CN102126958B - 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
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- CN102126958B CN102126958B CN2010106145843A CN201010614584A CN102126958B CN 102126958 B CN102126958 B CN 102126958B CN 2010106145843 A CN2010106145843 A CN 2010106145843A CN 201010614584 A CN201010614584 A CN 201010614584A CN 102126958 B CN102126958 B CN 102126958B
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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, particularly between a kind of rectifying and crystallization coupling preparation high purity (to) device and method of nitrotoluene, be applicable to the separation of contraposition in 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 particularly development of 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 meta-nitrotoluene is very large, complicated operation, energy consumption is high, poor product quality, and problem is many, the product of producing can only be for the manufacture of the product of low specification, sometimes even can not use, therefore to the user, bring larger trouble, this situation has also seriously restricted the development of China's medicine and relevant novel material.
Summary of the invention
The object 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, the para-nitrotoluene of producing, meta-nitrotoluene purity are all up to more than 99.9%, and energy consumption is low.
Technical solution of the present invention is: this preparation facilities comprises the negative pressure rectifying tower, condenser, falling-film reboiler, recycle pump, para-nitrotoluene crystallizer and meta-nitrotoluene crystallizer, connect feed line on the negative pressure rectifying tower, condenser is installed in the tower top 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 reboiler and recycle pump through pipeline at the bottom of the tower of negative pressure rectifying tower, falling-film 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, the 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 respectively the heat transferring medium pipeline on it, and heat transfer tube is sheet or fin, in pipe, are heat transferring medium, between pipe, are material.
Preparation method of the present invention comprises the 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 after Ortho Nitro Toluene by vacuum rectifying tower sends into inside by feed line (1) rectifying tower of efficient wire packing (6) is housed, evaporation through falling-film reboiler (7), material constantly carries out the phase exchange in the tower of rectifying tower, form lower boiling---the steam that meta-nitrotoluene content is higher at tower top, this steam is after overhead condenser (8) condensation, a part is back in 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 discharge mother liquor, the intensification sweating, the temperature increasing for melting materials successive processes obtains the meta-nitrotoluene of content more than 99.9%,
Two, falling-film reboiler is through continuous heating vaporization, carry out continuous rectifying in rectifying tower, rely on temperature head, at the bottom of high boiling para-nitrotoluene constantly flows into rectifying 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, discharge mother liquor, intensification sweating, temperature increasing for melting materials successive processes in the para-nitrotoluene crystallizer;
Three, the mother liquor that meta-nitrotoluene crystallizer (11) and para-nitrotoluene crystallizer (2) are discharged all turns back to rectifying tower, repeatedly vaporized in rectifying tower and liquefied, high boiling point is separated with low boiling point component, the nitre nitrotoluene between higher richness at the continuous simmer down to meta-nitrotoluene of tower top content, and the richness that continuous simmer down to para-nitrotoluene content is higher at the bottom of tower is to the nitre nitrotoluene, then row purifying during 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 ℃/h, crystallizer sweating heat-up rate: 1～2 ℃/h.
The present invention adopted the separation method of the vacuum rectifying tower of in-built efficient wire packing and crystallizer coupling prepare highly purified (to) nitrotoluene, simple in structure, technique is reasonable, easy to operate, can easily obtain the above para-nitrotoluene of content 99.9% and meta-nitrotoluene, Recycling Mother Solution is applied mechanically, almost not loss, and energy consumption is also lower.
The accompanying drawing explanation
Below in conjunction with drawings and Examples, the present invention is further described.
Fig. 1 is schematic flow sheet of the present invention.
In 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 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 reboiler 7, recycle pump 9, para-nitrotoluene crystallizer 2 and meta-nitrotoluene crystallizer 11, connect feed line 1 on negative pressure rectifying tower 6, condenser 8 is installed in the tower top 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 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 reboiler 7 and recycle pump 9 through pipeline at the bottom of the tower of negative pressure rectifying tower 6, falling-film 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 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 respectively heat transferring medium pipeline 3 on it, and heat transfer tube is sheet or fin, in pipe, are heat transferring medium, between pipe, are material.
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 after Ortho Nitro Toluene by vacuum rectifying tower sends into inside by feed line (1) rectifying tower of efficient wire packing (6) is housed, evaporation through falling-film reboiler (7), material constantly carries out the phase exchange in the tower of rectifying tower, form lower boiling---the steam that meta-nitrotoluene content is higher at tower top, this steam is after overhead condenser (8) condensation, a part is back in 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 discharge mother liquor, the intensification sweating, the temperature increasing for melting materials successive processes obtains the meta-nitrotoluene of content more than 99.9%,
Two, falling-film reboiler is through continuous heating vaporization, carry out continuous rectifying in rectifying tower, rely on temperature head, at the bottom of high boiling para-nitrotoluene constantly flows into rectifying 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, discharge mother liquor, intensification sweating, temperature increasing for melting materials successive processes in the para-nitrotoluene crystallizer;
Three, the mother liquor that meta-nitrotoluene crystallizer (11) and para-nitrotoluene crystallizer (2) are discharged all turns back to rectifying tower, repeatedly vaporized in rectifying tower and liquefied, high boiling point is separated with low boiling point component, the nitre nitrotoluene between higher richness at the continuous simmer down to meta-nitrotoluene of tower top content, and the richness that continuous simmer down to para-nitrotoluene content is higher at the bottom of tower is to the nitre nitrotoluene, then row purifying during 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 ℃/h, crystallizer sweating heat-up rate: 1～2 ℃/h.
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 ℃/h, crystallizer sweating heat-up rate: 1～2 ℃/h.
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 ℃/h, crystallizer sweating heat-up rate: 1～2 ℃/h.
Claims (4)
1. rectifying and crystallization coupling prepare high purity
meta-nitrotoluene and para-nitrotoluenedevice, it is characterized in that: this preparation facilities comprises negative pressure rectifying tower (6), condenser (8), falling-film reboiler (7), recycle pump (9), para-nitrotoluene crystallizer (2) and meta-nitrotoluene crystallizer (11), the upper feed line (1) that connects of negative pressure rectifying tower (6), condenser (8) is installed in the tower top of negative pressure rectifying tower (6), the bottom of condenser (8) connects meta-nitrotoluene crystallizer (11) through rich meta-nitrotoluene pipeline (15), upper meta-nitrotoluene mother liquor pipeline (12) and the meta-nitrotoluene finished product pipeline (13) of connecting of 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 reboiler (7) and recycle pump (9) through pipeline at the bottom of the tower of negative pressure rectifying tower (6), falling-film reboiler (7) connects para-nitrotoluene crystallizer (2) through rich para-nitrotoluene pipeline (10), upper para-nitrotoluene mother liquor pipeline (4) and the para-nitrotoluene finished product pipeline (5) of connecting of para-nitrotoluene crystallizer (2), para-nitrotoluene mother liquor pipeline (4) is communicated with negative pressure rectifying tower (6).
2. rectifying according to claim 1 and crystallization coupling prepare high purity
Meta-nitrotoluene and para-nitrotolueneDevice, 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 respectively heat transferring medium pipeline (3) on it, heat transfer tube is sheet or fin, in pipe, is heat transferring medium, between pipe, is material.
3. rectifying and crystallization coupling prepare high purity
Meta-nitrotoluene and para-nitrotolueneMethod, it is characterized in that this preparation method comprises the 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 after Ortho Nitro Toluene by vacuum rectifying tower sends into inside by feed line (1) rectifying tower of efficient wire packing (6) is housed, evaporation through falling-film reboiler (7), material constantly carries out the phase exchange in the tower of rectifying tower, form lower boiling---the steam that meta-nitrotoluene content is higher at tower top, this steam is after overhead condenser (8) condensation, a part is back in 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 discharge mother liquor, the intensification sweating, the temperature increasing for melting materials successive processes obtains the meta-nitrotoluene of content more than 99.9%,
Two, falling-film reboiler is through continuous heating vaporization, carry out continuous rectifying in rectifying tower, rely on temperature head, at the bottom of high boiling para-nitrotoluene constantly flows into rectifying 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, discharge mother liquor, intensification sweating, temperature increasing for melting materials successive processes in the para-nitrotoluene crystallizer;
Three, the mother liquor that meta-nitrotoluene crystallizer (11) and para-nitrotoluene crystallizer (2) are discharged all turns back to rectifying tower, repeatedly vaporized in rectifying tower and liquefied, high boiling point is separated with low boiling point component, at the higher rich meta-nitrotoluene of the continuous simmer down to meta-nitrotoluene of tower top content, and at the bottom of tower the higher rich para-nitrotoluene of continuous simmer down to para-nitrotoluene content, more further by high-efficiency mould, carry out purifying.
4. rectifying according to claim 3 and crystallization coupling prepare high purity
Meta-nitrotoluene and para-nitrotolueneMethod, 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 ℃/h, crystallizer sweating heat-up rate: 1～2 ℃/h.
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| 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 |
| 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 |
| 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 |
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