CN105646218A - High-temperature interlock esterification carbonylation unit for synthesis gas to glycol - Google Patents
High-temperature interlock esterification carbonylation unit for synthesis gas to glycol Download PDFInfo
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- CN105646218A CN105646218A CN201510987150.0A CN201510987150A CN105646218A CN 105646218 A CN105646218 A CN 105646218A CN 201510987150 A CN201510987150 A CN 201510987150A CN 105646218 A CN105646218 A CN 105646218A
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- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
- C07C67/00—Preparation of carboxylic acid esters
- C07C67/36—Preparation of carboxylic acid esters by reaction with carbon monoxide or formates
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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention relates to a high-temperature interlock esterification carbonylation unit for synthesis gas to glycol. The unit comprises a compressor, a pre-reactor, a feed heater, a reactive rectifying column, a rectifying column condenser, a rectifying column reflux tank, a reactor heater, a carbonylation reactor, a reactor knockout drum and a dimethyl oxalate absorption tower, which form gas-phase closed loop through pipes. The nit is an improvement on an esterification carbonylation unit for synthesis gas to glycol of the prior art, various key parts are provided with additional emergency shut-off valves and emergency opening valves; when the carbonylation reactor has abnormal temperature rise, a feeding sub-line cooperating with a connection torch isolates the carbonylation reactor form the esterification carbonylation unit; a nitrogen inlet tube is used to purge the original methyl nitrite of the carbonylation reactor to prevent the continuing exothermic decomposition of methyl nitrite, so as to achieve the purpose of protecting the carbonylation reactor. The unit can effectively prevent carbonylation reactor explosion due to temperature runaway, and protect the production line and live safety of the workers.
Description
Technical field
The present invention relates to synthesis gas preparing ethylene glycol industrialized producing technology, be specifically related to a kind of esterification carbonylation unit with high temperature interlocking mechanism.
Background technology
Synthesis gas preparing ethylene glycol process route generally divides four steps to complete, and the first step is esterification, and second step is oxonation, and the 3rd step is hydrogenation reaction, and the 4th step is refining; First step esterification and second step are oxonations is a complete blood circulation, constitutes esterification carbonylation unit; In synthesis gas preparing ethylene glycol process, first the intermediate products produced are dimethyl oxalate .s, dimethyl oxalate. reaction synthesizes in oxonation device, by methyl nitrite gas and CO (carbon monoxide converter) gas, under catalyst Pd/Al2O3 effect, reaction temperature, at 120-140 ��, completes under pressure 0.4MPa; This reaction is a strong exothermal reaction, and when reaction temperature is more than 140 ��, methyl nitrite is at catalyst surface generation intensive decomposition, moment releases substantial amounts of heat, and reactor and system gas expand, and reactor there will be temperature runaway, the now original safety valve jumping up of oxonation device, due to the generation of oxonation device temperature runaway, relief valve has little time pressure release, thus being easily caused the blast that oxonation device occurs.
Conventional oxonation device explosion phenomenon can be found everywhere; as: domestic first hand synthesis gas preparing ethylene glycol enterprise Tongliao occurred oxonation device to explode; also there is the case that oxonation device temperature runaway explodes in Henan coal industry; how effectively preventing oxonation device from temperature runaway occur, protection production safety and personal security are to become problem in the urgent need to address.
Summary of the invention
The technical problem to be solved in the present invention is in that providing a kind of high temperature suitable in synthesis gas preparing ethylene glycol to interlock is esterified carbonylation unit, ensures the safe operation of synthesis gas preparing ethylene glycol production line.
It is designed with following scheme for this present invention:
A kind of high temperature suitable in synthesis gas preparing ethylene glycol is interlocked and is esterified carbonylation unit, connects and composes the compressor of gas phase closed cycle, pre-reactor, feed heater, reactive distillation column, rectifying column condenser, rectifier column reflux tank, reactor heaters, oxonation device, reactor knockout drum and dimethyl oxalate. absorption tower including passing sequentially through pipeline;
Pipeline between described compressor and pre-reactor pass sequentially through oxygen emergency stop valve and out-of-bounds oxygen cutting valve be connected with feed oxygen trachea, described oxygen emergency stop valve and out-of-bounds pipeline between oxygen cutting valve are connected with blow-down pipe by oxygen emptying valve; Pipeline between described pre-reactor and feed heater is connected with raw material dinitrogen tetroxide trachea by dinitrogen tetroxide stop valve; Pipeline between described compressor and dimethyl oxalate. absorption tower is connected to torch by gaseous mixture quck-opening valve, pipeline between described rectifier column reflux tank and reactor heaters is provided with carbonylation charging main line stop valve, pipeline between described carbonylation charging main line stop valve and rectifier column reflux tank passes sequentially through carbonylation charging by-pass quck-opening valve and gaseous mixture quck-opening valve is connected with torch, and the pipeline between described carbonylation charging main line stop valve and reactor heaters is connected to nitrogen inlet by nitrogen feed quck-opening valve.
The beneficial effects of the present invention is:
The present invention makes improvement in the esterification carbonylation unit basis of existing synthesis gas preparing ethylene glycol, emergency cut-off, emergency opening valve is set up in each key component, be connected the charging by-pass of torch when oxonation actuator temperature rise abnormity, oxonation device is isolated esterification carbonylation unit, nitrogen inlet is utilized to purge the original methyl nitrite of oxonation device, prevent methyl nitrite from continuing decomposition caused heat release, thus reaching the purpose of protection oxonation device; Can effectively stop oxonation device and blast because of temperature runaway, protect the life security of production line and workman.
Accompanying drawing explanation
Below in conjunction with accompanying drawing, the specific embodiment of the present invention is described further, wherein:
Fig. 1 is the process equipment flow chart of the present invention.
Detailed description of the invention
Interlock with reference to a kind of high temperature suitable in synthesis gas preparing ethylene glycol shown in Fig. 1 and be esterified carbonylation unit, connect and compose the compressor 10 of gas phase closed cycle, pre-reactor 1, feed heater 2, reactive distillation column 3, rectifying column condenser 4, rectifier column reflux tank 5, reactor heaters 6, oxonation device 7, reactor knockout drum 8 and dimethyl oxalate. absorption tower 9 including passing sequentially through pipeline;
The liquid-phase outlet of rectifier column reflux tank 5 is connected with the fluid inlet of reactive distillation column 3 upper end by water pump 11.
Pipeline between described compressor 10 and pre-reactor 1 pass sequentially through oxygen emergency stop valve XV102 and out-of-bounds oxygen cutting valve XV101 be connected with feed oxygen trachea, described oxygen emergency stop valve XV102 and out-of-bounds pipeline between oxygen cutting valve XV101 are connected with blow-down pipe by oxygen emptying valve XV103, pipeline between described pre-reactor 1 and feed heater 2 is connected with raw material dinitrogen tetroxide trachea by dinitrogen tetroxide stop valve XV104, pipeline between described compressor 10 and dimethyl oxalate. absorption tower 9 is connected torch by gaseous mixture quck-opening valve XV108, pipeline between described rectifier column reflux tank 5 and reactor heaters 2 is provided with carbonylation charging main line stop valve XV106, pipeline between described carbonylation charging main line stop valve XV106 and rectifier column reflux tank 5 passes sequentially through carbonylation charging by-pass quck-opening valve XV105 and gaseous mixture quck-opening valve XV108 and is connected with torch, pipeline between described carbonylation charging main line stop valve XV105 and reactor heaters 6 is connected to nitrogen inlet by nitrogen feed quck-opening valve XV107.
Work process of the present invention is as follows: monitoring temperature in oxonation device 7, when finding temperature anomaly (more than 140 ��), esterification carbonylation cellular system interlocking valve event, out-of-bounds oxygen cutting valve XV101 and oxygen emergency close valve closing XV102 closedown, cut off unstripped gas oxygen, prevent from continuing reaction, generate methyl nitrite, because methyl nitrite is primary raw material and the decomposition caused heat release material of oxonation device;Oxygen emptying valve XV103 opens, and by oxygen emptying, it is prevented that valves leakage, enters system; Dinitrogen tetroxide stop valve XV104 closes, and dinitrogen tetroxide is also esterification raw material, it is prevented that have the generation of methyl nitrite; Carbonylation charging by-pass valve XV105 opens, and allows the mixing gas containing methyl nitrite, enters oxonation device, is released to torch burning by by-pass; Nitrogen quck-opening valve XV107 opens, and opens nitrogen inlet, purges the original methyl nitrite of oxonation device with nitrogen, it is prevented that methyl nitrite continues decomposition caused heat release; Gaseous mixture quck-opening valve XV108 opens, and allows rapid blow-down in system, removes torch burning, it is prevented that the methyl nitrite in system recyclegas decomposes; Carbonylation charging main line valve XV106 closes, and does not allow system include the recyclegas of methyl nitrite, enters oxonation device, stops methyl nitrite to continue to decompose in oxonation device, it is prevented that blast occurs; Compressor being stopped, owing to compressor inlet gas is released, import does not have pressure, and parking can protect compressor simultaneously.
The above; being only the present invention preferably detailed description of the invention, but scope is not limited thereto, any those familiar with the art is in the technical scope of present disclosure; the change that can readily occur in or replacement, all should be encompassed within protection scope of the present invention. Therefore scope is as the criterion with the protection domain of claims.
Claims (1)
1. it is applicable to a high temperature interlocking esterification carbonylation unit for synthesis gas preparing ethylene glycol, connects and composes the compressor of gas phase closed cycle, pre-reactor, feed heater, reactive distillation column, rectifying column condenser, rectifier column reflux tank, reactor heaters, oxonation device, reactor knockout drum and dimethyl oxalate. absorption tower including passing sequentially through pipeline; It is characterized in that:
Pipeline between described compressor and pre-reactor pass sequentially through oxygen emergency stop valve and out-of-bounds oxygen cutting valve be connected with feed oxygen trachea, described oxygen emergency stop valve and out-of-bounds pipeline between oxygen cutting valve are connected with blow-down pipe by oxygen emptying valve; Pipeline between described pre-reactor and feed heater is connected with raw material dinitrogen tetroxide trachea by dinitrogen tetroxide stop valve; Pipeline between described compressor and dimethyl oxalate. absorption tower is connected to torch by gaseous mixture quck-opening valve, pipeline between described rectifier column reflux tank and reactor heaters is provided with carbonylation charging main line stop valve, pipeline between described carbonylation charging main line stop valve and rectifier column reflux tank passes sequentially through carbonylation charging by-pass quck-opening valve and gaseous mixture quck-opening valve is connected with torch, and the pipeline between described carbonylation charging main line stop valve and reactor heaters is connected to nitrogen inlet by nitrogen feed quck-opening valve.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510987150.0A CN105646218A (en) | 2015-12-27 | 2015-12-27 | High-temperature interlock esterification carbonylation unit for synthesis gas to glycol |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510987150.0A CN105646218A (en) | 2015-12-27 | 2015-12-27 | High-temperature interlock esterification carbonylation unit for synthesis gas to glycol |
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| CN105646218A true CN105646218A (en) | 2016-06-08 |
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| Application Number | Title | Priority Date | Filing Date |
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| CN201510987150.0A Pending CN105646218A (en) | 2015-12-27 | 2015-12-27 | High-temperature interlock esterification carbonylation unit for synthesis gas to glycol |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107056619A (en) * | 2017-02-21 | 2017-08-18 | 安阳永金化工有限公司 | Regenerator safety device is esterified for coal-ethylene glycol methyl nitrite |
| CN108261992A (en) * | 2018-01-04 | 2018-07-10 | 中石化上海工程有限公司 | Automatically switch the method for ethylene unit front-end hydrogenation reactor |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN203683424U (en) * | 2013-12-27 | 2014-07-02 | 安徽淮化股份有限公司 | Carbonylation reaction device for preventing temperature runaway in process of preparing ethylene glycol from synthesis gas |
| CN203678352U (en) * | 2013-12-27 | 2014-07-02 | 安徽淮化股份有限公司 | Safety releasing carbonylation reactor for preparing ethylene glycol from synthesis gas |
| CN104297435A (en) * | 2014-10-29 | 2015-01-21 | 安徽淮化股份有限公司 | On-line detection system for preparing ethylene glycol with synthetic gas in industrial production |
-
2015
- 2015-12-27 CN CN201510987150.0A patent/CN105646218A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN203683424U (en) * | 2013-12-27 | 2014-07-02 | 安徽淮化股份有限公司 | Carbonylation reaction device for preventing temperature runaway in process of preparing ethylene glycol from synthesis gas |
| CN203678352U (en) * | 2013-12-27 | 2014-07-02 | 安徽淮化股份有限公司 | Safety releasing carbonylation reactor for preparing ethylene glycol from synthesis gas |
| CN104297435A (en) * | 2014-10-29 | 2015-01-21 | 安徽淮化股份有限公司 | On-line detection system for preparing ethylene glycol with synthetic gas in industrial production |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107056619A (en) * | 2017-02-21 | 2017-08-18 | 安阳永金化工有限公司 | Regenerator safety device is esterified for coal-ethylene glycol methyl nitrite |
| CN107056619B (en) * | 2017-02-21 | 2019-08-02 | 安阳永金化工有限公司 | Regenerator safety device is esterified for coal-ethylene glycol methyl nitrite |
| CN108261992A (en) * | 2018-01-04 | 2018-07-10 | 中石化上海工程有限公司 | Automatically switch the method for ethylene unit front-end hydrogenation reactor |
| CN108261992B (en) * | 2018-01-04 | 2020-01-14 | 中石化上海工程有限公司 | Method for automatically switching front hydrogenation reactor of ethylene device |
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Effective date of registration: 20160826 Address after: 232038 Anhui Province, Huainan city tianjia'an District Quanshan Applicant after: Anhui Huaihua Co., Ltd. Applicant after: PUJING CHEMICAL INDUSTRY (SHANGHAI) LIMITED Address before: 232038 Anhui Province, Huainan city tianjia'an District Quanshan Applicant before: Anhui Huaihua Co., Ltd. |
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Application publication date: 20160608 |