extraction mixed solution, can collect the higher ethanol of purity and energy additional income.
(5) de-butyleneglycol tower 4, adopts rough vacuum operation, reduces vapor pressure, saved energy consumption, the butyleneglycol that overhead extraction is qualified, additional income.
(6) the salable product ethylene glycol part from purifying ethylene glycol tower 5 overhead extraction is returned to de-butyleneglycol tower 4, improve top grade product output.
Accompanying drawing explanation
Fig. 1 is ethylene glycol rectifier unit system architecture schematic diagram in the industry of used synthetic gas preparing ethylene glycol;
Fig. 2 is ethylene glycol rectifier unit system architecture schematic diagram in synthetic gas preparing ethylene glycol of the present invention industry.
In figure: 1, one-level dealcoholize column; 2, secondary dealcoholize column; 3, de-ethanol tower; 4, de-butyleneglycol tower; 5; Purifying ethylene glycol tower; 6, hydrogenated products tank; 7, methanol tank; 8, Ethanol tank; 9, butyleneglycol tank; 10, salable product tank; 11, top grade product tank; 12, unacceptable product tank; 13, finished pot.
Embodiment
Ethylene glycol rectifier unit system in synthetic gas preparing ethylene glycol of the present invention industry, comprise the one-level dealcoholize column 1 be connected by pipeline with hydrogenation reaction products pot 6, the secondary dealcoholize column 2 being connected one-level dealcoholize column 1 by pipeline and the purifying ethylene glycol tower 5 connecting secondary dealcoholize column 2, described secondary dealcoholize column 2 with the pipeline between purifying ethylene glycol tower 5 is provided with the de-ethanol tower 3 and de-butyleneglycol tower 4 that are connected by pipeline, the tower top of described de-ethanol tower 3 connects Ethanol tank 8, and the tower top of described de-butyleneglycol tower 4 connects butyleneglycol tank 9; The entrance of described de-ethanol tower 3 is connected with the outlet of secondary dealcoholize column 2, and the outlet of described de-butyleneglycol tower 4 is connected with the entrance of purifying ethylene glycol tower 5; The tower top of described purifying ethylene glycol tower 5 connects at the bottom of salable product tank 10, still and connects top grade product tank 11; Described ethylene glycol salable product tank 10 is connected to the entrance of de-butyleneglycol tower 4 by return pipeline.
embodiment 1
In synthetic gas preparing ethylene glycol of the present invention industry, ethylene glycol rectification process is:
(1) ethylene glycol mixture (methyl alcohol 49.2% of hydrogenation job number hydrogenator generation, ethanol 0.14%, ethylene glycol 45.2%, butyleneglycol 1.0%, water 2.0%, methyl glycolate 2.46%), enter into rectifying job number, be introduced into one-level dealcoholize column 1, open 3kg steam, atmospheric distillation, from the light constituent methyl alcohol of overhead extraction 72 DEG C, enters into methanol tank 7, contains the mixed solution (methyl alcohol 16.24% of ethylene glycol at the bottom of tower, ethanol 2.9%, ethylene glycol 75.71%, butyleneglycol 1.7%, water 3.45%) enter into secondary dealcoholize column 2;
(2) open 3kg steam methyl alcohol from secondary dealcoholize column 2 overhead extraction 45 DEG C under vacuum tightness-0.045MPa, also enter methanol tank 7, secondary dealcoholize column 2 tower reactor ethylene glycol mixture (methyl alcohol 0.3%, ethanol 3.47%, ethylene glycol 91.65%, butyleneglycol 2.2%, water 2.38%) enter into de-ethanol tower 3;
(3) open 3kg steam ethanol from de-ethanol tower 3 overhead extraction 74 DEG C under vacuum tightness-0.045MPa, collect Ethanol tank 8, de-ethanol tower 3 tower reactor mixed solution (ethylene glycol 98%, other: 2%) enter de-butyleneglycol tower 4;
(4) under vacuum tightness-0.045MPa from the butyleneglycol of overhead extraction 148 DEG C, collect butyleneglycol tank 9, de-butyleneglycol tower 4 tower reactor ethylene glycol liquid (ethylene glycol 98.9%, butyleneglycol 1.10%) enters into purifying ethylene glycol tower 5 and refines;
(5) under vacuum tightness-0.045MPa from the ethylene glycol of overhead extraction 132.8 DEG C, collect salable product tank 10, and by a part of salable product ethylene glycol, return to de-butyleneglycol tower 4, the top grade product ethylene glycol (ethylene glycol 99.961% of tower reactor extraction 142.8 DEG C, butyleneglycol 0.039%), collect top grade product tank 11.
Claims (2)
1. ethylene glycol rectifier unit system in the industry of synthetic gas preparing ethylene glycol, comprise the one-level dealcoholize column (1) be connected by pipeline with hydrogenation reaction products pot (6), connect the secondary dealcoholize column (2) of one-level dealcoholize column (1) by pipeline and connect the purifying ethylene glycol tower (5) of secondary dealcoholize column (2), it is characterized in that: described secondary dealcoholize column (2) with the pipeline between purifying ethylene glycol tower (5) is provided with the de-ethanol tower (3) and de-butyleneglycol tower (4) that are connected by pipeline, the tower top of described de-ethanol tower (3) connects Ethanol tank (8), the tower top of described de-butyleneglycol tower (4) connects butyleneglycol tank (9), the entrance of described de-ethanol tower (3) is connected with the outlet of secondary dealcoholize column (2), and the outlet of described de-butyleneglycol tower (4) is connected with the entrance of purifying ethylene glycol tower (5), the tower top of described purifying ethylene glycol tower (5) connects at the bottom of salable product tank (10), still and connects top grade product tank (11), described ethylene glycol salable product tank (10) is connected to the entrance of de-butyleneglycol tower (4) by return pipeline.
2. ethylene glycol rectification process in the industry of synthetic gas preparing ethylene glycol, comprises the steps:
A), the ethylene glycol mixture of hydrogenation job number hydrogenator generation, enter into rectifying job number, be introduced into one-level dealcoholize column (1), open the cut of 3-5kg steam atmospheric distillation from overhead extraction 65 DEG C-75 DEG C, enter into methanol tank (7), the mixed solution containing ethylene glycol at the bottom of tower enters into secondary dealcoholize column (2);
B), open the rectifying under vacuum tightness-0.04 ~-0.05MPa of 3-5kg steam and, from the cut of secondary dealcoholize column (2) overhead extraction 42 DEG C-48 DEG C, also enter methanol tank (7), secondary dealcoholize column (2) tower reactor ethylene glycol mixture enters into de-ethanol tower (3);
C), open the rectifying under vacuum tightness-0.04 ~-0.05MPa of 3-5kg steam and, from the cut of de-ethanol tower (3) overhead extraction 72-78 DEG C, collect Ethanol tank (8), de-ethanol tower (3) tower reactor mixed solution enters de-butyleneglycol tower (4);
D), under vacuum tightness-0.04 ~-0.05MPa rectifying from the cut of de-butyleneglycol tower (4) overhead extraction 145-150 DEG C, collect butyleneglycol tank (9), de-butyleneglycol tower (4) tower reactor ethylene glycol liquid enters into purifying ethylene glycol tower (5) and refines;
E), under vacuum tightness-0.04 ~-0.05MPa rectifying from the ethylene glycol of purifying ethylene glycol tower (5) overhead extraction 132-133 DEG C, collect salable product tank (10), and by a part of salable product ethylene glycol, return to de-butyleneglycol tower (4), the top grade product ethylene glycol of tower reactor extraction 142-143 DEG C, collects top grade product tank (11).
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103435482B (en) * | 2013-08-06 | 2015-06-17 | 陕西煤业化工技术研究院有限责任公司 | Separation method and separation device of synthesis gas ethylene glycol product |
| CN103553877B (en) * | 2013-10-22 | 2015-06-17 | 新疆天业（集团）有限公司 | Method for rectifying ethylene glycol during production of ethylene glycol from calcium carbide furnace gas |
| CN105330514B (en) * | 2015-10-12 | 2017-06-16 | 天津衡创工大现代塔器技术有限公司 | A kind of purifying technique of synthesis gas preparing ethylene glycol |
| CN105218305B (en) * | 2015-10-12 | 2018-01-30 | 天津衡创工大现代塔器技术有限公司 | A kind of byproduct recovery process of synthesis gas preparing ethylene glycol |
| CN109956851B (en) * | 2019-04-08 | 2020-04-07 | 宁波中科远东催化工程技术有限公司 | System and method for rectifying ethylene glycol in preparation of ethylene glycol from synthesis gas |
| CN111905395A (en) * | 2019-05-07 | 2020-11-10 | 上海浦景化工技术股份有限公司 | Rectification separation system and separation process for preparing ethylene glycol from synthesis gas |
| CN112142564A (en) * | 2020-09-28 | 2020-12-29 | 合肥江新化工科技有限公司 | Device and method for improving quality of ethylene glycol product obtained by side production of ethylene glycol product tower |
| CN113148953B (en) * | 2021-04-20 | 2021-11-30 | 杭州中泰深冷技术股份有限公司 | System and method for preparing ethylene glycol from synthesis gas |
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| CN203174007U (en) * | 2013-03-21 | 2013-09-04 | 安徽淮化股份有限公司 | Ethylene glycol rectification device system in ethylene glycol production industry through synthesis gas |
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| CN101928201A (en) * | 2009-06-26 | 2010-12-29 | 上海焦化有限公司 | Purification technique for coal glycol rude products |
| CN102372596A (en) * | 2010-08-23 | 2012-03-14 | 中国石油化工股份有限公司 | Method for producing glycol product by separating synthetic gas |
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