CN102807492B - Process device for producing methyl nitrite - Google Patents
Process device for producing methyl nitrite Download PDFInfo
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- CN102807492B CN102807492B CN201210314836XA CN201210314836A CN102807492B CN 102807492 B CN102807492 B CN 102807492B CN 201210314836X A CN201210314836X A CN 201210314836XA CN 201210314836 A CN201210314836 A CN 201210314836A CN 102807492 B CN102807492 B CN 102807492B
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- fractionating tower
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- reaction fractionating
- methyl nitrite
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
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Abstract
The invention provides a process device for producing methyl nitrite. The process device comprises a reactive distillation tower, a pre-reactor, a pre-heater, a reboiler, a methanol recovering and buffering groove and an acid water groove, wherein a condenser is arranged in reactive distillation tower; the pre-reactor, the pre-heater, the reactive distillation tower, the reboiler and the methanol recovering and buffering groove are connected in sequence; the input end of the pre-reactor is connected with an NO recycle gas pipeline and an oxygen pipeline in a carbonylation reaction process respectively; the oxygen pipeline is provided with an air separating device; the two ends of a subcooler are communicated with the condenser and the reactive distillation tower respectively; one end of the subcooler is connected with a carbonylation reaction system; the input port of the acid water groove is connected with an acid water pipe and a process soft water pipe respectively; and a first circulation pump and a second circulation pump are arranged among the methanol recovering and buffering groove, the acid water groove and the reactive distillation tower respectively. The process device is simplified, production equipment is saved, the production cost is lowered, and the process device can be better applied to an ethylene glycol process.
Description
Technical field
The present invention relates to the process unit in a kind of ethylene glycol production, specifically a kind of ethylene glycol is produced the process unit of methyl nitrite in producing.
Background technology
Methyl nitrite, colourless gas.Fusing point-17 ℃.Boiling point-12 ℃.Facile hydrolysis discharges nitrous acid, producing methyl nitrite is an operation of producing in the ethylene glycol process unit, at present, the process unit of the production methyl nitrite usually adopted comprises the nitrogen tetroxide groove, nitrogen tetroxide vaporizer and technique demineralized water tank, wherein the technique demineralized water tank is stainless steel.Nitrogen tetroxide is as the raw material of manufacturing nitric acid, anhydrous metal salt and nitro co-ordination complex; In organic chemistry, be used as the inhibitor of oxygenant, nitrating agent and acrylic ester polymerization; In war industry, as producing explosive and rocket propellant, as strong oxidizer, the relevant device cost of nitrogen tetroxide is higher, and in esterification, oxygen is provided by the external world fully, and the cost accounting is high.Because tank is to utilize technique soft water to cause the waste of technique soft water, thereby cause the cost of whole production technique device to rise.
Summary of the invention
The object of the present invention is to provide a kind of process unit that can simplify the cost-saving production methyl nitrite of process unit.
The present invention has adopted following technical scheme: this device comprises reaction fractionating tower, pre-reactor, preheater, reboiler, Methanol Recovery dashpot and acid tank, described reaction fractionating tower is built-in with condenser, described pre-reactor, preheater, reaction fractionating tower, reboiler is connected successively with the Methanol Recovery dashpot, the input terminus of described pre-reactor respectively with the carbonylation reaction operation in NO circulation gas pipeline and oxygen pipeline connect, described oxygen pipeline is provided with air separation plant, the two ends of described recooler communicate with described condenser and reaction fractionating tower respectively, described recooler one end is connected with the carbonylation reaction system, described acid tank input aperture is connected with the technique hose with acid water pipe respectively, between the connection line of the output terminal of described Methanol Recovery dashpot and described acid tank output terminal and reaction fractionating tower, be respectively equipped with the first recycle pump and the second recycle pump.
Beneficial effect: the present invention has saved nitrogen tetroxide groove and nitrogen tetroxide evaporator plant, and can take full advantage of new fresh oxygen after with the alternative nitrogen tetroxide of sour water, producing methyl nitrite, has saved technique soft water, has greatly saved production cost.
The accompanying drawing explanation
Fig. 1 is syndeton schematic diagram of the present invention.
In figure: 1, nitrogen peroxide pre-reactor, 2, the nitrogen peroxide preheater, 3, reaction fractionating tower, 4, condenser, 5, reboiler, 6, the Methanol Recovery dashpot, 7, recooler, 8, acid tank, the 9, first recycle pump, 10, the second recycle pump, 11. acid water pipe, 12, the technique water pipe, 13, the NO circulating gas pipe, 14, air separation plant, 15, the carbonylation reaction system.
Embodiment
Below in conjunction with accompanying drawing, be described in further detail:
As shown in Figure 1, this device comprises nitrogen peroxide pre-reactor 1, nitrogen peroxide preheater 2, reaction fractionating tower 3, reboiler 5, Methanol Recovery dashpot 6 and acid tank 8, reaction fractionating tower 3 tower tops are built-in with condenser 4, nitrogen peroxide pre-reactor 1, nitrogen peroxide preheater 2, reaction fractionating tower 3, reboiler 4 is connected successively with Methanol Recovery dashpot 5, the input terminus of nitrogen peroxide pre-reactor 1 respectively with carbonylation reaction 15 operations in NO circulating gas pipe 13 and the oxygen pipeline of the NO circulation gas that comes of nitrogen compressor connect, oxygen pipeline is provided with air separation plant 14, outside air is isolated purity oxygen through air separation plant 14, the two ends of recooler 7 communicate with condenser 4 and reaction fractionating tower 3 respectively, recooler 7 one ends are connected with carbonylation reaction system 15, acid tank 8 input apertures are connected with technique soft water 12 pipes with acid water pipe 11 respectively, between the connection line of the output terminal of Methanol Recovery dashpot 6 and acid tank 8 output terminals and reaction fractionating tower 3, be respectively equipped with the first recycle pump 9 and the second recycle pump 10.
The chemical reaction related in working process in this process unit has: sour water is squeezed into the reaction fractionating tower middle part by pump, at lower decomposition: the 4HNO that is heated
3→ 2H
2O+4NO
2+ O
2,
1, the oxonation operation nitrogen compressor NO circulation gas come and the fresh O out-of-bounds come
2After mixing, enter nitrogen peroxide pre-reactor 1 and carry out the reaction of above-mentioned reaction formula (1): 2NO+O
2→ 2NO
2
2,Excessive NO enters reaction fractionating tower and NO
2The formula that reacts (2), NO+NO
2→ N
2O
3
3,N
2O
3The CH next with tower top
3OH liquid carries out the reaction of reaction formula (3): 2CH
3OH+N
2O
3→ 2CH
3ONO+H
2O
The working process of process unit is as follows: the NO circulation gas that nitrogen compressor comes in oxonation 15 operations is through NO circulating gas pipe 13 and out-of-bounds carry out the fresh O separated through air separation plant 14
2After mixing, enter nitrogen peroxide pre-reactor 1, then after pipeline enters nitrogen peroxide preheater 2 material is preheating to 70 ℃, gas mixture enters writing a Chinese character in simplified form of MN(methyl nitrite) bottom of reaction fractionating tower 3, this tower is pressurizing tower, working pressure is 0.3MPa, the tower head temperature is-5 ℃, at the bottom of tower, is controlled at 80 ℃.The top of reaction fractionating tower 3 adds pure methyl alcohol, sour water enters the middle part of reaction fractionating tower 3, the MN that reaction generates and unreacted other gases and part methyl alcohol are cold again by reaction fractionating tower 3 overhead condenser 4 condensations, reaction fractionating tower recooler 7, separate and remove most of methyl alcohol, the uncooled MN of containing gas is delivered to subsequent processing, i.e. the oxonation operation.And at the bottom of tower, forming 60% methanol solution, a part enters Methanol Recovery dashpot 5 and carries out self-circulation by the first recycle pump 9, improves reaction efficiency; A part directly enters lower operation to Methanol Recovery in addition, acid tank 8 tops are connected with acid water pipe 11 and technique hose 12, the normal sour water that uses, technique soft water can be used as supplementary, utilize process unit of the present invention to produce nitrous acid, can save production unit, and can better realize processing requirement, cost is lower.
Claims (4)
1. process unit of producing methyl nitrite, this device comprises reaction fractionating tower, pre-reactor, reboiler, recooler, Methanol Recovery dashpot and acid tank, described reaction fractionating tower is built-in with condenser, described pre-reactor, reaction fractionating tower, reboiler is connected successively with the Methanol Recovery dashpot, the delivery port of described Methanol Recovery dashpot delivery port and acid tank communicates with reaction fractionating tower respectively, the input terminus of described pre-reactor respectively with the carbonylation reaction operation in NO circulation gas pipeline with oxygen pipeline, be connected, the two ends of described recooler communicate with described condenser and reaction fractionating tower respectively, described recooler one end is connected with the carbonylation reaction system, described acid tank input aperture is connected with acid water pipe and technique hose respectively.
2. the process unit of production methyl nitrite according to claim 1, is characterized in that: between described pre-reactor and reaction fractionating tower, also be provided with preheater.
3. the process unit of production methyl nitrite according to claim 1 and 2, is characterized in that: be equipped with recycle pump on the connection line of described Methanol Recovery dashpot delivery port and acid tank delivery port and reaction fractionating tower.
4. the process unit of production methyl nitrite according to claim 1, it is characterized in that: described oxygen pipeline is provided with air separation plant.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210314836XA CN102807492B (en) | 2012-08-30 | 2012-08-30 | Process device for producing methyl nitrite |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201210314836XA CN102807492B (en) | 2012-08-30 | 2012-08-30 | Process device for producing methyl nitrite |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102807492A CN102807492A (en) | 2012-12-05 |
| CN102807492B true CN102807492B (en) | 2013-11-27 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201210314836XA Active CN102807492B (en) | 2012-08-30 | 2012-08-30 | Process device for producing methyl nitrite |
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Families Citing this family (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103007842A (en) * | 2012-12-26 | 2013-04-03 | 安阳盈德气体有限公司 | Methyl nitrite synthesis reactor |
| CN103182283B (en) * | 2013-03-21 | 2015-12-23 | 安徽淮化股份有限公司 | NO in ethylene glycol industrial production 2pre-reaction apparatus system |
| CN103435489B (en) * | 2013-09-13 | 2016-09-07 | 安徽淮化股份有限公司 | A kind of system synthesizing methyl nitrite and the method for synthesis methyl nitrite |
| CN103467299B (en) * | 2013-09-18 | 2018-06-19 | 安徽淮化股份有限公司 | The preparation method and device of methyl nitrite in a kind of synthesis gas preparing ethylene glycol technique |
| CN103936591B (en) * | 2014-04-14 | 2015-09-16 | 中国五环工程有限公司 | The renovation process of methyl nitrite |
| CN106904714A (en) * | 2017-02-14 | 2017-06-30 | 新疆天智辰业化工有限公司 | Nitrate reductase purification technique in coal-ethylene glycol production |
| CN106831439B (en) * | 2017-03-06 | 2019-01-01 | 西南化工研究设计院有限公司 | A kind of method and device preparing C1~C4 alkyl nitriteester |
| CN106883127B (en) * | 2017-04-14 | 2019-03-05 | 高化学（江苏）化工新材料有限责任公司 | A kind of device continuously generating methyl nitrite |
| CN107793316B (en) * | 2017-12-05 | 2020-04-07 | 中国科学院大连化学物理研究所 | Method for synthesizing methyl nitrite by microreactor |
| CN111265902B (en) * | 2020-03-09 | 2023-04-21 | 内蒙古兰格生物科技有限公司 | Continuous rectifying device |
| CN113648959B (en) * | 2021-08-30 | 2023-04-07 | 江苏永大化工机械股份有限公司 | Circulating esterification tower |
Family Cites Families (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE4307193A1 (en) * | 1993-03-08 | 1994-09-15 | Bayer Ag | Process for the preparation of C¶1¶-C¶4¶-alkyl nitrites |
| DE4338982A1 (en) * | 1993-11-15 | 1995-05-18 | Bayer Ag | Purification of exhaust gases containing alkyl nitrite |
| JP4134761B2 (en) * | 2002-03-06 | 2008-08-20 | 宇部興産株式会社 | Production method of alkyl nitrite |
| CN102008922B (en) * | 2010-09-14 | 2013-01-09 | 中北大学 | Process method and method for regenerating methyl nitrite in production of dimethyl oxalate |
| CN202022868U (en) * | 2011-04-08 | 2011-11-02 | 上海焦化有限公司 | Device for producing methyl nitrite and device for producing oxalic acid dimethyl ester by continuous circulating esterification and carbonylation coupling |
| CN202912871U (en) * | 2012-08-30 | 2013-05-01 | 安徽淮化股份有限公司 | Process device for producing methyl nitrite |
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| CN102807492A (en) | 2012-12-05 |
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Effective date of registration: 20160829 Address after: 232038 Anhui Province, Huainan city tianjia'an District Quanshan Patentee after: Anhui Huaihua Co., Ltd. Patentee after: PUJING CHEMICAL INDUSTRY (SHANGHAI) LIMITED Address before: 232038 Anhui Province, Huainan city tianjia'an District Quanshan Patentee before: Anhui Huaihua Co., Ltd. |
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Effective date of registration: 20210317 Address after: 201102 rooms 615-618, 6th floor, T1 / F, chengkai center, Lane 166, Minhong Road, Minhang District, Shanghai Patentee after: PUJING CHEMICAL INDUSTRY (SHA)LIMITED Address before: 232038 Anhui Province, Huainan city tianjia'an District Quanshan Patentee before: ANHUI HUAIHUA CHEMICAL GROUP Co.,Ltd. Patentee before: PUJING CHEMICAL INDUSTRY (SHA)LIMITED |