CN101759569B - Method for extracting high purity para-nitrochlorobenzene and ortho-nitrochlorobenzene by synthesis method of multistrand side track discharging rectification and continuous crystallization - Google Patents
Method for extracting high purity para-nitrochlorobenzene and ortho-nitrochlorobenzene by synthesis method of multistrand side track discharging rectification and continuous crystallization Download PDFInfo
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Abstract
The invention provides a method for extracting para-nitrochlorobenzene and ortho-nitrochlorobenzene by using a stranded siding discharging rectification and continuous crystallization integration method comprising the following steps: (1) raw materials are continuously fed into a rectifying column, heating is initiated when liquid level reaches 1/3 height of the rectifying column; (2) temperature at tower top is retained within 131-133 DEG C, temperature at side track D-2 is retained within 235.5-241 DEG C, temperature at D-3 is retained within 246-247 DEG C, temperature at the tower bottom is retained within 251-257 DEG C in the case of total reflux at stable temperature; (3). after separation, chlorobenzene light components are at the tower top, para-nitrochlorobenzene enrichmentliquid is at the side track D-2, ortho-nitrochlorobenzene enrichment liquid is at the side track D-3 and dinitrochloridizebenzene is at tower bottom D-4; (4) primary crystallization is carried out when components at side track D-2 are condensated; (5) after crystal scraping, para-nitrochlorobenzene with a concentration of more than 99% can be obtained; (6) primary crystallization is carried out on components at side track D-3; (7). secondary crystallization is carried out on remaining mother liquor; (8) after crystal scraping, ortho-nitrochlorobenzene purity is more than 99% and yield is more than 98%.The invention features short cycle, easy operation and low energy consumption.
Description
Technical field
The present invention relates to a kind of Multi-strand lateral line discharging rectifying and separate the technique of mixing nitro chlorobenzene with the continuous crystallisation Integration Method, being specifically related to a kind of Multi-strand lateral line discharging rectifying and continuous crystallization method and extracting the processing method of para-nitrochloro-benzene and ortho-nitrochlorobenzene from mix nitro chlorobenzene, is a kind of technique by single side line rectifying tower and continuous crystallization method extraction para-nitrochloro-benzene and ortho-nitrochlorobenzene from mix nitro chlorobenzene.
Background technology
Extract para-nitrochloro-benzene and ortho-nitrochlorobenzene in nitro chlorobenzene for mixing in conventional art, comparatively general method is mainly that the cut-out light constituent is as the nitration reaction raw material, then extract respectively wherein para-nitrochloro-benzene and ortho-nitrochlorobenzene cut, remaining dinitrochlorobenzene is as extracting the dinitrochlorobenzene raw material.In mixing the nitro chlorobenzene rectifying, generally all adopt batch fractionating, cut into Benzene Chloride, para-nitrochloro-benzene pregnant solution, ortho-nitrochlorobenzene pregnant solution different fractions.Even there is part producing to adopt continuous rectification, but be nearly all to use 2～3 rectifying tower to cut cut under different boiling, in the cut of gained with para-nitrochloro-benzene pregnant solution and ortho-nitrochlorobenzene pregnant solution by single-stage, periodic crystallisation after purification para-nitrochloro-benzene and ortho-nitrochlorobenzene.Obviously, traditional technology is that the cut that obtains different boiling needs corresponding 2～3 rectifying tower, and facility investment is large, energy consumption is large, yield is low, and production cost is corresponding higher, adopt simultaneously the gap crystallization, para-nitrochloro-benzene and ortho-nitrochlorobenzene purity and yield are lower.
Summary of the invention
In order to make up existing above-mentioned deficiency of producing, a kind of method that the present invention will provide Multi-strand lateral line discharging rectifying and continuous crystallisation Integration Method to extract high purity para-nitrochloro-benzene and ortho-nitrochlorobenzene, the method can realize extracting para-nitrochloro-benzene and the industrialization of ortho-nitrochlorobenzene cut from mix nitro chlorobenzene.By a tower, not only obtain the para-nitrochloro-benzene cut, obtain simultaneously the ortho-nitrochlorobenzene cut, in gained para-nitrochloro-benzene and ortho-nitrochlorobenzene liquid collecting cut, para-nitrochloro-benzene and ortho-nitrochlorobenzene content are all higher, and especially this process operation is simple, energy consumption is low, yield is high.And para-nitrochloro-benzene and the ortho-nitrochlorobenzene crystal purity is high, yield is high after continuous crystallisation, stock liquid can recycle.
The scheme of completing the foregoing invention task is: a kind of Multi-strand lateral line discharging rectifying and continuous crystallisation Integration Method extract the method for para-nitrochloro-benzene and ortho-nitrochlorobenzene, it is characterized in that, step is as follows,
(1). adopt continuous intermediate feed mode, raw material is squeezed into the rectifying tower reactor from mixing the nitro chlorobenzene storage tank, begins heating when liquid level reaches 1/3 place;
(2). when tower top, tower reactor temperature begin to stablize, when device reached total reflux, the tower top temperature was 131～133 ℃, and side line D-2 place temperature is 235.5～241 ℃, and side line D-3 place temperature is 246～247 ℃, and the tower reactor temperature is 251～257 ℃;
(3). after separation, the tower top component is the Benzene Chloride light constituent, and side line D-2 component is the para-nitrochloro-benzene pregnant solution; Content is more than 92%, and yield is more than 92%, and side line D-3 component is the ortho-nitrochlorobenzene pregnant solution; Content is more than 85%, and yield is more than 83.9%, and tower reactor D-4 is the dinitrochlorobenzene part;
(4). side line D-2 component is squeezed into after condensation in continuous crystallisation device raw material storage tank, for being rich in 92% above para-nitrochloro-benzene pregnant solution, squeezes into continuous crystallisation device primary crystallization through pump in raw material storage tank 2, and Tc is controlled at-6 ℃, and crystallization time is 3h;
(5). crystal scrapes through scraper, and the suction filtration oven dry enters finished pot after the funnel extraction, obtains 99% above para-nitrochloro-benzene;
(6). side line D-3 component is squeezed into after condensation in continuous crystallisation device raw material storage tank 3, squeezes in crystallization apparatus through pump, and the primary crystallization temperature is controlled at-3 ℃, and crystallization time is 1h;
(7). primary crystallization device residue mother liquor enters the secondary crystal device, and Tc is controlled at-6～7 ℃, and crystallization time is 2h;
(8). crystal scrapes through scraper, enters the ortho-nitrochlorobenzene finished pot from crystallizer bottom extraction filtrate, and the ortho-nitrochlorobenzene mass content can reach more than 99%, and yield reaches more than 98%.
The present invention is in above scheme,
After described step (3) was separated, the para-nitrochloro-benzene pregnant solution weight percent content of side line D-2 component was more than 92%, and yield is more than 92%; The ortho-nitrochlorobenzene pregnant solution content of described side line D-3 component is more than 85%, and yield is more than 83.9%;
Described step (4), the para-nitrochloro-benzene pregnant solution weight percent in raw material storage tank 2 is more than 92%.
In above scheme, in described raw material, the content of para-nitrochloro-benzene and ortho-nitrochlorobenzene is respectively 63.12% and 34.72%, and the load of Multi-strand lateral line rectifying tower tower top, side line D-2, side line D-3, tower reactor D-4 was respectively 0.005: 1,0.626: 1,0.34: 1,0.0276: 1 with the ratio of raw material inlet amount.
The present invention recommends: described mixing nitro chlorobenzene raw material is in the 27th plate charging of Multi-strand lateral line rectifying tower, structured packing is established in inside, the side line discharge internal partition is connected to airway and upflow tube flows for vapour-liquid, upper and lower end adopts flange plate to connect, D-2 extraction mouth is the 15th block of plate, and D-3 extraction mouth is the 45th block of plate.
Multi-strand lateral line discharging rectifying and continuous crystallization method extract the high purity para-nitrochloro-benzene from mix nitro chlorobenzene and ortho-nitrochlorobenzene technique detailed process is seen Fig. 1, Fig. 2, shown in Figure 3, and Multi-strand lateral line discharging rectifying and continuous crystallisation manufacturing condition are as shown in table 1,2.
The Multi-strand lateral line discharging rectifier unit as shown in Figure 1, device mainly comprises raw material storage tank 14, Multi-strand lateral line discharging rectifying tower 15, overhead product extraction mouth 16, side line D-2 extraction mouth 17, side line D-3 extraction mouth 18, tower reactor extraction mouth 19, condenser system 20 and pump P-1, P-2.Multi-strand lateral line discharging rectifying tower be linked in sequence from top to bottom stripping section, the second rectifying section, the first rectifying section, tower top end socket and condenser.Raw material is squeezed into tower reactor from 14 by pump, when liquid level reaches 1/3 place, begins heating and treats that total reflux, reflux ratio are 4, and the tower top temperature is 131～133 ℃, and side line D-2 place temperature is 235.5～241 ℃, and side line D-3 place temperature is 246～247 ℃, and the tower reactor temperature is 251～257 ℃; Control spinner-type flowmeter with the 30Kg/h continuously feeding, 16,17,18 and 19 place's continuous discharge amounts are shown in Table 3.
The continuous crystallisation device as shown in Figure 2, raw material storage tank 9, primary crystallization device 10, recrystallize device 11, mother liquor holding tank 12, crystal storage tank 13.Crystallization raw material storage tank 9 comes from 17 place's para-nitrochloro-benzene pregnant solutions, squeezes into 10 through pump.10 internal structures as shown in Figure 3, refrigerating fulid opening for feed 1, drive system 2, rotary drum 3, cooling system 4, refrigerating fulid outlet 5, doctor blade system 6, frame 7, charging tray 8.After raw material enters, drive system 2 drives rotary drum 3 rotations, the sodium-chlor refrigerating fulid enters 1, through cooling system 4, emit by 5 after cooling feed liquid, on charging tray 8, crystal is taken out of by rotary drum, after doctor blade system 6 scrapes after the funnel extraction suction filtration oven dry to finished pot, the residue mother liquor enters recrystallize 11 from the bottom of device discharge hole, remains at last mother liquor and enters 12.10 place's Tcs are controlled at-3 ℃, and crystallization time is 1h, and 11 place's Tcs are controlled at-6～7 ℃, and crystallization time is 2h.Multi-strand lateral line discharging rectifying and continuous crystallization method extract the high purity para-nitrochloro-benzene from mix nitro chlorobenzene and ortho-nitrochlorobenzene technique separating resulting as shown in table 3.
Multi-strand lateral line discharging rectifying of the present invention and continuous crystallization method extract high purity para-nitrochloro-benzene and ortho-nitrochlorobenzene technique from mix nitro chlorobenzene, the cycle is short, simple to operate, energy consumption is low, relative yield is high.in Multi-strand lateral line discharging rectifying tower temperature, input and output material speed, under the reflux ratio certain condition, in the para-nitrochloro-benzene pregnant solution, para-nitrochloro-benzene content is disposable can bring up to 92% (wt%) more than, yield reaches more than 92%, after continuous crystallisation, the para-nitrochloro-benzene crystal purity is more than 99%, yield is more than 89%, in the ortho-nitrochlorobenzene pregnant solution, ortho-nitrochlorobenzene content is disposable can bring up to 85% (wt%) more than, yield reaches more than 83%, after continuous crystallisation, the ortho-nitrochlorobenzene crystal purity is more than 99.2%, yield is more than 98%.
Description of drawings
Fig. 1 is Multi-strand lateral line discharging rectifier unit figure;
Fig. 2 is the continuous crystallisation setting drawing;
Fig. 3 is the crystallization apparatus structure iron.
Embodiment
Embodiment 1, and Multi-strand lateral line discharging rectifying and continuous crystallization method extract high purity para-nitrochloro-benzene and ortho-nitrochlorobenzene technique from mix nitro chlorobenzene, with reference to Fig. 1, Fig. 2:
(1). adopt continuous intermediate feed mode, raw material is squeezed in 15 tower reactor liquid level 1/3 place begin heating;
(2) begin to stablize when tower top, still temperature, when device reached total reflux, the tower top temperature was 131～133 ℃, and side line D-2 place temperature is 235.5～241 ℃, and side line D-3 place temperature is 246～247 ℃, and the tower reactor temperature is 251～257 ℃;
(3) after the separation, 16 place's components are the Benzene Chloride light constituent, and 17 place's components are the para-nitrochloro-benzene pregnant solution, mass content is more than 92%, and yield is more than 92%, and 18 place's components are the ortho-nitrochlorobenzene pregnant solution, mass content 85%, 19 place is for mixing the dinitrochlorobenzene part;
(4) side line D-2 component is squeezed into after condensation in continuous crystallisation device raw material storage tank, for being rich in 92% above para-nitrochloro-benzene pregnant solution, squeezes into continuous crystallisation device primary crystallization through pump in raw material storage tank 2, and Tc is controlled at-6 ℃, and crystallization time is 3h;
(5) crystal scrapes through scraper, and the suction filtration oven dry enters finished pot after the funnel extraction, obtains 99% above para-nitrochloro-benzene, and yield reaches more than 89%;
(6) side line D-3 component is squeezed into after condensation in continuous crystallisation device raw material storage tank 3, squeezes in crystallization apparatus through pump; The primary crystallization temperature is controlled at-3 ℃, and crystallization time is 1h,
(7) primary crystallization device residue mother liquor enters the secondary crystal device, and Tc is controlled at-6～7 ℃, and crystallization time is 2h;
(8) crystal scrapes through scraper, enters the ortho-nitrochlorobenzene finished pot from crystallizer bottom extraction filtrate, and ortho-nitrochlorobenzene purity can reach more than 99%, and yield reaches more than 98%.
Table 1 Multi-strand lateral line discharging rectification process condition
Table 2 continuous crystallisation processing condition
The rectifying of table 3 Multi-strand lateral line discharging and continuous crystallisation extract high purity para-nitrochloro-benzene and ortho-nitrochlorobenzene result from mix nitro chlorobenzene
Claims (2)
1. a Multi-strand lateral line discharging rectifying and continuous crystallisation Integration Method extract the method for para-nitrochloro-benzene and ortho-nitrochlorobenzene, it is characterized in that, step is as follows,
(1). adopt continuous intermediate feed mode, raw material is squeezed into the rectifying tower reactor from mixing the nitro chlorobenzene storage tank, begins heating when liquid level reaches 1/3 place;
(2). when tower top, tower reactor temperature begin to stablize, when device reached total reflux, the tower top temperature was 131～133 ℃, and side line D-2 place temperature is 235.5～241 ℃, and side line D-3 place temperature is 246～247 ℃, and the tower reactor temperature is 251～257 ℃;
(3). after separation, the tower top component is the Benzene Chloride light constituent, and side line D-2 component is the para-nitrochloro-benzene pregnant solution; Mass content is more than 92%, and yield is more than 92%, and side line D-3 component is the ortho-nitrochlorobenzene pregnant solution; Mass content is more than 85%, and yield is more than 83.9%, and tower reactor D-4 is the dinitrochlorobenzene part;
(4). side line D-2 component is squeezed into after condensation in continuous crystallisation device raw material storage tank, in raw material storage tank 2 for being rich in the above para-nitrochloro-benzene pregnant solution of quality 92%, squeeze into continuous crystallisation device primary crystallization through pump, Tc is controlled at-6 ℃, and crystallization time is 3h;
(5). crystal scrapes through scraper, and the suction filtration oven dry enters finished pot after the funnel extraction, obtains the above para-nitrochloro-benzene of weight percent 99%;
(6). side line D-3 component is squeezed into after condensation in continuous crystallisation device raw material storage tank 3, squeezes in crystallization apparatus through pump, and the primary crystallization temperature is controlled at-3 ℃, and crystallization time is 1h;
(7). primary crystallization device residue mother liquor enters the secondary crystal device, and Tc is controlled at-6～7 ℃, and crystallization time is 2h;
(8). crystal scrapes through scraper, enters the ortho-nitrochlorobenzene finished pot from crystallizer bottom extraction filtrate, and ortho-nitrochlorobenzene purity reaches weight percent more than 99%, and yield reaches more than 98%;
Table 1 Multi-strand lateral line discharging rectification process condition
Table 2 continuous crystallisation processing condition
The rectifying of table 3 Multi-strand lateral line discharging and continuous crystallisation extract para-nitrochloro-benzene and ortho-nitrochlorobenzene result from mix nitro chlorobenzene
2. Multi-strand lateral line discharging rectifying according to claim 1 and continuous crystallisation Integration Method extract the method for para-nitrochloro-benzene and ortho-nitrochlorobenzene, it is characterized in that, in described raw material, the content of para-nitrochloro-benzene and ortho-nitrochlorobenzene is respectively 63.12% and 34.72%, and the load of Multi-strand lateral line rectifying tower tower top, side line D-2, side line D-3, tower reactor D-4 was respectively 0.005: 1,0.626: 1,0.34: 1,0.0276: 1 with the ratio of raw material inlet amount.
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| CN101270031A (en) * | 2008-04-29 | 2008-09-24 | 南京师范大学 | Method for extracting dichlorobenzene cut fraction in mix chlorobenzene with continuous single-column multi-ply sidetrack discharge fractional distillation |
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| CN101270031A (en) * | 2008-04-29 | 2008-09-24 | 南京师范大学 | Method for extracting dichlorobenzene cut fraction in mix chlorobenzene with continuous single-column multi-ply sidetrack discharge fractional distillation |
Non-Patent Citations (4)
| Title |
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| 刘斌等.硝基氯苯生产技术.《氯碱工业》.2002,(第5期),31-32页. |
| 叶泳恒.硝基氯苯单塔精馏工艺的开发与应用.《石油化工》.1996,第25卷639-645. |
| 硝基氯苯单塔精馏工艺的开发与应用;叶泳恒;《石油化工》;19961231;第25卷;639-645 * |
| 硝基氯苯生产技术;刘斌等;《氯碱工业》;20020531(第5期);31-32页 * |
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