CN102126958A - Device and method for preparing high purity m/p-nitrotoluene by coupling rectification and crystallization - Google Patents
Device and method for preparing high purity m/p-nitrotoluene by coupling rectification and crystallization Download PDFInfo
- Publication number
- CN102126958A CN102126958A CN2010106145843A CN201010614584A CN102126958A CN 102126958 A CN102126958 A CN 102126958A CN 2010106145843 A CN2010106145843 A CN 2010106145843A CN 201010614584 A CN201010614584 A CN 201010614584A CN 102126958 A CN102126958 A CN 102126958A
- Authority
- CN
- China
- Prior art keywords
- nitrotoluene
- crystallizer
- para
- meta
- rectifying tower
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Images
Landscapes
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a device and method for preparing high purity m/p-nitrotoluene by coupling rectification and crystallization. In the device disclosed by the invention, a negative pressure rectifying tower (6) is connected with a raw material pipeline (1), a condenser (8) is arranged in the top of the negative pressure rectifying tower (6), the bottom of the condenser (8) is connected with an m-nitrotoluene crystallizer (11) through an m-nitrotoluene enriching pipeline (15), an m-nitrotoluene mother liquor (12) is connected with the negative pressure rectifying tower (6), the negative pressure rectifying tower (6) is connected with a vacuum pump (14) through a negative pressure pipeline (14), the bottom of the negative pressure rectifying tower (6) is connected with a falling film reboiler (7) and a circulating pump (9) through a pipeline, the falling film reboiler (7) is connected with a p-nitrotoluene crystallizer (2) through a p-nitrotoluene enriching pipeline (10), and a p-nitrotoluene mother liquor pipeline (4) is communicated with the negative pressure rectifying tower (6). The device disclosed by the invention has reasonable structure, simple process and low comprehensive energy consumption, is convenient in operation and is an ideal preparation device of high purity m/p-nitrotoluene.
Description
Technical field
The present invention relates between a kind of aromatic hydrocarbons isomers (to) preparation facilities and the method for nitrotoluene, between particularly a kind of rectifying and crystallization coupling preparation high purity (to) device and method of nitrotoluene, be applicable to the separation of contraposition in the MNT, a position isomers.
Background technology
MNT comprises Ortho Nitro Toluene, meta-nitrotoluene, three same isomer of para-nitrotoluene, and they have a wide range of applications in industries such as medicine, agricultural chemicals, dyestuff, rubber ingredients, novel materials.Along with scientific-technical progress, industry development, the development of particularly extraordinary medicine and novel material, to the purity requirement of basic material (as para-nitrotoluene, meta-nitrotoluene) also more and more higher (reaching 99.9%), therefore preparing high purity nitrotoluene raw material just seems more important.Conventional five towers or the seven tower distillation technologies of adopting of the separation of MNT, particularly the separating difficulty between para-nitrotoluene and the meta-nitrotoluene is very big, complicated operation, the energy consumption height, poor product quality, problem is many, the product of producing can only be used to make the product of low specification, sometimes even can not use, therefore brought bigger trouble to the user, this situation has also seriously restricted the development of China's medicine and relevant novel material.
Summary of the invention
The objective of the invention is to: provide between a kind of rectifying and crystallization coupling preparation high purity (to) device and method of nitrotoluene, this apparatus structure is simple, method is reasonable, easy to operate, good product quality, all up to more than 99.9%, energy consumption is low for para-nitrotoluene, the meta-nitrotoluene purity of producing.
Technical solution of the present invention is: this preparation facilities comprises the negative pressure rectifying tower, condenser, the falling film type reboiler, recycle pump, para-nitrotoluene crystallizer and meta-nitrotoluene crystallizer, connect feed line on the negative pressure rectifying tower, condenser is installed in the cat head of negative pressure rectifying tower, the bottom of condenser connects the meta-nitrotoluene crystallizer through rich meta-nitrotoluene pipeline, connect meta-nitrotoluene mother liquor pipeline and meta-nitrotoluene finished product pipeline on the meta-nitrotoluene crystallizer, meta-nitrotoluene finished product pipeline UNICOM negative pressure rectifying tower, the negative pressure rectifying tower connects vacuum pump through vacuum lines, connect falling film type reboiler and recycle pump through pipeline at the bottom of the tower of negative pressure rectifying tower, the falling film type reboiler connects the para-nitrotoluene crystallizer through rich para-nitrotoluene pipeline, connect para-nitrotoluene mother liquor pipeline and para-nitrotoluene finished product pipeline on the para-nitrotoluene crystallizer, para-nitrotoluene mother liquor pipeline is communicated with the negative pressure rectifying tower.
Wherein, para-nitrotoluene crystallizer and meta-nitrotoluene crystallizer are horizontal or the van-type structure, are communicated with the heat transferring medium pipeline on it respectively, and heat transfer tube is sheet or fin, are heat transferring medium in the pipe, are material between pipe.
Preparation method of the present invention may further comprise the steps:
One, raw material is thick nitrotoluene, contain the ortho position nitrotoluene in this thick nitrotoluene, position nitrotoluene between the contraposition nitrotoluene reaches, wherein the boiling point of Ortho Nitro Toluene is 222.3 ℃, the boiling point of meta-nitrotoluene is 231.9 ℃, the boiling point of para-nitrotoluene is 238.5 ℃, to isolate the thick nitrotoluene mixture that contains para-nitrotoluene and meta-nitrotoluene behind the Ortho Nitro Toluene by the rectification under vacuum tower sends into inside by feed line (1) rectifying tower of efficient wire packing (6) is housed, evaporation through falling film type reboiler (7), material constantly carries out vapour-liquid and exchanges mutually in the tower of rectifying tower, form lower boiling--the steam that-meta-nitrotoluene content is higher at cat head, this steam is after overhead condenser (8) condensation, a part is back in the rectifying tower, all the other collect meta-nitrotoluene crystallizer (11) by rich meta-nitrotoluene pipeline (15), process decrease temperature crystalline in the meta-nitrotoluene crystallizer, the discharging mother liquor, the intensification sweating, the temperature increasing for melting materials successive processes obtains the meta-nitrotoluene of content more than 99.9%;
Two, the falling film type reboiler is through successive heating vaporization, in rectifying tower, carry out continuous rectifying, rely on temperature head, high boiling para-nitrotoluene constantly flows at the bottom of the rectifying tower tower and reboiler, when reaching certain content, by rich para-nitrotoluene pipeline (10) input para-nitrotoluene crystallizer (2), material obtains the para-nitrotoluene of content more than 99.9% through decrease temperature crystalline, discharging mother liquor, intensification sweating, temperature increasing for melting materials successive processes in the para-nitrotoluene crystallizer;
Three, the mother liquor of meta-nitrotoluene crystallizer (11) and para-nitrotoluene crystallizer (2) discharge all turns back to rectifying tower, in rectifying tower, vaporize repeatedly and liquefy, high boiling point is separated with low boiling point component, nitre nitrotoluene between the higher richness of the continuous simmer down to meta-nitrotoluene of cat head content, and at the bottom of tower the higher richness of continuous simmer down to para-nitrotoluene content to the nitre nitrotoluene, row purifying during more further by high-efficiency mould.
Wherein, rectifying tower internal pressure: 50～200Pa, rectifying column bottom temperature: 160～185 ℃, the rectifying tower top temperature: 120～165 ℃, meta-nitrotoluene crystallizer charging mass concentration: 88%～96%, meta-nitrotoluene crystallizer cooling temperature: 0～10 ℃, para-nitrotoluene crystallizer charging mass concentration: 80%～95%, para-nitrotoluene crystallizer cooling temperature: 5～30 ℃, crystallizer crystallization cooling rate: 1～2 ℃/hour, crystallizer sweating heat-up rate: 1～2 ℃/hour.
The present invention adopted highly purified of the rectification under vacuum tower of the efficient wire packing of interior dress and crystallizer coupled separation processes produce (to) nitrotoluene, simple in structure, technology is reasonable, easy to operate, can easily obtain content 99.9% above para-nitrotoluene and meta-nitrotoluene, Recycling Mother Solution is applied mechanically, almost not loss, and energy consumption is also lower.
Description of drawings
The present invention is further described below in conjunction with drawings and Examples.
Fig. 1 is a schematic flow sheet of the present invention.
Among the figure: 1 feed line, 2 para-nitrotoluene crystallizers, 3 heat transferring medium pipelines, 4 para-nitrotoluene mother liquor pipelines, 5 para-nitrotoluene finished product pipelines, 6 negative pressure rectifying tower, 7 falling film type reboilers, 8 condensers, 9 recycle pumps, 10 rich para-nitrotoluene pipelines, 11 meta-nitrotoluene crystallizers, 12 meta-nitrotoluene mother liquor pipelines, 13 meta-nitrotoluene finished product pipelines, 14 vacuum lines, 15 rich meta-nitrotoluene pipelines.
Embodiment
With reference to Fig. 1, this preparation facilities comprises negative pressure rectifying tower 6, condenser 8, falling film type reboiler 7, recycle pump 9, para-nitrotoluene crystallizer 2 and meta-nitrotoluene crystallizer 11, connect feed line 1 on the negative pressure rectifying tower 6, condenser 8 is installed in the cat head of negative pressure rectifying tower 6, the bottom of condenser 8 connects meta-nitrotoluene crystallizer 11 through rich meta-nitrotoluene pipeline 15, connect meta-nitrotoluene mother liquor pipeline 12 and meta-nitrotoluene finished product pipeline 13 on the meta-nitrotoluene crystallizer 11, meta-nitrotoluene mother liquor pipeline 12 UNICOM's negative pressure rectifying tower 6, negative pressure rectifying tower 6 connects vacuum pump through vacuum lines 14, connect falling film type reboiler 7 and recycle pump 9 through pipeline at the bottom of the tower of negative pressure rectifying tower 6, falling film type reboiler 7 connects para-nitrotoluene crystallizer 2 through rich para-nitrotoluene pipeline 10, connect para-nitrotoluene mother liquor pipeline 4 and para-nitrotoluene finished product pipeline 5 on the para-nitrotoluene crystallizer 2, para-nitrotoluene mother liquor pipeline 4 is communicated with negative pressure rectifying tower 6.
Wherein, para-nitrotoluene crystallizer 2 and meta-nitrotoluene crystallizer 11 are horizontal or the van-type structure, are communicated with heat transferring medium pipeline 3 on it respectively, and heat transfer tube is sheet or fin, are heat transferring medium in the pipe, are material between pipe.
Embodiment 1: prepare para-nitrotoluene and meta-nitrotoluene according to following steps: one, raw material is thick nitrotoluene, contain the ortho position nitrotoluene in this thick nitrotoluene, position nitrotoluene between the contraposition nitrotoluene reaches, wherein the boiling point of Ortho Nitro Toluene is 222.3 ℃, the boiling point of meta-nitrotoluene is 231.9 ℃, the boiling point of para-nitrotoluene is 238.5 ℃, to isolate the thick nitrotoluene mixture that contains para-nitrotoluene and meta-nitrotoluene behind the Ortho Nitro Toluene by the rectification under vacuum tower sends into inside by feed line (1) rectifying tower of efficient wire packing (6) is housed, evaporation through falling film type reboiler (7), material constantly carries out vapour-liquid and exchanges mutually in the tower of rectifying tower, form lower boiling--the steam that-meta-nitrotoluene content is higher at cat head, this steam is after overhead condenser (8) condensation, a part is back in the rectifying tower, all the other collect meta-nitrotoluene crystallizer (11) by rich meta-nitrotoluene pipeline (15), process decrease temperature crystalline in the meta-nitrotoluene crystallizer, the discharging mother liquor, the intensification sweating, the temperature increasing for melting materials successive processes obtains the meta-nitrotoluene of content more than 99.9%;
Two, the falling film type reboiler is through successive heating vaporization, in rectifying tower, carry out continuous rectifying, rely on temperature head, high boiling para-nitrotoluene constantly flows at the bottom of the rectifying tower tower and reboiler, when reaching certain content, by rich para-nitrotoluene pipeline (10) input para-nitrotoluene crystallizer (2), material obtains the para-nitrotoluene of content more than 99.9% through decrease temperature crystalline, discharging mother liquor, intensification sweating, temperature increasing for melting materials successive processes in the para-nitrotoluene crystallizer;
Three, the mother liquor of meta-nitrotoluene crystallizer (11) and para-nitrotoluene crystallizer (2) discharge all turns back to rectifying tower, in rectifying tower, vaporize repeatedly and liquefy, high boiling point is separated with low boiling point component, nitre nitrotoluene between the higher richness of the continuous simmer down to meta-nitrotoluene of cat head content, and at the bottom of tower the higher richness of continuous simmer down to para-nitrotoluene content to the nitre nitrotoluene, row purifying during more further by high-efficiency mould; Wherein, rectifying tower internal pressure: 50Pa, rectifying column bottom temperature: 160 ℃, the rectifying tower top temperature: 120 ℃, meta-nitrotoluene crystallizer charging mass concentration: 88%, meta-nitrotoluene crystallizer cooling temperature: 0～10 ℃, para-nitrotoluene crystallizer charging mass concentration: 80%, para-nitrotoluene crystallizer cooling temperature: 5～30 ℃, crystallizer crystallization cooling rate: 1～2 ℃/hour, crystallizer sweating heat-up rate: 1～2 ℃/hour.
Embodiment 2: step is with embodiment 1, wherein, rectifying tower internal pressure: 125Pa, the rectifying column bottom temperature: 172 ℃, rectifying tower top temperature: 145 ℃, meta-nitrotoluene crystallizer charging mass concentration: 92%, meta-nitrotoluene crystallizer cooling temperature: 0～10 ℃, para-nitrotoluene crystallizer charging mass concentration: 88%, para-nitrotoluene crystallizer cooling temperature: 5～30 ℃, crystallizer crystallization cooling rate: 1～2 ℃/hour, crystallizer sweating heat-up rate: 1～2 ℃/hour.
Embodiment 3: step is with embodiment 1, wherein, rectifying tower internal pressure: 200Pa, the rectifying column bottom temperature: 185 ℃, rectifying tower top temperature: 165 ℃, meta-nitrotoluene crystallizer charging mass concentration: 96%, meta-nitrotoluene crystallizer cooling temperature: 0～10 ℃, para-nitrotoluene crystallizer charging mass concentration: 95%, para-nitrotoluene crystallizer cooling temperature: 5～30 ℃, crystallizer crystallization cooling rate: 1～2 ℃/hour, crystallizer sweating heat-up rate: 1～2 ℃/hour.
Claims (4)
1. between rectifying and crystallization coupling preparation high purity (to) device of nitrotoluene, it is characterized in that: this preparation facilities comprises negative pressure rectifying tower (6), condenser (8), falling film type reboiler (7), recycle pump (9), para-nitrotoluene crystallizer (2) and meta-nitrotoluene crystallizer (11), negative pressure rectifying tower (6) is gone up and is connected feed line (1), condenser (8) is installed in the cat head of negative pressure rectifying tower (6), the bottom of condenser (8) connects meta-nitrotoluene crystallizer (11) through rich meta-nitrotoluene pipeline (15), meta-nitrotoluene crystallizer (11) is gone up and is connected meta-nitrotoluene mother liquor pipeline (12) and meta-nitrotoluene finished product pipeline (13), meta-nitrotoluene mother liquor pipeline (12) UNICOM's negative pressure rectifying tower (6), negative pressure rectifying tower (6) connects vacuum pump through vacuum lines (14), connect falling film type reboiler (7) and recycle pump (9) through pipeline at the bottom of the tower of negative pressure rectifying tower (6), falling film type reboiler (7) connects para-nitrotoluene crystallizer (2) through rich para-nitrotoluene pipeline (10), para-nitrotoluene crystallizer (2) is gone up and is connected para-nitrotoluene mother liquor pipeline (4) and para-nitrotoluene finished product pipeline (5), and para-nitrotoluene mother liquor pipeline (4) is communicated with negative pressure rectifying tower (6).
Between rectifying 2. according to claim 1 and crystallization coupling preparation high purity (to) device of nitrotoluene, it is characterized in that: wherein, para-nitrotoluene crystallizer (2) and meta-nitrotoluene crystallizer (11) are horizontal or the van-type structure, be communicated with heat transferring medium pipeline (3) on it respectively, heat transfer tube is sheet or fin, in the pipe is heat transferring medium, is material between pipe.
Rectifying and crystallization coupling prepare between high purity (to) method of nitrotoluene, it is characterized in that this preparation method may further comprise the steps:
One, raw material is thick nitrotoluene, contain the ortho position nitrotoluene in this thick nitrotoluene, position nitrotoluene between the contraposition nitrotoluene reaches, wherein the boiling point of Ortho Nitro Toluene is 222.3 ℃, the boiling point of meta-nitrotoluene is 231.9 ℃, the boiling point of para-nitrotoluene is 238.5 ℃, to isolate the thick nitrotoluene mixture that contains para-nitrotoluene and meta-nitrotoluene behind the Ortho Nitro Toluene by the rectification under vacuum tower sends into inside by feed line (1) rectifying tower of efficient wire packing (6) is housed, evaporation through falling film type reboiler (7), material constantly carries out vapour-liquid and exchanges mutually in the tower of rectifying tower, form lower boiling--the steam that-meta-nitrotoluene content is higher at cat head, this steam is after overhead condenser (8) condensation, a part is back in the rectifying tower, all the other collect meta-nitrotoluene crystallizer (11) by rich meta-nitrotoluene pipeline (15), process decrease temperature crystalline in the meta-nitrotoluene crystallizer, the discharging mother liquor, the intensification sweating, the temperature increasing for melting materials successive processes obtains the meta-nitrotoluene of content more than 99.9%;
Two, the falling film type reboiler is through successive heating vaporization, in rectifying tower, carry out continuous rectifying, rely on temperature head, high boiling para-nitrotoluene constantly flows at the bottom of the rectifying tower tower and reboiler, when reaching certain content, by rich para-nitrotoluene pipeline (10) input para-nitrotoluene crystallizer (2), material obtains the para-nitrotoluene of content more than 99.9% through decrease temperature crystalline, discharging mother liquor, intensification sweating, temperature increasing for melting materials successive processes in the para-nitrotoluene crystallizer;
Three, the mother liquor of meta-nitrotoluene crystallizer (11) and para-nitrotoluene crystallizer (2) discharge all turns back to rectifying tower, in rectifying tower, vaporize repeatedly and liquefy, high boiling point is separated with low boiling point component, nitre nitrotoluene between the higher richness of the continuous simmer down to meta-nitrotoluene of cat head content, and at the bottom of tower the higher richness of continuous simmer down to para-nitrotoluene content to the nitre nitrotoluene, row purifying during more further by high-efficiency mould.
4. rectifying according to claim 1 and crystallization coupling prepare between high purity (to) method of nitrotoluene, it is characterized in that: wherein, rectifying tower internal pressure: 50～200Pa, rectifying column bottom temperature: 160～185 ℃, rectifying tower top temperature: 120～165 ℃, meta-nitrotoluene crystallizer charging mass concentration: 88%～96%, meta-nitrotoluene crystallizer cooling temperature: 0～10 ℃, para-nitrotoluene crystallizer charging mass concentration: 80%～95%, para-nitrotoluene crystallizer cooling temperature: 5～30 ℃, crystallizer crystallization cooling rate: 1～2 ℃/hour, crystallizer sweating heat-up rate: 1～2 ℃/hour.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010106145843A CN102126958B (en) | 2010-12-30 | 2010-12-30 | Device and method for preparing high purity m/p-nitrotoluene by coupling rectification and crystallization |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2010106145843A CN102126958B (en) | 2010-12-30 | 2010-12-30 | Device and method for preparing high purity m/p-nitrotoluene by coupling rectification and crystallization |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN102126958A true CN102126958A (en) | 2011-07-20 |
| CN102126958B CN102126958B (en) | 2013-12-04 |
Family
ID=44265278
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN2010106145843A Expired - Fee Related CN102126958B (en) | 2010-12-30 | 2010-12-30 | Device and method for preparing high purity m/p-nitrotoluene by coupling rectification and crystallization |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN102126958B (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104447343A (en) * | 2014-10-29 | 2015-03-25 | 青岛科技大学 | Method for by-producing steam in ortho-nitrotoluene separation process |
| CN105502788A (en) * | 2015-12-31 | 2016-04-20 | 遵义鑫湘生物科技有限公司 | Gallate wastewater disposal system |
| CN105906512A (en) * | 2016-05-13 | 2016-08-31 | 淮安绿源化工科技有限公司 | Single-tower separating technology and device for phenylenediamine isomers |
| CN107501230A (en) * | 2017-09-29 | 2017-12-22 | 福州大学 | Crystallization couples the device and method for preparing electron level ethylene carbonate with rectifying |
| CN113371906A (en) * | 2021-05-31 | 2021-09-10 | 湖北东方化工有限公司 | Dinitrotoluene recovery device and process |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1112545A (en) * | 1995-03-11 | 1995-11-29 | 天津大学北方化工新技术开发公司 | Refining process of vanillin |
| WO2000053561A1 (en) * | 1999-03-06 | 2000-09-14 | Basf Aktiengesellschaft | Fractional condensation of a product gas mixture containing acrylic acid |
| CN1715261A (en) * | 2004-06-28 | 2006-01-04 | 陈华国 | Process for producing high purity 1,2,4-trichlorobenzene and para-dichlorobenzene |
| DE102005017427A1 (en) * | 2005-04-15 | 2006-10-19 | Zimmer Ag | Process for the treatment of condensates from polycondensation |
| CN101250113A (en) * | 2008-03-28 | 2008-08-27 | 上海安诺芳胺化学品有限公司 | Method for refining p-phenylene diamine |
| CN201565153U (en) * | 2009-09-28 | 2010-09-01 | 浙江省常山化工有限责任公司 | Fin type crystallizer for nitrochlorobenzene production |
-
2010
- 2010-12-30 CN CN2010106145843A patent/CN102126958B/en not_active Expired - Fee Related
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1112545A (en) * | 1995-03-11 | 1995-11-29 | 天津大学北方化工新技术开发公司 | Refining process of vanillin |
| WO2000053561A1 (en) * | 1999-03-06 | 2000-09-14 | Basf Aktiengesellschaft | Fractional condensation of a product gas mixture containing acrylic acid |
| CN1715261A (en) * | 2004-06-28 | 2006-01-04 | 陈华国 | Process for producing high purity 1,2,4-trichlorobenzene and para-dichlorobenzene |
| DE102005017427A1 (en) * | 2005-04-15 | 2006-10-19 | Zimmer Ag | Process for the treatment of condensates from polycondensation |
| CN101250113A (en) * | 2008-03-28 | 2008-08-27 | 上海安诺芳胺化学品有限公司 | Method for refining p-phenylene diamine |
| CN201565153U (en) * | 2009-09-28 | 2010-09-01 | 浙江省常山化工有限责任公司 | Fin type crystallizer for nitrochlorobenzene production |
Non-Patent Citations (3)
| Title |
|---|
| DAVID A. BERRY AND KA M. NG: "Synthesis of Crystallization-Distillation Hybrid Separation Processes", 《AICHE JOURNAL》 * |
| 叶青，王车礼，裘兆蓉: "精馏- 熔融结晶耦合工艺", 《江苏石油化工学院学报》 * |
| 张敏华等: "高沸点差热敏性物系精馏塔", 《化学工程》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104447343A (en) * | 2014-10-29 | 2015-03-25 | 青岛科技大学 | Method for by-producing steam in ortho-nitrotoluene separation process |
| CN105502788A (en) * | 2015-12-31 | 2016-04-20 | 遵义鑫湘生物科技有限公司 | Gallate wastewater disposal system |
| CN105906512A (en) * | 2016-05-13 | 2016-08-31 | 淮安绿源化工科技有限公司 | Single-tower separating technology and device for phenylenediamine isomers |
| CN105906512B (en) * | 2016-05-13 | 2018-07-13 | 淮安绿源化工科技有限公司 | A kind of the single column separating technology and device of phenylenediamine isomer |
| CN107501230A (en) * | 2017-09-29 | 2017-12-22 | 福州大学 | Crystallization couples the device and method for preparing electron level ethylene carbonate with rectifying |
| CN107501230B (en) * | 2017-09-29 | 2023-06-23 | 福州大学 | Device and method for preparing electronic grade ethylene carbonate by coupling crystallization and rectification |
| CN113371906A (en) * | 2021-05-31 | 2021-09-10 | 湖北东方化工有限公司 | Dinitrotoluene recovery device and process |
Also Published As
| Publication number | Publication date |
|---|---|
| CN102126958B (en) | 2013-12-04 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN102126958B (en) | Device and method for preparing high purity m/p-nitrotoluene by coupling rectification and crystallization | |
| CN107253938A (en) | Cis-butenedioic anhydride direct hydrogenation prepares the production technology of high purity butylene dicarboxylic anhydride | |
| CN108329235B (en) | Process for producing high-purity chlorothalonil | |
| CN110885283A (en) | Energy-saving process for separating ethyl acetate-ethanol by heat integration extraction rectification with side extraction | |
| CN105906512B (en) | A kind of the single column separating technology and device of phenylenediamine isomer | |
| CN111888792B (en) | Device and method for separating tetrahydrofuran-ethanol-water azeotrope system by extractive distillation | |
| CN104968636A (en) | Device for preparing alkanol | |
| CN107721820B (en) | Method for separating ternary azeotrope by complete heat integration three-tower pressure swing distillation | |
| CN105777470B (en) | Process method and equipment for separating benzene and cyclohexane mixture | |
| CN107935807A (en) | A kind of system and method for recycling refined methyl cyclopentane and application thereof | |
| CN103055530A (en) | Solvent reinforced transformation thermal coupling rectification system for separating cyclohexanone and phenol | |
| CN114191837B (en) | Device and method for separating methanol-benzene-acetonitrile azeotrope system by extractive distillation | |
| CN101830788A (en) | Method for separating azeotropic mixture of ethyl methyl ketone and water through variable-pressure rectification | |
| CN109438500B (en) | Device and method for separating methyl chlorosilane by using internal thermally coupled rectifying tower | |
| CN203878081U (en) | Device system for solvent recovery in process of purifying phenazine by using RT base byproduct | |
| CN112479869B (en) | Method for rectifying dimethyl oxalate in coal chemical industry | |
| CN106631795B (en) | Method for separating isopropyl acetate and n-heptane azeotrope by heat integrated pressure swing distillation | |
| CN111202999B (en) | Rectification device and method for extracting high-purity mesitylene product from oil generated by isomerization reaction of trimethylbenzene | |
| CN107311871A (en) | The process for separation and purification of monomethyl amine diformazan amine blends in a kind of synthetic methylamine system | |
| CN202337741U (en) | Device for producing durene with C10 heavy aromatic | |
| CN106631888B (en) | Three tower variable-pressure rectification separating acetonitrile of Two-way Cycle-Methanol-benzene azeotropic mixture method | |
| CN111377793A (en) | Method for decoloring solvent oil and extracting durene | |
| CN218910199U (en) | System for purifying m-dichlorobenzene in mixed dichlorobenzene | |
| CN108383687A (en) | A kind of purification rectifying column and method of purification for 3- methyl-3-butene-1-alcohols | |
| CN209722009U (en) | A kind of polyisobutene process units that raw material cools down step by step |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20131204 Termination date: 20151230 |
|
| EXPY | Termination of patent right or utility model |