CN218653902U - DCB dissolves separator in succession - Google Patents
DCB dissolves separator in succession Download PDFInfo
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- CN218653902U CN218653902U CN202223065790.0U CN202223065790U CN218653902U CN 218653902 U CN218653902 U CN 218653902U CN 202223065790 U CN202223065790 U CN 202223065790U CN 218653902 U CN218653902 U CN 218653902U
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Abstract
The utility model provides a DCB dissolves separator in succession, include: the DCB transposition toluene solution material pool is used for storing and pumping the DCB transposition toluene solution; a hot water tank for storing and pumping hot water; the multi-stage static mixer is used for mixing the DCB transposition toluene solution and hot water, and a liquid inlet of the multi-stage static mixer is respectively connected with a liquid outlet of the DCB transposition toluene solution material pool and a liquid outlet of the hot water pool; and the centrifugal machine is used for centrifugally separating the DCB aqueous solution and the waste toluene solution, the top of the centrifugal machine is provided with a mixed liquid inlet, and the mixed liquid inlet is connected with the liquid outlet of the multistage static mixer. This device is the dissolution separation device who passes in and out the material in succession, and multistage static mixer improves the hot water dissolution efficiency of DCB transposition toluene solution, and high-efficient centrifugal separation DCB aqueous solution of centrifuge and useless toluene solution guarantee the purity of separation product, further improve the rate of recovery of useless toluene, have easy operation, consuming time short, advantage such as with low costs.
Description
Technical Field
The utility model relates to a material of organic pigment chemical industry dissolves the separation field, especially involves a DCB dissolves separator in succession.
Background
DCB is short for 3,3' -dichlorobenzidine, is an important intermediate for producing dichlorobenzidine yellow organic pigment, the yield of the series of yellow organic pigments produced by using the DCB as a raw material accounts for about 25 percent of the total amount of the organic pigments, and the organic pigments are widely applied to the production of coloring and pigment printing slurry and pigment dyeing slurry of printing ink, paint, rubber, plastics and the like.
The DCB production process is characterized in that o-nitrochlorobenzene is used as a raw material, a DCB reducing substance (2, 2-dichlorohydrazobenzene) toluene solution is obtained through hydrogenation reaction, and then the DCB reducing substance and hydrochloric acid are subjected to transposition reaction to obtain a DCB transposition toluene solution material. At present, when DCB transposition toluene solution materials are dissolved and separated at home and abroad, adopted reaction equipment is an intermittent reaction kettle, namely hot water is added into the dissolution kettle to dissolve the DCB transposition toluene solution for transparence, then the dissolution kettle is kept still for a period of time to wait for the DCB water solution and the waste toluene to be layered, and then an operator carries out manual separation by observing through a sight glass on site. The manual separation mode of the DCB transposition toluene solution is not only easy to cause misoperation, but also causes the waste toluene to enter the DCB water solution, and the manual separation causes the toluene contained in the DCB water solution to have larger amount, thereby influencing the poor product quality and lowering the recovery rate of the toluene.
The prior art CN104610072A discloses a method for preparing 3,3' -dichlorobenzidine hydrochloride by rearrangement, wherein the dissolving and separating steps adopt a batch-type dissolving and separating method: adding 0.5% diluted hydrochloric acid into the product of the rearrangement reaction, mixing, stirring, heating to 80 ℃, standing for layering, wherein the lower layer solution is 3,3' -dichlorobenzidine hydrochloride solution, the upper layer solution is a toluene layer, and recovering the upper layer solution toluene as a solvent for continuous use. The method manually separates the toluene layer from the 3,3 '-dichlorobenzidine hydrochloride solution layer, which not only easily causes the toluene mixed in the 3,3' -dichlorobenzidine hydrochloride solution to influence the product purity, but also easily causes the recovery rate of the upper layer toluene solution to be reduced.
The prior art CN113548972A discloses a production process of 3,3 '-dichlorobenzidine hydrochloride, which uses ortho-nitrochlorobenzene as a main raw material to carry out catalytic hydrogenation reduction reaction, the obtained reduction product is firstly rectified to remove waste toluene, then the rectified target product 2, 2-dichlorohydrazobenzene is transposed and separated to obtain the 3,3' -dichlorobenzidine hydrochloride, a centrifugal machine is adopted to carry out solid-liquid separation on the 3,3 '-dichlorobenzidine hydrochloride and dilute hydrochloric acid, the recycling of the byproduct 2-chloroaniline is realized, the product yield and the toluene recovery rate are higher, but the process of firstly removing the toluene by rectification and then carrying out the transposition reaction, and finally the centrifugal machine is used to carry out the solid-liquid separation to obtain the 3,3' -dichlorobenzidine hydrochloride is too complex, and the cost of rectifying and removing the toluene is higher.
SUMMERY OF THE UTILITY MODEL
The utility model aims at providing a new DCB transposition toluene solution separator, the process of solving traditional DCB transposition toluene solution separation is complicated, long consuming time, the separation purity is low, the problem that useless toluene rate of recovery is low.
The utility model provides a DCB dissolves separator in succession, include:
the DCB transposition toluene solution material pool is used for storing and pumping the DCB transposition toluene solution;
a hot water tank for storing and pumping hot water;
the multi-stage static mixer is used for mixing the DCB transposition toluene solution and hot water, and liquid inlets of the multi-stage static mixer are respectively connected with a liquid outlet of the DCB transposition toluene solution material pool and a liquid outlet of the hot water pool;
and the centrifugal machine is used for centrifugally separating the DCB aqueous solution and the waste toluene solution, the top of the centrifugal machine is provided with a mixed liquid inlet, and the mixed liquid inlet is connected with the liquid outlet of the multistage static mixer.
Compared with the prior art, the utility model provides a DCB dissolves separator in succession carries DCB transposition toluene solution and hot water and slowly mildly dissolves in the multistage static mixer in succession, DCB transposition toluene solution and hot water intensive mixing in multistage static mixer, obtain the mixed solution of DCB aqueous solution and useless toluene, mixed solution carries and carries out continuous centrifugation separation in the centrifuge, heavy liquid is the DCB aqueous solution, light liquid is useless toluene, centrifuge high-efficient separation light liquid and heavy liquid, need not to rely on manual separation, separate out high-purity DCB aqueous solution and useless toluene, the mode of business turn over material in succession need not to wait for DCB transposition toluene solution layering and can separate, shorten the consuming time of continuous dissolution separation, the continuous dissolution separation simple process of this device, consuming time weak point, the DCB aqueous solution of separation contains impurity less, the rate of recovery of useless toluene is high.
Preferably, a liquid inlet of the first-stage static mixer is connected with a liquid outlet of the DCB transposition toluene solution material pool and a liquid outlet of the hot water pool, a liquid outlet of the first-stage static mixer is connected with a liquid inlet of the second-stage static mixer, and a liquid outlet of the second-stage static mixer is connected with a liquid inlet of the mixed liquid. Multistage static mixer includes two-stage static mixer, guarantees that hot water and DCB transposition toluene solution can the intensive mixing dissolve, and the DCB transposition result in the DCB transposition toluene solution is fully dissolved to hot water, improves the separation purity of DCB aqueous solution and useless toluene to improve the recycle ratio of useless toluene.
Preferably, the centrifuge is a disk centrifuge.
Preferably, the centrifuge body is made of one of hastelloy, titanium alloy or fluorine-lined anticorrosive material.
The separation of the DCB transposition toluene solution belongs to liquid-liquid separation, the disc centrifuge can effectively separate heavy liquid and light liquid at high speed, and the separation degree is higher, so that impurities in the DCB water solution are reduced, and the recovery rate of waste toluene is improved; the centrifuge with good thermal stability and high corrosion resistance is selected, so that the centrifuge can be prevented from being corroded and damaged by organic solution, and impurities are introduced into the separation liquid.
Preferably, a first regulating valve is arranged between the liquid outlet of the DCB transposition toluene solution material pool and the liquid inlet of the multistage static mixer, and a second regulating valve is arranged between the liquid outlet of the hot water pool and the liquid inlet of the multistage static mixer. The first regulating valve and the second regulating valve are used for regulating the flow proportion of the DCB transposition toluene solution and hot water, the DCB transposition toluene solution and the hot water can be fully mixed and dissolved in the multistage static mixer, DCB transposition products are completely dissolved in the hot water, and the concentration of the DCB water solution is improved.
Preferably, the multistage static mixer is a pipeline static mixer.
Preferably, the static mixer is of the SK type or SX type.
An SK type or SX type pipeline type static mixer is selected to effectively increase the contact area of the DCB transposition toluene solution and hot water, so that the DCB transposition products and the hot water are fully mixed and dissolved in the multistage static mixer, and the purity of the DCB water solution and the recovery rate of the waste toluene in subsequent centrifugal separation are improved.
The beneficial effects of the utility model are that: the utility model relates to a multistage static mixer forms the dissolution piece-rate system of business turn over material in succession with disk centrifuge, in multistage static mixer, DCB transposition result fully dissolves the DCB aqueous solution that forms the high concentration in the hot water, DCB transposition result in the useless toluene reduces, the poor increase of quality of heavy liquid and light liquid, then can promote the centrifugation effect, and then the rate of recovery of useless toluene has also obtained the improvement, useless toluene and DCB aqueous solution high-efficient separation in high-speed disk centrifuge, the purity of the DCB aqueous solution that obtains is high, do not contain useless toluene impurity, and useless toluene of centrifuge autosegregation and DCB aqueous solution, it is consuming time short, need not to rely on artifical layered separation, the rate of recovery that has both improved useless toluene and the purity of DCB aqueous solution have reduced the separation cost again.
Drawings
FIG. 1 is a schematic structural view of a DCB continuous dissolution separation device according to an embodiment of the present invention;
description of the reference numerals:
1-DCB transposition toluene solution material pool; 2-a hot water tank; 3-a multistage static mixer; 4-a centrifuge; 5-a first flow meter; 6-a second flow meter; 7-a first regulating valve; 8-a second regulating valve; 31-first stage static mixer; 32-a second stage static mixer; 41-a liquid inlet of mixed liquid; 42-waste toluene outlet; and 43-DCB aqueous solution outlet.
Detailed Description
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. The components of the embodiments of the present invention generally described and illustrated in the figures herein may be arranged and designed in a wide variety of different configurations.
Thus, the following detailed description of the embodiments of the present invention, presented in the accompanying drawings, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. Based on the embodiments of the present invention, all other embodiments obtained by a person skilled in the art without making creative efforts belong to the protection scope of the present invention.
It should be noted that: like reference numbers and letters refer to like items in the following figures, and thus, once an item is defined in one figure, it need not be further defined and explained in subsequent figures.
In the description of the present invention, it should be noted that the terms "center", "upper", "lower", "left", "right", "vertical", "horizontal", "inner", "outer", and the like indicate orientations or positional relationships based on the orientations or positional relationships shown in the drawings, and are only for convenience of description and simplification of description, but do not indicate or imply that the device or element referred to must have a specific orientation, be constructed and operated in a specific orientation, and thus, should not be construed as limiting the present invention. Furthermore, the terms "first," "second," and "third" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance.
Referring to fig. 1, an embodiment of the present invention provides a DCB continuous dissolution and separation apparatus, which includes a DCB transposition toluene solution material pool 1, a hot water pool 2, a multistage static mixer 3, and a centrifuge 4.
The multistage static mixer 3 is an SK type or SX type pipeline type static mixer, and comprises a first-stage static mixer 31 and a second-stage static mixer 32, a DCB transposition toluene solution material pool 1 and a hot water pool 2 are respectively connected with a liquid inlet of the first-stage static mixer 31 through pipelines, a first flow meter 5 is arranged between the DCB transposition toluene solution material pool 1 and the first-stage static mixer 31, a first regulating valve 7 is further arranged between the first flow meter 5 and the first-stage static mixer 31, the first flow meter 5 is used for observing the pipeline flow of the DCB transposition toluene solution, and the first regulating valve 7 is used for conveniently regulating the reasonable flow of the DCB transposition toluene solution; be equipped with second flowmeter 6 between hot-water pond 2 and the first order static mixer 31, still install second governing valve 8 between second flowmeter 6 and first order static mixer 31, second flowmeter 6 is used for observing hydrothermal pipeline flow, be convenient for use second governing valve 8 to adjust reasonable hot water flow, the efficiency that hot water dissolved can be increased to the DCB transposition toluene solution flow of adaptation and hot water flow proportion, further shorten the consuming time of dissolving in succession, improve the work efficiency of dissolving separator in succession.
The liquid outlet of first order static mixer 31 is connected with the inlet of second level static mixer 32, and DCB transposition toluene solution and hot water are fed in at multistage static mixer 3 in succession, and intensive mixing helps improving the volume of dissolving that DCB transposition result dissolves in the hot water from the toluene, further improves the rate of recovery of useless toluene and the concentration of DCB aqueous solution, is favorable to follow-up centrifugal separation, improves separation efficiency.
The centrifuge 4 is a commercially available disc centrifuge of type LH270 of Huachengbaoyi factory, the top of the centrifuge is provided with a mixed liquid inlet 41, a waste toluene outlet 42 and a DCB aqueous solution outlet 43, the mixed liquid inlet 41 is connected with the liquid outlet of the second-stage static mixer 32, the waste toluene solution and the DCB aqueous solution are respectively conveyed to the waste toluene outlet 42 and the DCB aqueous solution outlet 43 after centrifugal separation of the centrifuge 4, secondary pollution caused by mixed flow is avoided, the waste toluene outlet 42 is connected with a waste toluene storage tank, the DCB aqueous solution outlet 43 is connected with a DCB aqueous solution storage tank, the centrifuge 4 is made of one of Hastelloy, titanium alloy or fluorine-lined anticorrosive materials, and the phenomenon that the DCB transposition toluene solution corrodes the centrifuge body and then pollutes the separation product is prevented.
Before the DCB continuous dissolving and separating device provided by the specific embodiment works, nitrogen purging pipelines are needed, so that the oxygen content in the device is reduced, and safety accidents caused by mixed ignition of toluene and oxygen are prevented. When the device is operated, the DCB transposition toluene solution in the DCB transposition toluene solution material pool 1 flows through the first flow meter 5 and the first regulating valve 7 and is conveyed into the first-stage static mixer 31, the hot water pool 2 conveys hot water with the temperature of 95 ℃ into the first-stage static mixer 31 through the second flow meter 6 and the second regulating valve 8 and is fully mixed with the DCB transposition toluene solution, the hot water fully dissolves DCB transposition products in the DCB transposition toluene solution, the components of the mixed solution are DCB aqueous solution and waste toluene solution, the mixed solution enters the centrifuge 4 from the mixed solution inlet 41 of the centrifuge 4, the centrifuge 4 is a disc centrifuge of titanium alloy material, the mixed solution starts centrifugal separation in the disc centrifuge, heavy liquid is DCB aqueous solution, the heavy liquid flows out from a DCB aqueous solution outlet 43 to a DCB aqueous solution storage tank, light liquid is waste toluene solution, the light liquid flows out from a waste toluene outlet 42 to the waste toluene storage tank, the DCB aqueous solution and the waste toluene solution do not need to be manually separated by the centrifuge 4, the multistage mixer 3 and the multistage mixer 4 are combined to design a mode of continuous material, the high-conversion efficiency of the hot water solution is improved, and the efficiency of the continuous conversion of the waste toluene solution is improved.
Although the present disclosure has been described above, the scope of the present disclosure is not limited thereto. Those skilled in the art can make various changes and modifications without departing from the spirit and scope of the present disclosure, and such changes and modifications will fall within the scope of the present disclosure.
Claims (8)
1. A DCB continuous dissolution separation apparatus, comprising:
the material pool (1) of the DCB transposition toluene solution is used for storing and pumping the DCB transposition toluene solution;
a hot water tank (2) for storing and pumping hot water;
the multistage static mixer (3) is used for mixing the DCB transposition toluene solution and the hot water, and a liquid inlet of the multistage static mixer is respectively connected with a liquid outlet of the DCB transposition toluene solution material pool (1) and a liquid outlet of the hot water pool (2);
centrifuge (4) for centrifugation DCB aqueous solution and useless toluene solution, its top is equipped with mixed liquid inlet (41), mixed liquid inlet (41) with the liquid outlet of multistage static mixer (3) is connected.
2. The continuous DCB dissolution and separation device according to claim 1, wherein the multistage static mixer (3) comprises a first stage static mixer (31) and a second stage static mixer (32), wherein the inlets of the first stage static mixer (31) are respectively connected to the outlet of the DCB indexing toluene solution material tank (1) and the outlet of the hot water tank (2), the outlet of the first stage static mixer (31) is connected to the inlet of the second stage static mixer (32), and the outlet of the second stage static mixer (32) is connected to the mixed solution inlet (41).
3. The DCB continuous dissolution separation apparatus of claim 1, wherein the centrifuge (4) is a disk centrifuge.
4. The DCB continuous dissolution separation apparatus according to claim 3, wherein the centrifuge (4) has a body made of one selected from Hastelloy, titanium alloy or fluorine-lined anticorrosive material.
5. The DCB continuous dissolution separation apparatus according to claim 1, wherein a first regulating valve (7) is arranged between the liquid outlet of the DCB transposition toluene solution material pool (1) and the liquid inlet of the multistage static mixer (3), and a second regulating valve (8) is arranged between the liquid outlet of the hot water pool (2) and the liquid inlet of the multistage static mixer.
6. The DCB continuous dissolution separation apparatus according to claim 5, wherein a first flow meter (5) is disposed between the DCB indexing toluene solution material pool (1) and the first regulating valve (7), and a second flow meter (6) is disposed between the hot water pool (2) and the second regulating valve (8).
7. The DCB continuous dissolution separation apparatus of claim 1, wherein the multistage static mixer (3) is a pipeline static mixer.
8. The DCB continuous dissolution separation apparatus of claim 7, wherein the pipe-type static mixer is SK type or SX type.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202223065790.0U CN218653902U (en) | 2022-11-18 | 2022-11-18 | DCB dissolves separator in succession |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202223065790.0U CN218653902U (en) | 2022-11-18 | 2022-11-18 | DCB dissolves separator in succession |
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| CN218653902U true CN218653902U (en) | 2023-03-21 |
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| CN202223065790.0U Active CN218653902U (en) | 2022-11-18 | 2022-11-18 | DCB dissolves separator in succession |
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